WO2020027329A1

WO2020027329A1 - Water surface-floating agrochemical preparation

Info

Publication number: WO2020027329A1
Application number: PCT/JP2019/030557
Authority: WO
Inventors: 治入波平; 隆浩大井; 秋山　正樹; 西山　政希; 野澤　俊太郎; 黒津　裕一; 祐太郎田中; 学吉川; 誠一久津間
Original assignee: 北興化学工業株式会社
Priority date: 2018-08-03
Filing date: 2019-08-02
Publication date: 2020-02-06
Also published as: CN112584702B; JPWO2020027329A1; KR20210040400A; JP2022189970A; JP7389746B2; JP7476281B2; CN112584702A

Abstract

The present invention addresses the problem of providing a water surface-floating agrochemical preparation which exhibits good floating properties and diffusion properties in a flooding treatment under shallow water conditions, and with which this performance is maintained even after long term storage. This problem is solved by providing a water surface-floating agrochemical preparation which is characterized: by containing (a) an agrochemical active ingredient, (b) a floating carrier, and (c) at least one type selected from sodium alkylnaphthalene sulfonates and sodium dialkylsuccinate sulfonates; in that (d) the long axis/short axis ratio of the bottom surface of a particle is 1.1-1.4; (e) 80 wt% or more of particles have particle sizes within the range 2.80-1.70 mm; and (f) the number of particles per 1g is 50-150.

Description

Waterborne pesticide formulation

The present invention is excellent in diffusivity and storability, showing good buoyancy and diffusivity in the treatment of paddy fields, especially in flooding treatment under shallow water conditions, and its performance is maintained even after long-term storage. Water-floating pesticide preparations.

粒 Granule, powder, wettable powder, tablet, pack, flowable, aqueous solvent, liquid, emulsion, etc. are known as the dosage form of the agricultural chemical formulation for paddy rice. In recent years, as a labor-saving method of spraying pesticides, pesticide preparations (jumbo agents, flowable agents for undiluted water flooding spraying, etc.) that can be sprayed simply by throwing in from the ridge without entering a paddy field have been developed and used. However, since such a pesticide formulation sprays the pesticide active ingredient locally at a high concentration, it takes a long time for the pesticide active ingredient to uniformly diffuse into the surface water, Rice phytotoxicity or lack of effect due to uneven distribution has become a problem. As a means for solving these problems, it is required that the pesticide active ingredient be promptly and uniformly dispersed after the pesticide formulation is put into a flooded paddy field.

に対し Various methods have been proposed in response to the above-mentioned requirements.

In the pamphlet of International Publication WO 2016-129466 (Patent Document 1), a particle size containing a pesticidal active ingredient, a surfactant, a hollow body, and a solid carrier and having a particle size of 3 mm or more is 80% or more. A method for producing a granular pesticidal composition having a distribution and a property of floating on a water surface, and disintegrating on the water surface within 30 minutes, comprising: (a) a part of a pesticidal active ingredient; Kneading a mixture containing a part of the activator, a part of the hollow body, a part of the solid carrier, and water; (b) kneading the mixture obtained in the step (a), (C) drying the granulated product obtained in the step (b) to obtain granules; and (d) performing the step (c). Crushing the obtained granules; and (e) in the step (d). Kneading a mixture containing the obtained crushed material, the remainder of the pesticidal active ingredient, the remainder of the surfactant, the remainder of the hollow body, the remainder of the solid carrier, and water; (f) the above (e) (G) discharging the kneaded material obtained in the step (b) from a screen having a hole diameter of 3 mm or more using an extrusion granulator; and (g) granulating the granulated material obtained in the step (f). Drying. Granular pesticide compositions have been proposed.

In WO 2016-114200 pamphlet (Patent Document 2), one or more pesticidal active ingredients, a poorly water-soluble polysaccharide having water retention and suppressed swelling in water, a surfactant, A water-containing mixture containing a hollow body, a solid carrier, and water is extruded, granulated, and then dried to remove water. The above-mentioned particle size distribution, having the property of floating on the water surface, and a pesticide granular composition that disintegrates on the water surface within 30 minutes and a method for producing the same, the water-floating large granular pesticide composition containing a water-containing raw material There has been proposed a high-quality water-floating large-sized granular pesticide composition and a method for producing the same.

In the pamphlet of International Publication No. 2015-159906 (Patent Document 3), those containing an agrochemical active ingredient, a floating carrier and water in the range of 0.3 to 3% by mass and having a particle size of 3 mm or more have a particle size distribution of 80% or more. A large pesticide formulation that floats on the surface of the water and disintegrates on the surface of the water within 30 minutes after being thrown into the water, and contains all of the pesticidal active ingredients and auxiliary ingredients (excluding water) that constitute the pesticide formulation. For a total of n kinds of raw materials, a water-floating large granular pesticide formulation having a value X defined by the formula (1) in the range of 0.5 to 2 and a method for producing the same have been proposed.

In JP-A-2012-116788 (Patent Document 4), (a) a bactericidal active ingredient and / or an insecticidal active ingredient, (b) a specific polyoxyethylene alkyl ether, (c) a specific sodium alkylnaphthalene sulfonate, A water-floating pesticide formulation using d) isoparaffin having a distillation point of 277 ° C. to 353 ° C. and (e) a water-floating hollow body has been proposed.

JP-A-2012-116787 (Patent Document 5) discloses (a) a herbicidal active ingredient, (b) a specific polyoxyethylene alkyl ether represented by the general formula (1), and (c) a specific alkylnaphthalenesulfonic acid. A water-floating herbicidal preparation using sodium, (d) isoparaffin having a distillation point of 277 ° C. to 353 ° C., and (e) a water-floating hollow body has been proposed.

In WO 2005-29956 pamphlet (Patent Document 6), a non-disintegrable pesticide granule containing an acidic pesticide active ingredient, a cationic surfactant and a basic substance, which does not disintegrate in water within 30 minutes, a surfactant The particles have a particle size distribution of 80% by mass or more, containing particles having a particle size of 3 mm or more, and have the property of floating on the water surface immediately after being dropped on the water surface, but collapse within 30 minutes. There has been proposed a homogeneously diffusible granular pesticide formulation characterized by the following.

Japanese Patent Application Laid-Open No. 2002-179507 (Patent Document 7) discloses that a substance containing an agrochemical active ingredient and having a particle size of 3 mm or more has a particle size distribution of 80% and a property of floating on the water surface, and has a water surface within 30 minutes. Uniformly diffusible granular pesticide formulation that disintegrates in the above and a uniform diffusible granular product that is spread and spread over an area of 5% to 50% of the total paddy area at a distance of 1m or more from the levee of the paddy field under flooding Pesticide formulations have been proposed.

Japanese Patent Application Laid-Open No. 2002-128605 (Patent Document 8) proposes a water-applied pesticide formulation characterized by using an active ingredient of pesticide, a floating hollow body, and a specific polyoxyalkylene alkyl ether phosphate or a salt thereof. ing.

Japanese Patent Application Laid-Open No. 2000-351701 (Patent Document 9) discloses a water surface containing one or more water surface spreaders composed of a C2 to C4 alkyl alcohol oxide adduct of a C4 to C10 alkyl alcohol and a derivative thereof, and an agricultural chemical active ingredient. Planktonic pesticide solid formulations have been proposed.

JP-A-2001-114603 (Patent Document 10) discloses an inorganic salt, an organic salt, and an organic acid having a particle diameter of 1/10 to 1/2 with respect to the minor axis of the pesticidal active ingredient and the pesticidal solid composition. There has been proposed an agrochemical solid composition comprising one or more water-soluble substances selected from saccharides, saccharides and urea.

Japanese Patent Application Laid-Open No. 2000-319103 (Patent Document 11) discloses a particulate pesticidal water-floatable formulation containing a pesticide active ingredient, a surfactant, a solid carrier, a water-floatability imparting agent and water, and having a water content after molding. A water-suspendable particulate pesticide formulation characterized by being 0.3 to 6 parts per 100 parts by weight and a method for producing the same have been proposed.

Japanese Patent Application Laid-Open No. 2000-319102 (Patent Document 12) discloses that a water-suspendable particulate pesticide containing a pesticidal active ingredient, a surfactant, a solid carrier, and a water-suspendability imparting agent is used to disintegrate the water-suspended particulate pesticide. There has been proposed a water-drop type pesticide formulation packaged in a water-soluble film bag having a dissolution time of 1/5 or less.

Japanese Patent Application Laid-Open No. 2000-302602 (Patent Document 13) discloses that an active ingredient for agricultural chemicals, a surfactant, a solid carrier, an agent for imparting water surface floatability, water, and if necessary, other auxiliary agents are contained. Weight of 0.03 g to 0.3 g, and the density of one grain is 0.4 or more and less than 1.0 (2) The ratio of the short diameter to the long diameter of one grain is 1 to 3, and the external shape composed of a curved surface (3) A water-suspendable particulate pesticide formulation characterized in that the time required for the particles floating on the water surface to disintegrate and disperse is within 30 minutes, and a method for producing the same has been proposed.

In JP-A-11-310503 (Patent Document 14), a pesticide powder formulation or granule having the property of floating and spreading on the water surface and containing no foaming agent is packaged in a perforated water-soluble film. There has been proposed an agricultural chemical pack for throwing in paddy fields, which is prevented from solidifying over time.

拡散 Each prior art has improved diffusivity, but this is the diffusivity under conditions where the water depth (water volume) is guaranteed. On the other hand, in some fields, only a shallow water depth (less than 3 cm) can be maintained due to reasons such as water leakage and natural water reduction. Under such conditions, because the distance between the water surface and the soil is short, if the buoyancy is small, the formulation will stranded or buried in the soil at the time of spraying and settled in large quantities at the spraying point, resulting in phytotoxicity or poor diffusion at the spraying point The effect may be insufficient. Further, the shallow water depth is synonymous with the small amount of water, and in a preparation in which the active ingredient diffuses through the water surface and water, the range in which the active ingredient can diffuse is limited as compared with the normal water depth (about 5 cm). In such fields, more excellent floating and diffusing properties are required, and the prior art was hardly satisfactory. Further, with respect to maintaining these properties even after long-term storage, there is no mention in the prior art, and there is a demand for a formulation excellent in all of floating properties, diffusibility and storage stability.

WO 2016/129466 pamphlet WO 2016/114200 pamphlet WO 2015/159906 pamphlet JP 2012-116788 A JP 2012-116787 A WO 2005/29956 pamphlet JP 2002-179507 A JP-A-2002-128605 JP 2000-351701 A JP 2001-114603 A JP 2000-319103 A JP 2000-319102 A JP 2000-302602 A JP-A-11-310503

The present invention has been made in view of the above-mentioned conventional drawbacks, and in flooding treatment under shallow water conditions, a water-floating pesticide formulation having excellent diffusibility, more specifically, having excellent floating properties of a pesticide formulation, and being sprayed. The formulation diffuses on the water surface without settling below the surface of the water, and the formulation shows excellent diffusibility in water even after disintegration in water over time, and its performance is maintained even after long-term storage The purpose of the present invention is to provide a water-susceptible pesticide formulation.

The present inventors have intensively studied to solve the above problems. As a result, the pesticidal active ingredient, a floating carrier, and as the anionic surfactant, one or more selected from the group consisting of sodium alkylnaphthalenesulfonate and sodium dialkylsuccinatesulfonate. The purpose of the present invention is to provide a water-susceptible pesticide preparation characterized in that the particle size ranges from 1.1 to 1.4, the particle size is 2.80 mm to 1.70 mm, 80% by weight or more, and the number of particles per gram is 50 to 150. I found to do.
In addition, as an agrochemical active ingredient, a floating carrier, an anionic surfactant, a polyoxyalkylene alkyl ether phosphate ester salt is contained together with a water-soluble alkylene glycol such as propylene glycol, and as an anionic surfactant. Furthermore, it has been found that a water-floating pesticide formulation containing at least one selected from sodium alkylnaphthalenesulfonate and sodium dialkylsuccinatesulfonate has excellent diffusibility. Then, the ratio of the major axis / minor axis of the bottom surface of the particles of this preparation is 1.1 to 1.6, and the particle size is 80% by weight or more in the range of 2.80 mm to 1.70 mm, and the number of particles per gram is 50 to 200. By doing so, it has been found that the diffusivity of the water-floating pesticide formulation is particularly excellent.
Further, in the above pesticide preparation having a water surface floating property, the particle size is 90% by weight or more in the range of 2.80 mm to 1.70 mm, and the floating carrier is a shirasu balloon having an average particle diameter of 90 to 120 μm; Further, as an agent, alkyl naphthalene sulfonic acid formaldehyde condensate Na, naphthalene sulfonic acid formaldehyde condensate Na, and partially desulfonated lignin sulfonic acid Na (in the case of containing a polyoxyalkylene alkyl ether phosphate ester salt and a water-soluble alkylene glycol, , Lignin sulfonate), and carboxymethylcellulose Na (polyoxyalkylene alkyl ether phosphate salt and water-soluble alkylene glycol as a binder) Found more preferable to contain at least one) selected from the Le cellulose Na and polyvinyl alcohol, and have completed the present invention.

That is, the present invention has the following contents as its gist.
[1] A water surface containing: a) an agricultural chemical active ingredient; b) a hollow body as a floating carrier; and c) at least one selected from sodium alkylnaphthalenesulfonate and sodium dialkylsuccinatesulfonate as an anionic surfactant. A floating pesticide formulation that has the following characteristics:
d) the ratio of major axis / minor axis of the bottom surface of the grains is 1.1 to 1.4;
e) The particle size is at least 80% by weight in the range of 2.80 mm to 1.70 mm, and f) The number of particles per gram is 50 to 150.
[2] e) The water-floating pesticide preparation according to [1], wherein the particle size is 90% by weight or more in a range of 2.80 mm to 1.70 mm.
[3] The water-floating agrochemical formulation according to any of [1] or [2], wherein the hollow body as the floating carrier is a shirasu balloon having an average particle diameter of 90 to 120 μm.
[4] The composition further comprises, as an anionic surfactant, at least one selected from an alkylnaphthalenesulfonic acid formaldehyde condensate Na, a naphthalenesulfonic acid formaldehyde condensate Na, and a partially desulfonated sodium ligninsulfonate. The water-floating pesticide formulation according to any one of [1] to [3].
[5] The water-floating pesticide formulation according to any one of [1] to [4], further comprising carboxymethylcellulose Na as a binder.
[6] a) an agrochemical active ingredient, b) a hollow body as a floating carrier, c) a polyoxyalkylene alkyl ether phosphate ester salt represented by the following general formula (I) and a water-soluble alkylene glycol, and d) a pigment. A water-floating pesticide formulation comprising, as an ionic surfactant, at least one selected from sodium alkylnaphthalenesulfonate and sodium dialkylsuccinatesulfonate.

[Wherein, R represents a linear or branched alkyl group having 8 to 10 carbon atoms, A represents an alkylene group having 2 to 4 carbon atoms, n represents an integer of 1 to 20; And q represent an integer in which p + q = 3 and p = 1 or 2, and M represents a hydrogen atom, an alkali metal atom, an ammonium group, or an organic ammonium group. When there are a plurality of R, A, and M, the types may be the same or different. ]
[7] The water-floating pesticide preparation according to [6], wherein the water-soluble alkylene glycol is propylene glycol.
[8] The pesticide formulation according to [6] or [7], having the following characteristics:
e) the ratio of major axis / minor axis of the bottom surface of the grains is 1.1 to 1.6;
f) 80% by weight or more in a particle size range of 2.80 mm to 1.70 mm, and g) 50 to 200 particles per gram.
[9] f) The water-floating pesticide preparation according to [8], wherein the particle size is 90% by weight or more in a range of 2.80 mm to 1.70 mm.
[10] The water-floating pesticide formulation according to any one of [6] to [9], wherein the hollow body as the floating carrier is a shirasu balloon having an average particle diameter of 90 to 120 μm.
[11] The composition further comprises, as an anionic surfactant, at least one selected from an alkylnaphthalenesulfonic acid formaldehyde condensate Na, a naphthalenesulfonic acid formaldehyde condensate Na, and a ligninsulfonic acid Na [6]. ] The water-floating pesticide preparation according to any one of [10] to [10].
[12] The water-floating pesticide according to any one of [6] to [11], further comprising at least one selected from carboxymethylcellulose Na and polyvinyl alcohol as a binder.

Since the water-floating pesticide formulation of the present invention has good floatability and diffusibility, it is excellent in the water surface movement of the formulation itself and the diffusivity after the formulation collapses even in flooded sewage under shallow water conditions below 3 cm. Even after long-term storage, its performance can be maintained. Therefore, at the time of spraying, a spraying machine such as a power spraying machine or a spraying tool such as a granulator is not necessarily required, and manual spraying can be performed. In addition, the use scene is not limited because it is spread even when sprayed from one side of the ridge. Furthermore, since the quality deterioration is suppressed even after long-term storage, it is possible to hold the storage in advance. Therefore, the water-floating pesticide formulation of the present invention is a labor-saving formulation in which the physical, temporal, and economic burden on the sprayer is reduced.

Hereinafter, the water-floating pesticide formulation of the present invention will be described in more detail.

<A. About composition components>
The pesticidal active ingredient that can be used in the present invention may be any one as long as it can be applied to paddy rice. Such pesticidal active ingredients include the following.

《Insecticidal active ingredient》
For example, as an insecticidal active ingredient, an organic phosphorus compound (MEP, diazinon, etc.), a carbamate compound (BPMC, carbosurphan, etc.), a pyrethroid compound (cycloprothrin, etc.), a nereistoxin compound (such as thiocyclam), a neonicotinoid compound ( Insecticides of imidacloprid, thiamethoxam, clothianidin, dinotefuran, etc., diamides (flubendiamide, chlorantraniliprole, cyantraniliprole, etc.), phenylpyrazoles (fipronil, ethiprole, etc.), and spinosyns (spinosad, spinetoram, etc.) And insect growth regulators (tebufenozide, chromafenozide, methoxyfenozide, buprofezin, etc.), and other synthetic insecticides (pymetrozine, triflumezopyrim, etc.) and biological pesticides.

《Bactericidal active ingredient》
Examples of the bactericidal active ingredient include inorganic coppers, organic coppers, inorganic sulfur agents, organic sulfur agents, organic phosphorus compounds (such as IBP), melanin biosynthesis inhibitors (pyroquilon, tricyclazole, carpropamide, diclosimet, phenoxanil, etc.). , Benzimidazoles (such as benomyl, thiophanatemethyl, dietofencarb), amides (such as mepronil, flutolanyl, flametopyr, penflufen, floxapyroxad, thifluzamide, thiazinyl, isotianil), and sterol biosynthesis inhibitors (such as pefurazoate, ipconazole, simeconazole) , Strobilurins (azoxystrobin, metominostrobin, orysastrobin, etc.), antibiotic fungicides (kasugamycin, validamycin, etc.), other synthetic fungicides, biological pesticides, etc. It is.

<< herbicidal active ingredient >>
Examples of the herbicidal active ingredients include phenoxy acids (MCPA thioethyl, MCPB ethyl, etc.), carbamates, acid amides (tenylchlor, butachlor, bromobutide, etc.), acetanilides, ureas, sulfonylureas (bensulfuronmethyl, Benzofuranylalkylsulfonic acid (such as benfresate), pyrimidyloxybenzoic acid (such as penoxsulam), triazine (such as simethrin), diazine, diazole (such as pyrazolate and benzophenap), bipyridylium, Dinitroaniline type, aromatic carboxylic acid type, imidazolinone type, fatty acid type, organic phosphorus type, amino acid type, tetrazolinone type (fentrazamide etc.), diphenyl ether type (bifenox etc.), oki Zolidinedione type (such as pentoxazone), nitrile type, phenylphthalimide type, cineol type, indandione type, benzofuran type, triazolopyrimidine type, oxazinone type (such as oxadiclomephone), allyltriazolinone type, isourazole type, pyrimidinylthiophthalide type And triazolinones (such as ipfencarbazone), and triketones (such as tefuryltrione, mesotrione, and benzobicyclone) inorganic herbicides.

《Plant growth regulator》
Examples of plant growth regulators include ethylene-based, auxin-based, cytokinin-based, and gibberellin-based.

Specific specific pesticidal active ingredients contained therein are, for example, “Agricultural Chemical Handbook 2016 Edition” (published by the Japan Plant Protection Association), “SHIBUYA INDEX 13th Edition” (published by the SHIBUYA INDEX Research Group), “The Pesticide Manual Sixteenth Edition "(published by British Crop Protection Corporation).

In addition, as the pesticidal active ingredient used in the present invention, if it serves the same purpose as the present invention and is applied as a water-floating pesticide formulation, other than the above-mentioned conventionally known or future-developed pesticide active ingredients, Ingredients can also be applied.

The above pesticidal active ingredient may be used alone or in combination of two or more without any problem. The amount added is usually 0.01 to 60% by weight, preferably 0.05 to 50% by weight in the preparation.

《Floating carrier》
The buoyant carrier used in the present invention has a function of a disintegration aid because it has a hollow body, so that buoyancy is generated. It contributes to diffusivity in terms of floating, disintegrating properties. Examples of the agent include those having a hollow body such as a shirasu balloon, a fly ash balloon, a ceramic balloon, and a synthetic resin hollow body. If these components have too large an average particle size, the formulation tends to become brittle. Therefore, those having an average particle size of 200 μm or less are preferable.

Shirasu balloons having an average particle diameter of 90 to 120 μm are particularly preferable in consideration of the balance between the floating properties, disintegration properties and the hardness of the preparation.

浮遊 The amount of the floating carrier that can be used in the present invention may be an amount sufficient to float the preparation on the water surface, and is usually 2.0 to 80% by weight, preferably 5.0 to 70% by weight. One or more of the above may be used.

<< Alkyl naphthalene sulfone Na and dialkyl succinate sulfonate Na >> (anionic surfactant)
Since the alkyl naphthalene sulfone Na and the dialkyl succinate sulfonate Na used in the present invention are anionic surfactants having a good balance between wettability and dispersibility, one kind of these anionic surfactants is used. The above-mentioned content contributes to the disintegration and dispersibility of the preparation, and this function maintains the performance even after long-term storage. In addition, during the production, an effect of reducing the amount of water required for granulation due to its wetting ability and reducing the load at the time of granulation is also provided.

添加 The addition amount of sodium alkylnaphthalenesulfone and sodium dialkylsuccinatesulfonate which can be used in the present invention is 0.5 to 30% by weight, preferably 1 to 20% by weight in the preparation.

<< Alkylnaphthalenesulfonic acid formaldehyde condensate Na, naphthalenesulfonic acid formaldehyde condensate Na, partially desulfonated sodium ligninsulfonate, and sodium ligninsulfonate >> (additional anionic surfactant)
The water-floating pesticide formulation of the present invention has a diffusivity by further adding one or more selected from alkyl naphthalene sulfonic acid formaldehyde condensate Na, naphthalene sulfonic acid formaldehyde condensate Na, and partially desulfonated lignin sulfonic acid Na. And enhance the storage stability function.

Each component is a polymeric sulfonic acid surfactant having a molecular weight of several thousand to several tens of thousands, and its dispersibility is enhanced when used in combination with sodium alkyl nalnaphthalene sulfonate and sodium dialkyl succinate sulfonate. It is maintained after storage.

In the case of containing a polyoxyalkylene alkyl ether phosphoric acid ester salt and a water-soluble alkylene glycol described below, it is selected from alkyl naphthalene sulfonic acid formaldehyde condensate Na, naphthalene sulfonic acid formaldehyde condensate Na, and sodium lignin sulfonic acid. The addition of one or more enhances the diffusivity and storage stability functions.

The addition amount of the alkyl naphthalene sulfonic acid formaldehyde condensate Na, the naphthalene sulfonic acid formaldehyde condensate Na, the partially desulfonated sodium lignin sulfonate, and the sodium lignin sulfonate which can be used in the present invention is 0.5 to 30% by weight in the preparation. %, Preferably 1 to 20% by weight.

<< Polyoxyalkylene alkyl ether phosphate ester salt >> (anionic surfactant)
The following general formula (I) used in the present invention

[Wherein, R represents a linear or branched alkyl group having 8 to 10 carbon atoms, A represents an alkylene group having 2 to 4 carbon atoms, n represents an integer of 1 to 20; And q represent an integer in which p + q = 3 and p = 1 or 2, and M represents a hydrogen atom, an alkali metal atom, an ammonium group, or an organic ammonium group. When there are a plurality of R, A, and M, the types may be the same or different. ]
The polyoxyalkylene alkyl ether phosphate salt represented by the formula (1) has excellent spreadability, wettability, dispersibility and ability to gel upon contact with water. When the formulation comes into contact with water, the component gels in the form of incorporating the pesticidal active ingredient or the buoyant carrier, thereby diffusing the pesticide active ingredient farther with the buoyancy enhanced by the buoyant carrier. Becomes possible. In addition, when the gel is dissolved in water, the component is present at a high concentration around the pesticide active component, so that the component is efficiently adsorbed to the pesticide active component, and even after the gel state is released, the pesticide activity is further increased. Components diffuse. In addition, since the gelling ability is not deteriorated, the effect of imparting the spreading and dispersing power to the preparation and the aid of floating are maintained even after long-term storage.

In the present invention, examples of the alkylene group represented by A in the phosphate ester salt represented by the general formula (I) include an ethylene group having 2 carbon atoms, a propylene group having 3 carbon atoms, and a butylene group having 4 carbon atoms. Can be
The alkylene group preferably contains an ethylene group having 2 carbon atoms in order to exhibit the expanding power and the gelling ability in the present invention. The alkylene group represented by A may be only an ethylene group having 2 carbon atoms, or may be an ethylene group having 2 carbon atoms, a propylene group having 3 carbon atoms, a butylene group having 4 carbon atoms, or both. May be included.
In the present invention, the alkyl group represented by R in the phosphoric acid ester salt represented by the general formula (I) has 8 to 10 carbon atoms in order to balance solubility in water and spreading power on the water surface. And the alkyl group includes an n-octyl group, an n-decyl group, an isodecyl group, a 2-ethylhexyl group, and the like.
In the present invention, the phosphate salt represented by the general formula (I) is not particularly limited as long as the cation (M in the formula) which is a phosphate ion pair is within a range not to lose the function of the present invention. , M include a hydrogen atom, a lithium atom, an alkali metal atom such as a sodium atom or a potassium atom, and the substituent includes an organic ammonium such as an ammonium group, a methyl ammonium group, or a dimethyl ammonium group. Groups.
In this preparation, since a heating and drying step is included in the manufacturing process, the cation (M in the formula) is preferably K ⁺ , Na ⁺ , or H ⁺ which is hardly volatilized even in the heating and drying step.
In the present invention, the phosphate ester salt represented by the general formula (I) has the number of phosphate ester bonds of 1 (monoester) in order to balance solubility in water and spreading power on the water surface. ) Or 2 (diester). When the phosphate ester salt is a monoester, p = 1 and q = 2. In this case, the alkyl groups represented by R may be the same or different. When the phosphate is a diester, p = 2 , Q = 1, and in this case, the atoms and the like represented by M may be the same or different.
In the present invention, the phosphoric acid monoester salt and the phosphoric acid diester salt represented by the general formula (I) may be used alone or as a mixture.

The amount of the polyoxyalkylene alkyl ether phosphate ester salt that can be used in the present invention is 1 to 40% by weight, preferably 3 to 25% by weight in the preparation. No problem.

《Water-soluble alkylene glycol》
The water-soluble alkylene glycol used in the present invention is essential for exhibiting the function of the polyoxyalkylene alkyl ether phosphate salt. A feature of the water-soluble alkylene glycol having both hydrophilicity and lipophilicity is that when used in combination with a polyoxyalkylene alkyl ether, the water dissolution time of the gel generated upon contact with water is adjusted. This not only maximizes the spreading and dispersing power of the polyoxyalkylene alkyl ether phosphoric acid ester salt, but also retains the floating carrier in the gel, thereby providing an auxiliary floating effect to the formulation. The following effects can also be obtained.

The water-soluble alkylene glycol that can be used in the present invention may be any water-miscible water, and examples thereof include ethylene glycol, propylene glycol, butylene glycol, pentylene glycol, and hexylene glycol. There is no problem even if the above are used together.

添加 The amount of the water-soluble alkylene glycol usable in the present invention is 0.5 to 20% by weight, preferably 1 to 10% by weight in the preparation.

《Binder》
Auxiliary binders include dextrins (such as roasted dextrins and enzyme-modified dextrins), acid-degraded starch, oxidized starch, pregelatinized starch, etherified starch (such as carboxymethyl starch and hydroxyalkyl starch), and esterified starch (acetic acid). Starches and phosphate starches), processed starches such as cross-linked starches and grafted starches, natural substances such as sodium alginate, gum arabic, gelatin, tragacanth gum, locust bean gum, and casein, such as sodium carboxymethylcellulose, hydroxyethylcellulose, Cellulose derivatives such as hydroxypropylcellulose, hydroxypropylmethylcellulose, methylcellulose, ethylcellulose and acetylcellulose, and for example, polyvinyl alcohol and polyvinyl alcohol Although Rupiroridon etc., is not limited to, no problem be used in combination with one or more of these.

Further, carboxymethylcellulose Na is preferable from the viewpoint of disintegration dispersibility.
In addition, when it contains a polyoxyalkylene alkyl ether phosphate ester salt and a water-soluble alkylene glycol, carboxymethylcellulose Na or polyvinyl alcohol is preferable from the viewpoint of disintegration dispersibility.
The content of the binder usable in the present invention is preferably 0.1 to 10% by weight.

《Other auxiliaries》
The water-floating pesticide formulation of the present invention may contain the following components as an auxiliary agent in addition to the above-mentioned components as long as the effects of the present invention are not lost.

For example, examples of the surfactant include a nonionic surfactant, an anionic surfactant other than the above, a cationic surfactant, and an amphoteric surfactant.

Examples of the nonionic surfactant include polyoxyethylene alkyl aryl ether, polyoxyethylene alkyl ether, polyoxyethylene aryl aryl ether, polyoxyethylene alkyl ester, and sorbitan alkyl ester.

Other anionic surfactants include dodecylbenzene sulfonate, alkyl sulfonate, lauryl sulfate, α-olefin sulfonate, polyoxyethylene alkyl sulfosuccinate, polyoxyethylene alkyl ether sulfate, Polyoxyethylene alkyl aryl ether sulfate, polyoxyethylene aryl phenyl ether phosphate, polyoxyethylene styryl phenyl ether phosphate, and (co) polymers of carboxylic acids such as acrylic acid and maleic acid, and styrene sulfone Sodium salts and potassium salts of those obtained by copolymerizing an acid, a vinyl group and the like can be mentioned.
The sodium and potassium salts of (co) polymers of carboxylic acids such as acrylic acid and maleic acid, and those obtained by copolymerizing them with styrenesulfonic acid and vinyl groups, contribute to the disintegration and dispersibility of the preparation. Can be expected.

Examples of the cationic surfactant include an alkyltrimethylammonium salt, an alkyldimethylbenzylammonium salt, and an alkylpyridinium salt.

Examples of the amphoteric surfactant include dialkylaminoethyl betaine and alkyldimethylbenzyl betaine.

界面 Surfactants that can be used in the present invention are not limited to these examples, and one or more surfactants may be used in combination. The content of the surfactant in the preparation is preferably 0.1 to 20% by weight.

固体 Examples of the solid carrier usable in the present invention include the following.

For example, clay, quartz, calcite, sepiolite, dolomite, chalk, kaolin, pyrophyllite, sericite, halothite, metahalothite, Kibushi clay, Frogme clay, pottery stone, ziglite, allophane, shirasu, Natural minerals such as keratin, talc, pumice, sepiolite, bentonite, hectorite, zeolite, and diatomaceous earth, such as calcined clay, perlite, vermiculite, attapulgaz clay, and calcined products of natural minerals such as calcined diatomaceous earth, such as carbonic acid Inorganic salts such as magnesium, calcium carbonate, sodium carbonate, sodium bicarbonate, ammonium sulfate, sodium sulfate, magnesium sulfate, diammonium hydrogen phosphate, ammonium dihydrogen phosphate, and potassium chloride, such as glucose, fructose, sucrose, and lactose Sugars, eg Polysaccharides such as starch, powdered cellulose, and dextrin; organic substances such as urea, urea derivatives, benzoic acid and salts of benzoic acid; and plants such as wood flour, corn cob, walnut shell, and tobacco stem , White carbon and the like.

添加 The amount of the solid carrier that can be used in the present invention is 3 to 95% by weight, preferably 5 to 90% by weight in the preparation.

Examples of preservatives and antibiotic agents include potassium sorbate, p-chloro-m-xylenol, butyl p-oxybenzoate, 1,2-benzoisothiazolin-3-one, 5-chloro-2-methyl-4-isothiazoline-3 PH adjusters such as -one and 2-methyl-4-isothiazolin-3-one such as hydrochloric acid, sulfuric acid, citric acid, phosphoric acid, and magnesium carbonate; An inhibitor, an ultraviolet inhibitor, a crystal precipitation inhibitor, and the like may be added, but are not limited to the auxiliaries exemplified here.

添加 The amount of these auxiliaries that can be used in the present invention is 0.01 to 15% by weight, preferably 0.1 to 10% by weight in the preparation.

<B. About physical properties of preparation>
In the water-floating pesticide preparation of the present invention, in order to exhibit good floating and diffusibility, and to show an effect of excellent preservation, not only the preparation components but also the following <the major axis of the bottom of the particle / Physical properties of the pesticide formulation such as "short diameter ratio", "particle size", and "number of particles per 1g" are required.

《Long diameter / short diameter ratio of the bottom of the grain》
In the water-floating pesticide formulation of the present invention, the bottom surface of the grain refers to a surface derived from the screen hole at the time of granulation, and the major axis and the minor axis at the bottom are obtained by drawing a straight line (diameter) passing through the center of the bottom. The maximum diameter is the major axis, and the minimum diameter is the minor axis.

Therefore, the ratio of the major axis / minor axis of the bottom surface of the granules is determined by measuring the maximum diameter (major axis) and the minimum diameter (minor axis) of the cross-sectional portion with a microscope after cutting the product with a cutter so that the bottom surface becomes a cross section. It refers to a value obtained by calculating the ratio of the major axis to the minor axis as the average value of 10 preparations.

In the water-floating pesticide formulation of the present invention, adjusting the ratio of the major axis to the minor axis at the bottom surface of the grain has an effect on the floatability, diffusibility, and storage stability (formulation distance after long-term storage, diffusion distance) of the formulation. Contribute. It is essential to adjust the ratio of major axis / minor axis to a range of 1.1 to 1.4 in order to impart the effect of improving the floating and diffusivity. The ratio of the major axis / minor axis is a parameter expressing the shape of the preparation, and 1.0 (minimum value) is such that the shape of the bottom surface is a perfect circle, and the larger the value, the closer the shape of the grain becomes to a flat shape. When the ratio of major axis / minor axis is 1.0, the movement of the preparation on the water surface is slow, causing a decrease in diffusibility. When the ratio is more than 1.4, the movement on the water surface becomes faster but disintegrates and disperses quickly. As a result, the diffusion distance of the active ingredient is reduced.
When the polyoxyalkylene alkyl ether phosphate salt and propylene glycol are contained, the gel formed upon contact with water increases the disintegration time of the preparation into water. Up to 6 is possible. Further, regarding the formulation reach distance and diffusion distance after long-term storage, when the ratio of major axis / minor axis is 1.1 or more, deterioration in quality after long-term storage is suppressed. These factors may be due to an increase in the area of the formulation that comes into contact with the water surface with an increase in the ratio of the major axis / minor axis, thereby making the formulation more susceptible to the buoyancy of the water, or increasing the release rate of the surfactant at the surface of the water. It is presumed that the efficiency of collapse and dispersion of the water surface is improved.

As a method of adjusting the ratio of major axis / minor axis, in the extrusion granulation step, the diameter of the extruded hole is adjusted at the time of granulation, and then, in the granulation step, a drum-type granulator or a machine for rotating the granules such as a malmerizer. The method of controlling the ratio of the long diameter to the short diameter by controlling the centrifugal force by rotating the granulated material before drying using the method described above.
Note that the granules before drying are soft because the binder contains water and is swollen, and when the granulated particle size (extruded hole diameter) is large, the granulated material is also affected by its own weight. For this reason, when a rotational motion is applied, the centrifugal force and the own weight act, and the cross section of the granulated material becomes flat (the generation of a long diameter and a short diameter).

《Granularity》
In the water-floating pesticide formulation of the present invention, the particle size is determined based on the weight of the formulation remaining on the 1.70 mm sieve when 100 g of the formulation is sieved with 2.80 mm and 1.70 mm test sieves. , Is calculated from the following equation (1).

において In the water-floating pesticide preparation of the present invention, adjusting the particle size contributes to the floating and diffusion properties of the preparation. From the viewpoint of the balance between the floating property and the diffusibility, the particle size is essential to be 80% by weight or more in the range of 2.80 mm to 1.70 mm, and more preferably 90% by weight or more. In the particle size, those smaller than the particle size range are less likely to sink due to less buoyancy because the amount of buoyant carrier is small, and those with larger particle size are slower in movement on the water surface due to the larger weight per particle. , The diffusivity becomes worse.

As a method of adjusting the particle size, the extrusion hole diameter at the time of granulation is adjusted in the extrusion granulation step, and then, in the sizing step, the length of the granules of the granulated product before drying is appropriately adjusted to control the particle size. Method. The granulator used for adjusting the particle size is not particularly limited, but a rotary granulator such as a drum granulator or a marmellaizer, and a crushing granulator such as a pin mill, an oscillator, a Landel mill, and a nebulizer. Can be used. From the viewpoint of economical efficiency and labor saving at the time of production, a rotary particle sizer such as a drum type particle sizer capable of simultaneously adjusting the ratio of the major axis to the minor axis of the bottom of the grains is preferable.

<< Number of grains per 1g >>
In the water-floating pesticide preparation of the present invention, the number of particles per 1 g is a value obtained by measuring the number of particles of 5.0 g of the weighed preparation with a particle counter, and dividing the measured value by 1/5 (rounded off to the decimal point). Indicated by

In the water-floating pesticide formulation of the present invention, adjusting the number of particles per gram contributes to the floatability and diffusibility of the formulation. It is essential that the number of grains per 1 g is 50 to 150 from the viewpoint of the balance between the floating property and the diffusive property. For the same reason as the above particle size, particles having more than 150 particles per gram have small particles, and have low buoyancy, so that they tend to sink. Movement slows down and the diffusivity deteriorates.
In addition, when the polyoxyalkylene alkyl ether phosphate salt and propylene glycol are contained, even if the particles have a small buoyancy due to the enhanced diffusivity, they can be diffused farther, so that the upper limit of the number of particles per gram can be up to 200. .

As a method for adjusting the number of particles per 1 g, a method of controlling the number of particles per 1 g by crushing the granules before drying in the sizing step is exemplified. The granulator used for adjusting the number of grains is not particularly limited, but a rotary granulator such as a drum-type granulator or a malmerizer, and a crushing-type granulator such as a pin mill, an oscillator, a Landel mill, and a nebulizer. Machine can be used. From the viewpoints of economical efficiency and labor saving during production, a rotary particle sizer such as a drum type particle sizer capable of simultaneously adjusting the ratio of the major axis / minor axis of the bottom surface of the grains and the particle size is preferable.

<Production method of pesticide formulation floating on water>
The water-floating pesticide preparation of the present invention is produced by an extrusion granulation method, and is advantageous in terms of economy and production efficiency.

As the production process, an agrochemical active ingredient, a floating carrier, at least one selected from sodium alkylnaphthalenesulfonate and sodium dialkylsuccinatesulfonate, if necessary, a polyoxyalkylene alkyl ether phosphate salt, if necessary, Then, at least one selected from alkyl naphthalene sulfonic acid formaldehyde condensate Na, naphthalene sulfonic acid formaldehyde condensate Na, and partially desulfonated lignin sulfonic acid Na, and lignin sulfonic acid Na, and various adjuvants are added. Mix uniformly using a juice mixer, hammer mill, Lodige mixer or ribbon mixer. Water is added to this mixture and kneaded using a double-arm kneader or a ribbon mixer. When the agricultural chemical active ingredient is wet-pulverized and added to the slurry for reasons such as mixing accuracy, it is added together with water at the time of kneading.

において In the granulating step and the sizing step after the kneading step, the physical properties of the water-floating pesticide preparation of the present invention are adjusted. In the sizing process, the ratio of the major axis / minor axis, the particle size, and the number of grains at the bottom of the grains may be adjusted at once, or the particle size and the number of grains may be adjusted after adjusting the ratio of the major axis / minor axis of the grains at the bottom. Good. It is preferable to omit the number of steps and adjust them all at once from the viewpoint of improving economical efficiency at the time of manufacturing.

において In the granulation and sizing step, first, the mixture is granulated using an extrusion granulator such as a basket granulator or a screw granulator. The extrusion pore diameter during granulation is preferably 2.8 to 3.0 mm in order to adjust the physical properties of the water-floating pesticide formulation of the present invention. If the extruded pore diameter, the water-floating pesticide formulation of the present invention of the present invention is obtained by sizing the obtained granules with a machine such as a drum-type sizing machine and a melomerizer that applies centrifugal force. In addition to the ratio of major axis / minor axis at the bottom surface being 1.1 to 1.4, the particle size is to be 80% by weight or more in the range of 2.80 mm to 1.70 mm so that the number of particles per gram is 50 to 150. It can be sized. After sizing, the resultant is dried using a fluidized bed drier or a bed drier, and then sieved to obtain the water-floating pesticide formulation used in the present invention.

When a pesticidal active ingredient whose dissolution is to be promoted is used in combination, a coating step can be added as long as the effect of the present invention is not lost.

<Use form of water-floating pesticide formulation>
The water-floating pesticide preparation of the present invention is directly sprayed without entering a paddy field. Examples of the spraying method include manual spraying, spraying in a container such as a cup, mechanical spraying using a power sprayer, aerial spraying using a radio-controlled helicopter, a drone, or the like, water sprinkling spraying on water flowing into a paddy field, and the like. Considering the aspect of avoiding the exposure of the sprayer to the exposure, a spraying method that does not directly touch the formulation is preferable. The application rate is usually 50 to 500 g, preferably 75 to 300 g per 10a.

Hereinafter, the present invention will be specifically described based on examples, but the present invention is not limited thereto.

In the following Examples and Comparative Examples, “parts” means “parts by weight” and “%” means “% by weight”.

Further, in the following Examples and Comparative Examples, the equipment (microscope, sieve shaker, particle number measuring device) used for measuring the ratio of the major axis / minor axis, the particle size, and the number of particles in the water-floating pesticide formulation are respectively VHX-5000 (manufactured by Keyence Corporation) sieve shaking machine 振 Low tap type (manufactured by Iida Seisakusho), multi-auto counter KC-1M5 type (manufactured by Fujiwara Seisakusho).

[Example 1]
Kasugamycin 24.0 parts (bactericidal active ingredient), Shirasu balloon (average particle diameter 70-90 μm) (floating carrier) 25.0 parts, alkylnaphthalenesulfonic acid Na 3.0 parts, dextrin 5.0 parts, bentonite 10.0 Parts, 30.0 parts of pearlite and 3.0 parts of clay were pulverized and mixed with a hammer mill (Sample Mill KIIW-1, manufactured by Dalton) to obtain a powder mixture. The obtained powder mixture was put into a double-arm kneader (KDHJ, manufactured by Dalton), and kneaded for 15 minutes after water addition. Next, this water-kneaded product was granulated by an extrusion granulator equipped with a basket type screen having a hole diameter of 3.0 mm. The obtained granules were pre-dried, sized with a drum type granulator, and dried with a fluidized bed drier. This was sieved at 3.35 mm to 2.00 mm to obtain a water-floating pesticide formulation. The particle size of the obtained preparation was 85% in the range of 2.80 to 1.70 mm, the ratio of major axis / minor axis at the bottom was 1.2, and the number of particles per gram was 98.

[Example 2]
The pharmaceutical composition was 24.0 parts of kasugamycin (a bactericidal active ingredient), 30.0 parts of fly ash balloon (average particle diameter of 80 to 120 μm) (floating carrier), 1.5 parts of sodium dialkylsuccinatesulfonate, 2.0 parts of carboxymethylcellulose Na2.0. Parts, 35.0 parts of perlite, 7.5 parts of clay, 2.8 mm in particle size, and prepared a water-floating pesticide formulation according to Example 1. The particle size of the obtained preparation was 83% in the range of 2.80 to 1.70 mm, the ratio of major axis / minor axis at the bottom was 1.2, and the number of particles per 1 g was 105.

[Example 3]
The pharmaceutical composition was 24.0 parts of kasugamycin (bactericidal active ingredient), 2.0 parts of acrylonitrile resin balloon (average particle diameter of 20 to 40 μm) (floating carrier), 3.0 parts of sodium alkylnaphthalenesulfonate, 2.0 parts of sodium polyacrylate. Parts, 2.0 parts of carboxymethylcellulose Na, 57.0 parts of pearlite, 10.0 parts of clay, and a particle diameter of 3.0 mm. The particle size of the obtained preparation was 86% in the range of 2.80 to 1.70 mm, and the ratio of major axis / minor axis at the bottom was 1.3, and the number of particles per gram was 113.

[Example 4]
The formulation composition was 24.0 parts of kasugamycin (bactericidal active ingredient), 25.0 parts of ceramic balloon (average particle diameter of 20 to 150 μm) (floating carrier), 3.0 parts of sodium alkylnaphthalenesulfonate, 2.0 parts of carboxymethyl cellulose Na, Diatomaceous earth: 36.0 parts, clay: 10.0 parts, particle size: 3.0 mm, and a water-floating pesticide formulation was prepared according to Example 1. The particle size of the obtained preparation was 93% in the range of 2.80 to 1.70 mm, the ratio of major axis / minor axis at the bottom was 1.1, and the number of particles per 1 g was 83.

[Example 5]
The formulation composition was 24.0 parts of kasugamycin (bactericidal active ingredient), 30.0 parts of shirasu balloon (average particle diameter 70 to 90 μm) (floating carrier), 1.5 parts of sodium dialkylsuccinatesulfonate, and 1.5 parts of acrylic acid-maleic acid. Example 1 was made into 2.0 parts of polymer Na, 3.0 parts of carboxymethylcellulose Na, 10.0 parts of bentonite, 20.0 parts of pearlite, 4.5 parts of white carbon, 5.0 parts of clay, and a particle size of 2.8 mm. A water-floating pesticide formulation was prepared according to the standard. The particle size of the obtained preparation was 95% in the range of 2.80 to 1.70 mm, and the ratio of major axis / minor axis at the bottom was 1.3, and the number of particles per gram was 88.

[Example 6]
The pharmaceutical composition was 24.0 parts of kasugamycin (bactericidal active ingredient), 30.0 parts of shirasu balloon (average particle size of 90 to 120 μm) (floating carrier), 3.0 parts of sodium alkylnaphthalenesulfonate, acryl-methacrylic acid copolymer Na water 2.0 parts, carboxymethyl cellulose Na 3.0 parts, diatomaceous earth 33.0 parts, clay 5.0 parts, and a particle diameter 2.8 mm were prepared. The particle size of the obtained preparation was 88% in the range of 2.80 to 1.70 mm, the ratio of major axis / minor axis at the bottom was 1.2, and the number of particles per 1 g was 96.

[Example 7]
The pharmaceutical composition was 24.0 parts of kasugamycin (bactericidal active ingredient), 25.0 parts of shirasu balloon (average particle size of 90 to 120 μm) (floating carrier), 1.5 parts of sodium dialkylsuccinatesulfonate, and 3.0 parts of sodium polyacrylate. Parts, 3.0 parts of carboxymethylcellulose Na, 37.0 parts of diatomaceous earth, 6.5 parts of clay, and a particle size of 3.0 mm. The particle size of the obtained preparation was 87% in the range of 2.80 to 1.70 mm, and the ratio of major axis / minor axis at the bottom surface was 1.4, and the number of particles per 1 g was 110.

Example 8
The pharmaceutical composition was 24.0 parts of kasugamycin (a bactericidal active ingredient), 30.0 parts of shirasu balloon (average particle size of 90 to 120 μm) (floating carrier), 3.0 parts of sodium alkylnaphthalenesulfonate, acrylic-maleic acid copolymer A water-floating pesticide formulation was prepared according to Example 1 with 3.0 parts of Na, 3.0 parts of carboxymethylcellulose Na, 32.0 parts of pearlite, 5.0 parts of clay, and a particle diameter of 3.0 mm. The particle size of the obtained preparation was 96% in the range of 2.80 to 1.70 mm, the ratio of major axis / minor axis at the bottom was 1.2, and the number of particles per gram was 98.

[Example 9]
Formulation composition was 24.0 parts of kasugamycin (bactericidal active ingredient), 30.0 parts of shirasu balloon (average particle size of 90 to 120 μm) (floating carrier), 1.5 parts of sodium dialkylsuccinatesulfonate, acrylic acid-vinylsulfonic acid 2.0 parts of copolymer Na, 2.0 parts of carboxymethylcellulose Na, 34.5 parts of perlite, 6.0 parts of clay, and 2.8 mm in particle diameter were prepared, and a water-floating pesticide formulation was prepared according to Example 1. . The particle size of the obtained preparation was 97% in the range of 2.80 to 1.70 mm, and the ratio of major axis / minor axis at the bottom was 1.3, and the number of particles per 1 g was 87.

[Example 10]
The composition of the formulation is 24.0 parts of kasugamycin (bactericidal active ingredient), 30.0 parts of shirasu balloon (average particle size 70 to 90 μm) (floating carrier), 3.0 parts of sodium alkylnaphthalenesulfonate, and formaldehyde condensate of alkylnaphthalenesulfonic acid 3.0 parts of Na, 2.0 parts of acryl-methacrylic acid copolymer Na, 2.0 parts of carboxymethylcellulose Na, 28.5 parts of pearlite, 7.5 parts of clay, 2.8 mm in particle diameter, according to Example 1. Thus, a water-floating pesticide formulation was prepared. The particle size of the obtained preparation was 85% in the range of 2.80 to 1.70 mm, the ratio of major axis / minor axis at the bottom was 1.2, and the number of particles per 1 g was 76.

[Example 11]
The pharmaceutical composition was 24.0 parts of kasugamycin (bactericidal active ingredient), 30.0 parts of fly ash balloon (average particle diameter of 80 to 120 μm) (floating carrier), 1.5 parts of sodium dialkylsuccinatesulfonate, and partially desulfonated lignin. 3.0 parts of sodium sulfonate, 2.0 parts of sodium polyacrylate, 2.0 parts of carboxymethylcellulose Na, 10.0 parts of bentonite, 18.5 parts of perlite, 5.0 parts of white carbon, 4.0 parts of clay, particle size A water-floating pesticide formulation was prepared according to Example 1 with a thickness of 3.0 mm. The particle size of the obtained preparation was 87% in the range of 2.80 to 1.70 mm, and the ratio of major axis / minor axis at the bottom was 1.3, and the number of particles per gram was 93.

[Example 12]
The composition of the formulation was 24.0 parts of kasugamycin (bactericidal active ingredient), 30.0 parts of ceramic balloon (average particle diameter of 20 to 150 μm) (floating carrier), 3.0 parts of sodium alkylnaphthalenesulfonate, and Naphthalenesulfonic acid formaldehyde condensate Na3 2.0 parts, acrylic-vinyl sulfonic acid copolymer Na 2.0 parts, carboxymethyl cellulose Na 2.0 parts, bentonite 10.0 parts, diatomaceous earth 21.0 parts, clay 5.0 parts, and a particle size of 2.8 mm. A water-floating pesticide formulation was prepared according to Example 1. The particle size of the obtained preparation was 95% in the range of 2.80 to 1.70 mm, the ratio of major axis / minor axis at the bottom was 1.1, and the number of particles per 1 g was 85.

Example 13
The pharmaceutical composition was 24.0 parts of kasugamycin (bactericidal active ingredient), 2.0 parts of acrylonitrile resin balloon (average particle diameter of 20 to 40 μm) (floating carrier), 1.5 parts of sodium dialkylsuccinatesulfonate, and partially desulfonated lignin. Example 1 3.0 parts of sodium sulfonic acid, 2.0 parts of acrylic acid-maleic acid copolymer Na, 2.0 parts of carboxymethyl cellulose Na, 55.5 parts of diatomaceous earth, 10.0 parts of clay, and 3.0 mm in particle diameter. A water-floating pesticide formulation was prepared according to the standard. The particle size of the obtained preparation was 95% in the range of 2.80 to 1.70 mm, and the ratio of major axis / minor axis at the bottom was 1.3, and the number of particles per gram was 68.

[Example 14]
The pharmaceutical composition was 24.0 parts of kasugamycin (a bactericidal active ingredient), 30.0 parts of shirasu balloon (average particle diameter of 90 to 120 μm) (floating carrier), 3.0 parts of sodium alkylnaphthalenesulfonate, and condensate of alkylnaphthalenesulfonic acid formaldehyde. 3.0 parts of Na, 3.0 parts of acryl-vinylsulfonic acid copolymer Na, 2.0 parts of carboxymethylcellulose Na, 10.0 parts of bentonite, 22.0 parts of pearlite, 3.0 parts of clay, and a particle size of 2.8 mm. A water-floating pesticide formulation was prepared according to Example 1. The particle size of the obtained preparation was 88% in the range of 2.80 to 1.70 mm, and the ratio of major axis / minor axis at the bottom was 1.3, and the number of particles per 1 g was 111.

[Example 15]
The pharmaceutical composition was 24.0 parts of kasugamycin (bactericidal active ingredient), 30.0 parts of shirasu balloon (average particle size of 90 to 120 μm) (floating carrier), 1.5 parts of sodium dialkylsuccinatesulfonate, formaldehyde condensate of naphthalenesulfonic acid Na 3.0 parts, acrylic acid-methacrylic acid copolymer Na 3.0 parts, carboxymethyl cellulose Na 3.0 parts, bentonite 10.0 parts, perlite 10.0 parts, white carbon 7.5 parts, clay 8.0 parts, A water-susceptible pesticide formulation was prepared according to Example 1 with a particle diameter of 3.0 mm. The particle size of the obtained preparation was 86% in the range of 2.80 to 1.70 mm, and the ratio of major axis / minor axis at the bottom surface was 1.4, and the number of particles per 1 g was 105.

[Example 16]
Formulation composition was 24.0 parts of kasugamycin (bactericidal active ingredient), Shirasu balloon (average particle diameter 90 to 120 μm) (floating carrier) 30.0 parts, alkylnaphthalenesulfonic acid Na 3.0 parts, partially desulfonated ligninsulfonic acid Na 3.0 parts, acrylic-maleic acid copolymer Na 3.0 parts, carboxymethyl cellulose Na 3.0 parts, perlite 29.0 parts, clay 5.0 parts, particle size 3.0 mm. To prepare a water-floating pesticide formulation. The particle size of the obtained preparation was 94% in the range of 2.80 to 1.70 mm, and the ratio of major axis / minor axis at the bottom surface was 1.3, and the number of particles per 1 g was 121.

[Example 17]
The composition of the formulation was 24.0 parts of kasugamycin (bactericidal active ingredient), 30.0 parts of shirasu balloon (average particle diameter 90 to 120 μm) (floating carrier), 1.5 parts of sodium dialkylsuccinatesulfonate, and formaldehyde condensation of alkylnaphthalenesulfonic acid. The product surface was 3.0 parts, Na polyacrylate 3.0 parts, carboxymethylcellulose Na 3.0 parts, diatomaceous earth 30.5 parts, clay 5.0 parts, and a particle diameter of 2.8 mm. A pesticide formulation was prepared. The particle size of the obtained preparation was 93% in the range of 2.80 to 1.70 mm, and the ratio of major axis / minor axis at the bottom surface was 1.4, and the number of particles per 1 g was 83.

[Example 18]
12.0 parts of pymetrozine (insecticidally active ingredient), 25.0 parts of shirasu balloon (average particle size 70 to 90 μm) (floating carrier), 3.0 parts of sodium alkylnaphthalenesulfonate, 3.0 parts of polyvinyl alcohol, 47. 0 parts and 10.0 parts of clay were pulverized and mixed with a hammer mill (Sample Mill KIIW-1, manufactured by Dalton) to obtain a powder mixture. The obtained powder mixture was put into a double-arm kneader (KDHJ, manufactured by Dalton), and kneaded for 15 minutes after water addition. Next, this water-kneaded product was granulated by an extrusion granulator equipped with a basket type screen having a hole diameter of 3.0 mm. The obtained granules were pre-dried, sized with a drum type granulator, and dried with a fluidized bed drier. This was sieved at 3.35 mm to 2.00 mm to obtain a water-floating pesticide formulation. The particle size of the obtained preparation was 83% in the range of 2.80 to 1.70 mm, and the ratio of major axis / minor axis at the bottom surface was 1.3, and the number of particles per gram was 89.

[Example 19]
The formulation was composed of 12.0 parts of pymetrozine (insecticidally active ingredient), 25.0 parts of fly ash balloon (average particle size: 80 to 120 μm) (floating carrier), 1.5 parts of sodium dialkylsuccinatesulfonate, and 3.0 parts of carboxymethylcellulose Na. Parts, 48.5 parts of perlite, 10.0 parts of clay, 2.8 mm in particle diameter, and prepared a water-floating pesticide formulation according to Example 16. The particle size of the obtained preparation was 86% in the range of 2.80 to 1.70 mm, and the ratio of major axis / minor axis at the bottom surface was 1.4, and the number of particles per 1 g was 97.

[Example 20]
The formulation was composed of 12.0 parts of pymetrozine (an insecticidal active ingredient), 2.0 parts of an acrylonitrile resin balloon (average particle diameter: 20 to 40 μm) (floating carrier), 3.0 parts of sodium alkylnaphthalenesulfonate, and 3.0 parts of sodium polyacrylate. Parts, 2.0 parts of carboxymethylcellulose Na, 60.0 parts of perlite, 18.0 parts of clay, and a particle size of 3.0 mm, and a water-floating pesticide formulation was prepared according to Example 18. The particle size of the obtained preparation was 88% in the range of 2.80 to 1.70 mm, and the ratio of major axis / minor axis at the bottom surface was 1.3, and the number of particles per 1 g was 106.

[Example 21]
The formulation was composed of 12.0 parts of pymetrozine (insecticidally active ingredient), 30.0 parts of ceramic balloon (average particle size of 20 to 150 μm) (floating carrier), 3.0 parts of sodium alkylnaphthalenesulfonate, 2.0 parts of carboxymethylcellulose Na, Diatomaceous earth: 43.0 parts, clay: 10.0 parts, particle size: 3.0 mm, and a water-floating pesticide formulation was prepared according to Example 18. The particle size of the obtained preparation was 93% in the range of 2.80 to 1.70 mm, and the ratio of major axis / minor axis at the bottom surface was 1.4, and the number of particles per gram was 82.

[Example 22]
The formulation was composed of 12.0 parts of pymetrozine (active insecticide), 30.0 parts of shirasu balloon (average particle size 70 to 90 μm) (floating carrier), 1.5 parts of sodium dialkylsuccinatesulfonate, Example 18: 2.0 parts of polymer Na, 2.0 parts of carboxymethylcellulose Na, 10.0 parts of bentonite, 30.0 parts of pearlite, 5.0 parts of white carbon, 7.5 parts of clay, 2.8 mm in particle size A water-floating pesticide formulation was prepared in accordance with. The particle size of the obtained preparation was 96% in the range of 2.80 to 1.70 mm, and the ratio of major axis / minor axis at the bottom was 1.3, and the number of particles per gram was 88.

[Example 23]
Formulation composition was 12.0 parts of pymetrozine (insecticidally active ingredient), 30.0 parts of shirasu balloon (average particle size of 90 to 120 μm) (floating carrier), 3.0 parts of sodium alkylnaphthalenesulfonate, acrylic-methacrylic acid copolymer Based on Example 18, a water-floating pesticide formulation was prepared according to Example 18 with 2.0 parts of Na, 3.0 parts of carboxymethylcellulose Na, 40.0 parts of diatomaceous earth, 10.0 parts of clay, and a particle size of 2.8 mm. The particle size of the obtained preparation was 84% in the range of 2.80 to 1.70 mm, and the ratio of major axis / minor axis at the bottom surface was 1.4, and the number of particles per 1 g was 93.

[Example 24]
The formulation was composed of 12.0 parts of pymetrozine (insecticidally active ingredient), 30.0 parts of shirasu balloon (average particle size of 90 to 120 μm) (floating carrier), 1.5 parts of sodium dialkylsuccinatesulfonate, and 2.0 parts of sodium polyacrylate. Parts, 3.0 parts of carboxymethylcellulose Na, 45.0 parts of diatomaceous earth, 6.5 parts of clay, and a particle diameter of 3.0 mm. The particle size of the obtained preparation was 83% in the range of 2.80 to 1.70 mm, and the ratio of major axis / minor axis at the bottom was 1.3, and the number of particles per 1 g was 97.

[Example 25]
Formulation composition was 12.0 parts of pymetrozine (insecticidally active ingredient), 25.0 parts of shirasu balloon (average particle size of 90 to 120 μm) (floating carrier), 3.0 parts of sodium alkylnaphthalenesulfonate, acrylic-maleic acid copolymer A water-floating pesticide formulation was prepared according to Example 18 using 3.0 parts of Na, 2.0 parts of carboxymethylcellulose Na, 45.0 parts of perlite, 10.0 parts of clay, and a particle size of 3.0 mm. The particle size of the obtained preparation was 94% in the range of 2.80 to 1.70 mm, and the ratio of major axis / minor axis at the bottom surface was 1.4, and the number of particles per gram was 95.

[Example 26]
Formulation composition was 12.0 parts of pymetrozine (insecticidally active ingredient), 25.0 parts of shirasu balloon (average particle size of 90 to 120 μm) (floating carrier), 1.5 parts of dialkyl succinatesulfonic acid Na, acrylic acid-vinylsulfonic acid 3.0 parts of copolymer Na, 3.0 parts of carboxymethylcellulose Na, 48.5 parts of perlite, 7.0 parts of clay, and 2.8 mm in particle diameter were prepared, and a water-floating pesticide formulation was prepared according to Example 18. . The particle size of the obtained preparation was 97% in the range of 2.80 to 1.70 mm, and the ratio of major axis / minor axis at the bottom surface was 1.4, and the number of particles per 1 g was 107.

[Example 27]
Formulation composition is 12.0 parts of pymetrozine (insecticidally active ingredient), 28.0 parts of shirasu balloon (average particle diameter 70 to 90 μm) (floating carrier), 3.0 parts of sodium alkylnaphthalenesulfonate, formaldehyde condensate of alkylnaphthalenesulfonic acid Na 3.0 parts, acrylic-methacrylic acid copolymer Na 3.0 parts, carboxymethylcellulose Na 3.0 parts, perlite 38.0 parts, clay 10.0 parts, particle size 2.8 mm Thus, a water-floating pesticide formulation was prepared. The particle size of the obtained preparation was 83% in the range of 2.80 to 1.70 mm, and the ratio of major axis / minor axis at the bottom surface was 1.4, and the number of particles per gram was 91.

[Example 28]
Formulation composition was 12.0 parts of pymetrozine (insecticidally active ingredient), 28.0 parts of fly ash balloon (average particle diameter: 80 to 120 μm) (floating carrier), 1.5 parts of sodium dialkylsuccinatesulfonate, partially desulfonated lignin 3.0 parts of sodium sulfonic acid, 3.0 parts of sodium polyacrylate, 2.0 parts of carboxymethylcellulose Na, 10.0 parts of bentonite, 30.0 parts of perlite, 5.0 parts of white carbon, 5.5 parts of clay, particle size 3.0 mm and a water-floating pesticide formulation was prepared according to Example 18. The particle size of the obtained preparation was 87% in the range of 2.80 to 1.70 mm, and the ratio of major axis / minor axis at the bottom was 1.3, and the number of particles per gram was 83.

[Example 29]
Formulation composition was 12.0 parts of pymetrozine (insecticidally active ingredient), 25.0 parts of ceramic balloon (average particle size of 20 to 150 μm) (floating carrier), 3.0 parts of sodium alkylnaphthalenesulfonate, and Naphthalenesulfonic acid formaldehyde condensate Na3 2.0 parts, 3.0 parts of acryl-vinylsulfonic acid copolymer Na, 3.0 parts of carboxymethylcellulose Na, 10.0 parts of bentonite, 36.0 parts of diatomaceous earth, 5.0 parts of clay, and 2.8 mm in particle diameter. A water-floating pesticide formulation was prepared according to Example 18. The particle size of the obtained preparation was 98% in the range of 2.80 to 1.70 mm, and the ratio of major axis / minor axis at the bottom surface was 1.4, and the number of particles per 1 g was 86.

[Example 30]
Formulation composition was 12.0 parts of pymetrozine (insecticidally active ingredient), 2.0 parts of acrylonitrile resin balloon (average particle size: 20 to 40 μm) (floating carrier), 1.5 parts of sodium dialkylsuccinatesulfonate, partially desulfonated lignin 3.0 parts of sodium sulfonic acid, 2.0 parts of acrylic acid-maleic acid copolymer Na, 2.0 parts of carboxymethylcellulose Na, 35.0 parts of perlite, 35.0 parts of diatomaceous earth, 7.5 parts of clay, particle size: 3. 0 mm, and a water-floating pesticide formulation was prepared according to Example 18. The particle size of the obtained preparation was 93% in the range of 2.80 to 1.70 mm, and the ratio of major axis / minor axis at the bottom was 1.3, and the number of particles per gram was 95.

[Example 31]
Formulation composition was 12.0 parts of pymetrozine (insecticidal active ingredient), 28.0 parts of shirasu balloon (average particle size of 90 to 120 μm) (floating carrier), 3.0 parts of sodium alkylnaphthalenesulfonate, and condensate of alkylnaphthalenesulfonic acid formaldehyde 3.0 parts of Na, 3.0 parts of acryl-vinylsulfonic acid copolymer Na, 2.0 parts of carboxymethylcellulose Na, 10.0 parts of bentonite, 30.0 parts of pearlite, 9.0 parts of clay, and 2.8 mm in particle diameter. A water-floating pesticide formulation was prepared according to Example 18. The particle size of the obtained preparation was 84% in the range of 2.80 to 1.70 mm, and the ratio of major axis / minor axis at the bottom surface was 1.4, and the number of particles per 1 g was 108.

[Example 32]
Formulation composition is 12.0 parts of pymetrozine (insecticidally active ingredient), 30.0 parts of shirasu balloon (average particle size of 90 to 120 μm) (floating carrier), 1.5 parts of sodium dialkylsuccinatesulfonate, formaldehyde condensate of naphthalenesulfonic acid Na 3.0 parts, acrylic acid-methacrylic acid copolymer Na 3.0 parts, carboxymethyl cellulose Na 2.0 parts, bentonite 10.0 parts, perlite 19.5 parts, white carbon 15.0 parts, clay 4.0 parts, A water-susceptible pesticide formulation was prepared according to Example 18 with a particle diameter of 3.0 mm. The particle size of the obtained preparation was 83% in the range of 2.80 to 1.70 mm, the ratio of major axis / minor axis at the bottom was 1.2, and the number of particles per 1 g was 90.

[Example 33]
Formulation composition was 12.0 parts of pymetrozine (insecticidally active ingredient), 30.0 parts of shirasu balloon (average particle size of 90 to 120 μm) (floating carrier), 3.0 parts of sodium alkylnaphthalenesulfonic acid, and partially desulfonated ligninsulfonic acid 3.0 parts of Na, 2.0 parts of acrylic-maleic acid copolymer Na, 2.0 parts of carboxymethylcellulose Na, 40.0 parts of pearlite, 8.0 parts of clay, and 3.0 mm in particle diameter. Thus, a water-floating pesticide formulation was prepared. The particle size of the obtained preparation was 95% in the range of 2.80 to 1.70 mm, and the ratio of major axis / minor axis at the bottom surface was 1.4, and the number of particles per gram was 88.

[Example 34]
Formulation composition was 12.0 parts of pymetrozine (insecticidally active ingredient), 30.0 parts of shirasu balloon (average particle diameter 90 to 120 μm) (floating carrier), 1.5 parts of sodium dialkylsuccinatesulfonate, formaldehyde condensation of alkylnaphthalenesulfonic acid Product Na 3.0 parts, sodium polyacrylate 2.0 parts, carboxymethylcellulose Na 2.0 parts, diatomaceous earth 44.5 parts, clay 5.0 parts, particle diameter 2.8 mm, and floating on the water surface according to Example 18. A pesticide formulation was prepared. The particle size of the obtained preparation was 96% in the range of 2.80 to 1.70 mm, the ratio of major axis / minor axis at the bottom was 1.2, and the number of particles per 1 g was 99.

[Example 35]
After mixing 10.0 parts of ipfencarbazone (herbicidally active ingredient), 1.0 part of sodium alkylnaphthalenesulfonate, and 14.0 parts of water, the average particle diameter becomes 1.0 μm with Dynomill (manufactured by Shinmaru Enterprises). To obtain a slurry. Further, 25.0 parts of a shirasu balloon (average particle diameter 70 to 90 μm) (floating carrier), 2.0 parts of sodium alkylnaphthalenesulfonate, 2.0 parts of polyvinyl alcohol, 5.0 parts of bentonite, 42.0 parts of pearlite, 13.0 parts of the clay was pulverized and mixed with a hammer mill (Sample Mill KIIW-1, manufactured by Dalton) to obtain a powder mixture. The obtained slurry and powder mixture were put into a double-arm kneader (KDHJ, manufactured by Dalton) and kneaded for 15 minutes after adding water. Next, this water-kneaded product was granulated by an extrusion granulator equipped with a basket type screen having a hole diameter of 3.0 mm. The obtained granules were pre-dried, sized with a drum type granulator, and dried with a fluidized bed drier. This was sieved at 3.35 mm to 2.00 mm to obtain a water-floating pesticide formulation. The particle size of the obtained preparation was 84% in the range of 2.80 to 1.70 mm, and the ratio of major axis / minor axis at the bottom surface was 1.4, and the number of particles per 1 g was 109.

[Example 36]
Formulation composition is ipfencarbazone 10.0 parts (herbicidal active ingredient), fly ash balloon (average particle diameter 80 to 120 μm) (floating carrier) 28.0 parts, dialkyl succinate sulfonate Na 1.5 parts, carboxymethyl cellulose 2.0 parts of Na, 51.5 parts of perlite, 7.0 parts of clay (of which the composition used for the slurry was 10.0 parts of ipfencarbazone, 1.0 part of sodium dialkylsuccinatesulfonate, 14.0 parts of water) The particle size was 2.8 mm, and a water-floating pesticide formulation was prepared according to Example 35. The particle size of the obtained preparation was 86% in the range of 2.80 to 1.70 mm, the ratio of major axis / minor axis at the bottom was 1.2, and the number of particles per gram was 115.

[Example 37]
Formulation composition is ipfencarbazone 10.0 parts (herbicidal active ingredient), acrylonitrile resin balloon (average particle size 20 to 40 μm) (floating carrier) 2.0 parts, alkylnaphthalenesulfonic acid Na 3.0 parts, polyacrylic acid 2.0 parts of Na, 3.0 parts of carboxymethylcellulose Na, 70.0 parts of perlite, 10.0 parts of clay (of which the composition used for the slurry was 10.0 parts of ipfencarbazone, 1.0 part of alkylnaphthalenesulfonic acid Na, (14.0 parts of water), the particle size was 3.0 mm, and a pesticide formulation having a water-floating surface was prepared according to Example 35. The particle size of the obtained preparation was 88% in the range of 2.80 to 1.70 mm, the ratio of major axis / minor axis at the bottom was 1.2, and the number of particles per 1 g was 123.

[Example 38]
The formulation composition was 10.0 parts of ipfencarbazone (herbicidally active ingredient), 28.0 parts of ceramic balloon (average particle size of 20 to 150 μm) (floating carrier), 3.0 parts of sodium alkylnaphthalenesulfonate, and Na2 of polyacrylate. 2.0 parts, carboxymethylcellulose Na 3.0 parts, diatomaceous earth 48.0 parts, clay 8.0 parts (of which the composition used for the slurry was ipfencarbazone 10.0 parts, alkylnaphthalenesulfonic acid Na 1.0 parts, water 14.0 parts), the particle size was 3.0 mm, and a water-floating pesticide formulation was prepared according to Example 35. The particle size of the obtained preparation was 92% in the range of 2.80 to 1.70 mm, and the ratio of major axis / minor axis at the bottom surface was 1.3, and the number of particles per 1 g was 103.

[Example 39]
The formulation composition was 10.0 parts of ipfencarbazone (herbicidally active ingredient), 25.0 parts of shirasu balloon (average particle size 70 to 90 μm) (floating carrier), 1.5 parts of sodium dialkylsuccinatesulfonate, acrylic acid- Maleic acid copolymer Na 2.0 parts, carboxymethyl cellulose Na 3.0 parts, bentonite 10.0 parts, perlite 33.5 parts, white carbon 10.0 parts, clay 5.0 parts (of which the composition used for the slurry is 10.0 parts of ipfencarbazone, 1.0 part of sodium dialkylsuccinatesulfonate, 14.0 parts of water) and a particle diameter of 2.8 mm were prepared according to Example 35 to prepare a water-floating pesticide formulation. The particle size of the obtained preparation was 95% in the range of 2.80 to 1.70 mm, and the ratio of major axis / minor axis at the bottom surface was 1.4, and the number of particles per 1 g was 100.

[Example 40]
The pharmaceutical composition was 10.0 parts of ipfencarbazone (herbicidally active ingredient), 30.0 parts of shirasu balloon (average particle size of 90 to 120 μm) (floating carrier), 3.0 parts of sodium alkylnaphthalenesulfonate, acrylic-methacrylic acid 2.0 parts of copolymer Na, 2.0 parts of carboxymethylcellulose Na, 43.0 parts of diatomaceous earth, 10.0 parts of clay (of which the composition used for the slurry was 10.0 parts of ipfencarbazone, 1 part of alkylnaphthalenesulfonic acid Na1. 0 parts, water 14.0 parts) and a particle size of 2.8 mm, and a water-floating pesticide formulation was prepared according to Example 35. The particle size of the obtained preparation was 87% in the range of 2.80 to 1.70 mm, the ratio of major axis / minor axis at the bottom was 1.1, and the number of particles per 1 g was 123.

[Example 41]
Formulation composition is ipfencarbazone 10.0 parts (herbicidal active ingredient), Shirasu balloon (average particle size 90 to 120 μm) (floating carrier) 25.0 parts, dialkyl succinate sulfonate Na 1.5 parts, polyacrylic acid 3.0 parts of Na, 3.0 parts of carboxymethylcellulose Na, 50.0 parts of diatomaceous earth, 7.5 parts of clay (of which the composition used for the slurry is 10.0 parts of ipfencarbazone, 1.0 part of dialkyl succinatesulfonic acid Na) , Water 14.0 parts) and a particle size of 3.0 mm, and a water-floating pesticide formulation was prepared according to Example 35. The particle size of the obtained preparation was 84% in the range of 2.80 to 1.70 mm, and the ratio of major axis / minor axis at the bottom surface was 1.3, and the number of particles per gram was 109.

[Example 42]
The pharmaceutical composition was 10.0 parts of ipfencarbazone (herbicidally active ingredient), 30.0 parts of shirasu balloon (average particle size of 90 to 120 μm) (floating carrier), 3.0 parts of sodium alkylnaphthalenesulfonate, acrylic-maleic acid 3.0 parts of copolymer Na, 2.0 parts of carboxymethylcellulose Na, 45.0 parts of pearlite, 7.0 parts of clay (of which the composition used for the slurry was 10.0 parts of ipfencarbazone, Na1 of alkylnaphthalenesulfonic acid). (0 parts, water 14.0 parts), the particle size was 3.0 mm, and a water-floating pesticide formulation was prepared according to Example 35. The particle size of the obtained preparation was 96% in the range of 2.80 to 1.70 mm, and the ratio of major axis / minor axis at the bottom surface was 1.3, and the number of particles per gram was 103.

[Example 43]
The formulation was composed of 10.0 parts of ipfencarbazone (herbicidal active ingredient), 28.0 parts of shirasu balloon (average particle size of 90 to 120 μm) (floating carrier), 1.5 parts of sodium dialkylsuccinatesulfonate, acrylic acid- Vinyl sulfonic acid copolymer Na 3.0 parts, carboxymethyl cellulose Na 3.0 parts, perlite 50.0 parts, clay 4.5 parts (of which the composition used for the slurry was 10.0 parts of ipfencarbazone, dialkyl succinate (1.0 part of sodium sulfonate, 14.0 parts of water) and a particle size of 2.8 mm, and a water-floating pesticide formulation was prepared according to Example 35. The particle size of the obtained preparation was 95% in the range of 2.80 to 1.70 mm, the ratio of major axis / minor axis at the bottom was 1.2, and the number of particles per gram was 126.

[Example 44]
Formulation composition is 10.0 parts of ipfencarbazone (herbicidally active ingredient), 28.0 parts of shirasu balloon (average particle diameter of 70 to 90 μm) (floating carrier), 3.0 parts of sodium alkylnaphthalenesulfonic acid, and alkylnaphthalenesulfonic acid 3.0 parts of formaldehyde condensate Na, 3.0 parts of acryl-methacrylic acid copolymer Na, 2.0 parts of carboxymethylcellulose Na, 46.0 parts of perlite, 5.0 parts of clay (of which the composition used for the slurry was ipfencarba) 10.0 parts of zon, 1.0 part of sodium alkylnaphthalenesulfonate, 14.0 parts of water), the particle size was 2.8 mm, and a water-floating pesticide formulation was prepared according to Example 35. The particle size of the obtained preparation was 86% in the range of 2.80 to 1.70 mm, the ratio of major axis / minor axis at the bottom was 1.2, and the number of particles per 1 g was 113.

[Example 45]
The formulation was 10.0 parts of ipfencarbazone (herbicidally active ingredient), 28.0 parts of fly ash balloon (average particle diameter of 80 to 120 μm) (floating carrier), 1.5 parts of sodium dialkylsuccinatesulfonate, and 3.0 parts of sodium sulfonated lignin sulfonic acid, 2.0 parts of sodium polyacrylate, 2.0 parts of carboxymethyl cellulose Na, 10.0 parts of bentonite, 20.0 parts of pearlite, 15.0 parts of white carbon, 8.5 parts of clay ( Among them, the composition used for the slurry was 10.0 parts of ipfencarbazone, 1.0 part of dialkylsuccinatesulfonate, 14.0 parts of water), the particle size was 3.0 mm, and the water surface was determined according to Example 35. A floating pesticide formulation was prepared. The particle size of the obtained preparation was 84% in the range of 2.80 to 1.70 mm, and the ratio of major axis / minor axis at the bottom surface was 1.4, and the number of particles per 1 g was 99.

[Example 46]
The formulation was 10.0 parts of ipfencarbazone (herbicidally active ingredient), 28.0 parts of ceramic balloon (average particle size of 20 to 150 μm) (floating carrier), 3.0 parts of sodium alkylnaphthalenesulfonate, and formaldehyde naphthalenesulfonate Condensate Na 3.0 parts, acrylic-vinyl sulfonic acid copolymer Na 2.0 parts, carboxymethyl cellulose Na 3.0 parts, bentonite 10.0 parts, diatomaceous earth 38.0 parts, clay 6.0 parts (used in slurry The composition was 10.0 parts of ipfencarbazone, 1.0 part of sodium alkylnaphthalenesulfonate, 14.0 parts of water), the particle size was 2.8 mm, and a water-floating pesticide formulation was prepared according to Example 35. did. The particle size of the obtained preparation was 96% in the range of 2.80 to 1.70 mm, the ratio of major axis / minor axis at the bottom was 1.1, and the number of particles per 1 g was 108.

[Example 47]
The pharmaceutical composition was 10.0 parts of ipfencarbazone (herbicidally active ingredient), 2.0 parts of acrylonitrile resin balloon (average particle diameter of 20 to 40 μm) (floating carrier), 1.5 parts of sodium dialkylsuccinatesulfonate, 1.5 parts of 3.0 parts of sodium sulfonated ligninsulfonic acid, 2.0 parts of acrylic acid-maleic acid copolymer Na, 2.0 parts of carboxymethylcellulose Na, 10.0 parts of perlite, 61.5 parts of diatomaceous earth, 8.0 parts of clay (including slurry) The composition used was 10.0 parts of ipfencarbazone, 1.0 part of sodium dialkylsuccinatesulfonate, 14.0 parts of water), and the particle size was 3.0 mm. A pesticide formulation was prepared. The particle size of the obtained preparation was 93% in the range of 2.80 to 1.70 mm, and the ratio of major axis / minor axis at the bottom surface was 1.4, and the number of particles per 1 g was 103.

[Example 48]
Formulation composition is ipfencarbazone 10.0 parts (herbicidal active ingredient), Shirasu balloon (average particle size 90 to 120 μm) (floating carrier) 25.0 parts, alkyl naphthalene sulfonic acid Na 3.0 parts, alkyl naphthalene sulfonic acid 3.0 parts of formaldehyde condensate Na, 2.0 parts of acryl-vinylsulfonic acid copolymer Na, 3.0 parts of carboxymethylcellulose Na, 10.0 parts of bentonite, 38.0 parts of perlite, 6.0 parts of clay (including slurry) The composition thus obtained was 10.0 parts of ipfencarbazone, 1.0 part of sodium alkylnaphthalenesulfonate, 14.0 parts of water), the particle size was 2.8 mm, and the pesticide formulation having a water-floating surface was prepared according to Example 35. Prepared. The particle size of the obtained preparation was 84% in the range of 2.80 to 1.70 mm, the ratio of major axis / minor axis at the bottom was 1.2, and the number of particles per 1 g was 113.

[Example 49]
Formulation composition is ipfencarbazone 10.0 parts (herbicidal active ingredient), shirasu balloon (average particle diameter 90 to 120 μm) (floating carrier) 28.0 parts, dialkyl succinate sulfonic acid Na 1.5 parts, naphthalene sulfonic acid Formaldehyde condensate Na 3.0 parts, acrylic acid-methacrylic acid copolymer Na 2.0 parts, carboxymethyl cellulose Na 3.0 parts, bentonite 10.0 parts, perlite 25.0 parts, white carbon 10.0 parts, clay 7. 5 parts (of which the composition used for the slurry was 10.0 parts of ipfencarbazone, 1.0 part of sodium dialkylsuccinatesulfonate, 14.0 parts of water), and the particle size was 3.0 mm. Thus, a water-floating pesticide formulation was prepared. The particle size of the obtained preparation was 83% in the range of 2.80 to 1.70 mm, the ratio of major axis / minor axis at the bottom was 1.1, and the number of particles per 1 g was 96.

[Example 50]
The pharmaceutical composition was 10.0 parts of ipfencarbazone (herbicidally active ingredient), 25.0 parts of shirasu balloon (average particle size of 90 to 120 μm) (floating carrier), 3.0 parts of sodium alkylnaphthalenesulfonate, and partially desulfonated. Lignin sulfonic acid Na 3.0 parts, acrylic-maleic acid copolymer Na 3.0 parts, carboxymethyl cellulose Na 2.0 parts, perlite 45.0 parts, clay 9.0 parts (of which the composition used for the slurry was ipfencarba) (10.0 parts of zon, 1.0 part of sodium alkylnaphthalenesulfonate, 14.0 parts of water), the particle size was 3.0 mm, and a water-floating pesticide formulation was prepared according to Example 35. The particle size of the obtained preparation was 94% in the range of 2.80 to 1.70 mm, and the ratio of major axis / minor axis at the bottom surface was 1.3, and the number of particles per 1 g was 97.

[Example 51]
Formulation composition was 10.0 parts of ipfencarbazone (herbicidally active ingredient), 28.0 parts of shirasu balloon (average particle size of 90 to 120 μm) (floating carrier), 1.5 parts of sodium dialkylsuccinatesulfonate, alkylnaphthalenesulfone Acid formaldehyde condensate Na 3.0 parts, polyacrylic acid Na 3.0 parts, carboxymethylcellulose Na 3.0 parts, diatomaceous earth 48.0 parts, clay 3.5 parts (the composition used for the slurry was ipfencarbazone 10.3). 0 part, 1.0 part of sodium dialkylsuccinatesulfonate, 14.0 parts of water), and the particle size was 2.8 mm. The particle size of the obtained preparation was 97% in the range of 2.80 to 1.70 mm, the ratio of major axis / minor axis at the bottom was 1.2, and the number of particles per 1 g was 90.

[Example 52]
12.0 parts of simetryn (herbicidal active ingredient), 30.0 parts of shirasu balloon (average particle diameter 70 to 90 μm) (floating carrier), 3.0 parts of sodium alkylnaphthalenesulfonate, 5.0 parts of dextrin, 10.0 parts of bentonite Parts, 38.0 parts of pearlite and 2.0 parts of clay were pulverized and mixed with a hammer mill (Sample Mill KIIW-1, manufactured by Dalton) to obtain a powder mixture. The obtained powder mixture was put into a double-arm kneader (KDHJ, manufactured by Dalton), and kneaded for 15 minutes after water addition. Next, this water-kneaded product was granulated by an extrusion granulator equipped with a basket type screen having a hole diameter of 3.0 mm. The obtained granules were pre-dried, sized with a drum type granulator, and dried with a fluidized bed drier. This was sieved at 3.35 mm to 2.00 mm to obtain a water-floating pesticide formulation. The particle size of the obtained preparation was 83% in the range of 2.80 to 1.70 mm, and the ratio of major axis / minor axis at the bottom surface was 1.4, and the number of particles per gram was 93.

[Example 53]
The formulation was composed of 12.0 parts of simethrin (herbicidal active ingredient), 28.0 parts of fly ash balloon (average particle diameter of 80 to 120 μm) (floating carrier), 1.5 parts of sodium dialkylsuccinatesulfonate, and 3.0 parts of carboxymethyl cellulose Na. Parts, 43.0 parts of perlite, 12.5 parts of clay, 2.8 mm in particle diameter, and a water-floating pesticide formulation was prepared according to Example 50. The particle size of the obtained preparation was 85% in the range of 2.80 to 1.70 mm, the ratio of major axis / minor axis at the bottom was 1.2, and the number of particles per gram was 88.

[Example 54]
The formulation was composed of 12.0 parts of simetryn (herbicidal active ingredient), 2.0 parts of acrylonitrile resin balloon (average particle diameter of 20 to 40 μm) (floating carrier), 3.0 parts of sodium alkylnaphthalenesulfonate and 2.0 parts of sodium polyacrylate. Parts, 2.0 parts of carboxymethylcellulose Na, 65.0 parts of pearlite, 14.0 parts of clay, and a particle diameter of 3.0 mm. The particle size of the obtained preparation was 87% in the range of 2.80 to 1.70 mm, and the ratio of major axis / minor axis at the bottom surface was 1.4, and the number of particles per 1 g was 97.

[Example 55]
The formulation was composed of 12.0 parts of simetryn (herbicidal active ingredient), 28.0 parts of ceramic balloon (average particle size of 20 to 150 μm) (floating carrier), 3.0 parts of sodium alkylnaphthalenesulfonate, 3.0 parts of carboxymethylcellulose Na, Diatomaceous earth was 45.0 parts, clay was 9.0 parts, and the particle size was 3.0 mm. A water-floating pesticide formulation was prepared according to Example 52. The particle size of the obtained preparation was 93% in the range of 2.80 to 1.70 mm, and the ratio of major axis / minor axis at the bottom surface was 1.3, and the number of particles per 1 g was 96.

[Example 56]
Formulation composition was 12.0 parts of simetryn (herbicidal active ingredient), 28.0 parts of shirasu balloon (average particle size 70 to 90 μm) (floating carrier), 1.5 parts of sodium dialkylsuccinatesulfonate, and 1.5 parts of acrylic acid-maleic acid. Example 52: Polymer Na 2.0 parts, carboxymethylcellulose Na 3.0 parts, bentonite 10.0 parts, pearlite 30.0 parts, white carbon 8.0 parts, clay 5.5 parts, particle size 2.8 mm A water-floating pesticide formulation was prepared in accordance with. The particle size of the obtained preparation was 96% in the range of 2.80 to 1.70 mm, and the ratio of major axis / minor axis at the bottom surface was 1.4, and the number of particles per gram was 108.

[Example 57]
Formulation composition was 12.0 parts of simetryn (herbicidally active ingredient), 28.0 parts of shirasu balloon (average particle size of 90 to 120 μm) (floating carrier), 3.0 parts of sodium alkylnaphthalenesulfonate, acrylic-methacrylic acid copolymer Based on Example 52, 2.0 parts of Na, 3.0 parts of carboxymethyl cellulose, 47.0 parts of diatomaceous earth, 5.0 parts of clay, and a particle size of 2.8 mm were prepared. The particle size of the obtained preparation was 87% in the range of 2.80 to 1.70 mm, the ratio of major axis / minor axis at the bottom was 1.2, and the number of particles per 1 g was 95.

[Example 58]
The formulation was composed of 12.0 parts of simetryn (herbicidal active ingredient), 30.0 parts of shirasu balloon (average particle size of 90 to 120 μm) (floating carrier), 1.5 parts of sodium dialkylsuccinatesulfonate, and 3.0 parts of sodium polyacrylate. Parts, 3.0 parts of carboxymethylcellulose Na, 45.0 parts of diatomaceous earth, 5.5 parts of clay, and a particle diameter of 3.0 mm, and a water-floating pesticide formulation was prepared according to Example 52. The particle size of the obtained preparation was 84% in the range of 2.80 to 1.70 mm, and the ratio of major axis / minor axis at the bottom surface was 1.4, and the number of particles per 1 g was 97.

[Example 59]
Formulation composition was 12.0 parts of simetryn (herbicidally active ingredient), Shirasu balloon (average particle diameter of 90 to 120 μm) (floating carrier) 30.0 parts, Na of alkylnaphthalenesulfonic acid 3.0 parts, acrylic-maleic acid copolymer 3.0 parts of Na, 2.0 parts of carboxymethylcellulose Na, 46.0 parts of pearlite, 4.0 parts of clay, and 3.0 mm in particle diameter were prepared, and a water-floating pesticide formulation was prepared in accordance with Example 52. The particle size of the obtained preparation was 96% in the range of 2.80 to 1.70 mm, the ratio of major axis / minor axis at the bottom was 1.2, and the number of particles per 1 g was 93.

[Example 60]
Formulation composition was 12.0 parts of simetryn (herbicidal active ingredient), 30.0 parts of shirasu balloon (average particle size of 90 to 120 μm) (floating carrier), 1.5 parts of sodium dialkylsuccinatesulfonate, acrylic acid-vinylsulfonic acid 2.0 parts of copolymer Na, 2.0 parts of carboxymethylcellulose Na, 47.5 parts of perlite, 5.0 parts of clay, and 2.8 mm in particle diameter were prepared, and a water-floating pesticide formulation was prepared according to Example 52. . The particle size of the obtained preparation was 94% in the range of 2.80 to 1.70 mm, and the ratio of major axis / minor axis at the bottom surface was 1.4, and the number of particles per 1 g was 98.

[Example 61]
Formulation composition: 12.0 parts of simetryn (herbicidal active ingredient), 30.0 parts of shirasu balloon (average particle diameter 70 to 90 μm) (floating carrier), 3.0 parts of sodium alkylnaphthalenesulfonic acid, formaldehyde condensate of alkylnaphthalenesulfonic acid 3.0 parts of Na, 2.0 parts of acryl-methacrylic acid copolymer Na, 2.0 parts of carboxymethylcellulose Na, 40.0 parts of pearlite, 8.0 parts of clay, and 2.8 mm in particle diameter. To prepare a water-floating pesticide formulation. The particle size of the obtained preparation was 84% in the range of 2.80 to 1.70 mm, and the ratio of major axis / minor axis at the bottom surface was 1.3, and the number of particles per 1 g was 108.

[Example 62]
Formulation composition was 12.0 parts of simetryn (herbicidally active ingredient), 28.0 parts of fly ash balloon (average particle diameter of 80 to 120 μm) (floating carrier), 1.5 parts of sodium dialkylsuccinatesulfonate, and partially desulfonated lignin. 3.0 parts of sodium sulfonic acid, 3.0 parts of sodium polyacrylate, 2.0 parts of carboxymethylcellulose Na, 10.0 parts of bentonite, 25.0 parts of pearlite, 10.0 parts of white carbon, 5.5 parts of clay, particle size 3.0 mm and a water-floating pesticide formulation was prepared according to Example 52. The particle size of the obtained preparation was 83% in the range of 2.80 to 1.70 mm, and the ratio of major axis / minor axis at the bottom surface was 1.4, and the number of particles per 1 g was 100.

[Example 63]
Formulation composition was 12.0 parts of simetryn (herbicidal active ingredient), 30.0 parts of ceramic balloon (average particle diameter of 20 to 150 μm) (floating carrier), 3.0 parts of sodium alkylnaphthalenesulfonate, and Naphthalenesulfonic acid formaldehyde condensate Na3 2.0 parts, 3.0 parts of acrylic-vinyl sulfonic acid copolymer Na, 2.0 parts of carboxymethyl cellulose Na, 10.0 parts of bentonite, 30.0 parts of diatomaceous earth, 7.0 parts of clay, and a particle size of 2.8 mm. A water-floating pesticide formulation was prepared according to Example 52. The particle size of the obtained preparation was 95% in the range of 2.80 to 1.70 mm, the ratio of major axis / minor axis at the bottom was 1.2, and the number of particles per 1 g was 97.

[Example 64]
Formulation composition was 12.0 parts of simetryn (herbicidal active ingredient), acrylonitrile resin balloon (average particle size 20 to 40 μm) (floating carrier) 2.0 parts, dialkyl succinate sulfonate Na 1.5 parts, partially desulfonated lignin Example 52: 3.0 parts of sodium sulfonic acid, 2.0 parts of acrylic acid-maleic acid copolymer Na, 2.0 parts of carboxymethylcellulose Na, 67.5 parts of diatomaceous earth, 10.0 parts of clay, and a particle size of 3.0 mm A water-floating pesticide formulation was prepared according to the standard. The particle size of the obtained preparation was 94% in the range of 2.80 to 1.70 mm, the ratio of major axis / minor axis at the bottom was 1.2, and the number of particles per 1 g was 96.

[Example 65]
Formulation composition: 12.0 parts of simethrin (herbicidal active ingredient), 30.0 parts of shirasu balloon (average particle size: 90 to 120 μm) (floating carrier), 3.0 parts of sodium alkylnaphthalenesulfonic acid, formaldehyde condensate of alkylnaphthalenesulfonic acid 3.0 parts of Na, 3.0 parts of acryl-vinylsulfonic acid copolymer Na, 2.0 parts of carboxymethylcellulose Na, 10.0 parts of bentonite, 30.0 parts of pearlite, 7.0 parts of clay, and 2.8 mm in particle diameter. A water-floating pesticide formulation was prepared according to Example 52. The particle size of the obtained preparation was 86% in the range of 2.80 to 1.70 mm, and the ratio of major axis / minor axis at the bottom surface was 1.4, and the number of particles per 1 g was 93.

[Example 66]
Formulation composition is 12.0 parts of simetryn (herbicidally active ingredient), 30.0 parts of shirasu balloon (average particle size of 90 to 120 μm) (floating carrier), 1.5 parts of sodium dialkylsuccinatesulfonate, formaldehyde condensate of naphthalenesulfonic acid 3.0 parts of Na, 2.0 parts of acrylic acid-methacrylic acid copolymer Na, 2.0 parts of carboxymethyl cellulose Na, 10.0 parts of bentonite, 20.0 parts of pearlite, 15.0 parts of white carbon, 4.5 parts of clay, A water-susceptible pesticide formulation was prepared according to Example 52 with a particle diameter of 3.0 mm. The particle size of the obtained preparation was 83% in the range of 2.80 to 1.70 mm, and the ratio of major axis / minor axis at the bottom surface was 1.4, and the number of particles per 1 g was 101.

[Example 67]
Formulation composition was 12.0 parts of simethrin (herbicidal active ingredient), 30.0 parts of shirasu balloon (average particle diameter of 90 to 120 μm) (floating carrier), 3.0 parts of sodium alkylnaphthalenesulfonic acid, and partially desulfonated ligninsulfonic acid. 3.0 parts of Na, 3.0 parts of acrylic-maleic acid copolymer Na, 3.0 parts of carboxymethylcellulose Na, 39.0 parts of pearlite, 7.0 parts of clay, and 3.0 mm in particle diameter. Thus, a water-floating pesticide formulation was prepared. The particle size of the obtained preparation was 93% in the range of 2.80 to 1.70 mm, the ratio of major axis / minor axis at the bottom was 1.1, and the number of particles per 1 g was 94.

[Example 68]
12.0 parts of simethrin (herbicidal active ingredient), 25.0 parts of shirasu balloon (average particle diameter 90 to 120 μm) (floating carrier), 1.5 parts of sodium dialkylsuccinatesulfonate, formaldehyde condensation of alkylnaphthalenesulfonic acid Product Na 3.0 parts, polyacrylic acid Na 2.0 parts, carboxymethylcellulose Na 3.0 parts, diatomaceous earth 48.5 parts, clay 5.0 parts, particle diameter 2.8 mm. A pesticide formulation was prepared. The particle size of the obtained preparation was 97% in the range of 2.80 to 1.70 mm, the ratio of major axis / minor axis at the bottom was 1.2, and the number of particles per gram was 98.

[Example 69]
Benfresate 18.0 parts (herbicidal active ingredient), shirasu balloon (average particle size 70 to 90 μm) (floating carrier) 30.0 parts, alkylnaphthalenesulfonic acid Na 3.0 parts, dextrin 3.0 parts, polyvinyl alcohol 1. 0 parts, 5.0 parts of bentonite, 30.0 parts of pearlite, and 10.0 parts of clay were pulverized and mixed with a hammer mill (Sample Mill KIIW-1, manufactured by Dalton) to obtain a powder mixture. The obtained powder mixture was put into a double-arm kneader (KDHJ, manufactured by Dalton), and kneaded for 15 minutes after water addition. Next, this water-kneaded product was granulated by an extrusion granulator equipped with a basket type screen having a hole diameter of 3.0 mm. The obtained granules were pre-dried, sized with a drum type granulator, and dried with a fluidized bed drier. This was sieved at 3.35 mm to 2.00 mm to obtain a water-floating pesticide formulation. The particle size of the obtained preparation was 83% in the range of 2.80 to 1.70 mm, the ratio of major axis / minor axis at the bottom was 1.2, and the number of particles per 1 g was 93.

[Example 70]
The formulation was 18.0 parts of benfresate (herbicidal active ingredient), 28.0 parts of fly ash balloon (average particle size of 80 to 120 μm) (floating carrier), 1.5 parts of sodium dialkylsuccinatesulfonate, 2.0 parts of carboxymethylcellulose Na Parts, 45.5 parts of perlite, 5.0 parts of clay, and 2.8 mm in particle size, and a water-floating pesticide formulation was prepared according to Example 50. The particle size of the obtained preparation was 87% in the range of 2.80 to 1.70 mm, and the ratio of major axis / minor axis at the bottom surface was 1.4, and the number of particles per 1 g was 83.

[Example 71]
The formulation was 18.0 parts benfresate (herbicidal active ingredient), 2.0 parts of acrylonitrile resin balloon (average particle diameter 20 to 40 μm) (floating carrier), 3.0 parts of sodium alkylnaphthalenesulfonate, 2.0 parts of sodium polyacrylate. Parts, 2.0 parts of carboxymethylcellulose Na, 63.0 parts of perlite, 10.0 parts of clay, and a particle diameter of 3.0 mm. The particle size of the obtained preparation was 84% in the range of 2.80 to 1.70 mm, and the ratio of major axis / minor axis at the bottom surface was 1.3, and the number of particles per 1 g was 86.

[Example 72]
The formulation was 18.0 parts of benfresate (herbicidal active ingredient), 30.0 parts of ceramic balloon (average particle diameter of 20 to 150 μm) (floating carrier), 3.0 parts of sodium alkylnaphthalenesulfonate, 3.0 parts of carboxymethylcellulose Na, Diatomaceous earth was 39.0 parts, clay was 7.0 parts, and the particle size was 3.0 mm. A water-floating pesticide formulation was prepared according to Example 69. The particle size of the obtained preparation was 94% in the range of 2.80 to 1.70 mm, and the ratio of major axis / minor axis at the bottom surface was 1.4, and the number of particles per 1 g was 97.

[Example 73]
The pharmaceutical composition was 18.0 parts of benfresate (herbicidal active ingredient), 28.0 parts of shirasu balloon (average particle size 70 to 90 μm) (floating carrier), 1.5 parts of sodium dialkylsuccinatesulfonate, and 1.5 parts of acrylic acid-maleic acid. Example 69 Polymer Na was 2.0 parts, carboxymethyl cellulose Na was 3.0 parts, bentonite was 10.0 parts, perlite was 25.0 parts, white carbon was 7.5 parts, clay was 5.0 parts, and the particle size was 2.8 mm. A water-floating pesticide formulation was prepared in accordance with. The particle size of the obtained preparation was 93% in the range of 2.80 to 1.70 mm, the ratio of major axis / minor axis at the bottom was 1.2, and the number of particles per gram was 82.

[Example 74]
The pharmaceutical composition was 18.0 parts of benfresate (herbicidal active ingredient), Shirasu balloon (average particle diameter 90 to 120 μm) (floating carrier) 30.0 parts, alkylnaphthalenesulfonic acid Na 3.0 parts, acrylic-methacrylic acid copolymer 2.0 parts of Na, 2.0 parts of carboxymethylcellulose Na, 40.0 parts of diatomaceous earth, 5.0 parts of clay, and a particle size of 2.8 mm were prepared according to Example 69 to prepare a water-floating pesticide formulation. The particle size of the obtained preparation was 86% in the range of 2.80 to 1.70 mm, and the ratio of major axis / minor axis at the bottom surface was 1.4, and the number of particles per 1 g was 85.

[Example 75]
The pharmaceutical composition was 18.0 parts of benfresate (herbicidally active ingredient), 30.0 parts of shirasu balloon (average particle diameter 90 to 120 μm) (floating carrier), 1.5 parts of sodium dialkylsuccinatesulfonate, 3.0 parts of sodium polyacrylate. Parts, 2.0 parts of carboxymethylcellulose Na, 40.0 parts of diatomaceous earth, 5.5 parts of clay, and a particle size of 3.0 mm, and a water-floating pesticide formulation was prepared according to Example 69. The particle size of the obtained preparation was 85% in the range of 2.80 to 1.70 mm, and the ratio of major axis / minor axis at the bottom surface was 1.3, and the number of particles per gram was 80.

[Example 76]
The formulation was 18.0 parts of benfresate (herbicidally active ingredient), 28.0 parts of shirasu balloon (average particle size of 90 to 120 μm) (floating carrier), 3.0 parts of sodium alkylnaphthalenesulfonate, acrylic-maleic acid copolymer 3.0 parts of Na, 2.0 parts of carboxymethylcellulose, 38.0 parts of perlite, 8.0 parts of clay, and 3.0 mm in particle size were prepared, and a water-floating pesticide formulation was prepared according to Example 69. The particle size of the obtained preparation was 93% in the range of 2.80 to 1.70 mm, the ratio of major axis / minor axis at the bottom was 1.2, and the number of particles per 1 g was 91.

[Example 77]
The pharmaceutical composition was 18.0 parts of benfresate (herbicidal active ingredient), Shirasu balloon (average particle diameter 90 to 120 μm) (floating carrier) 25.0 parts, dialkyl succinate sulfonic acid Na 1.5 parts, acrylic acid-vinyl sulfonic acid 2.0 parts of copolymer Na, 2.0 parts of carboxymethylcellulose Na, 46.5 parts of perlite, 5.0 parts of clay, and 2.8 mm in particle diameter were prepared, and a water-floating pesticide formulation was prepared according to Example 69. . The particle size of the obtained preparation was 97% in the range of 2.80 to 1.70 mm, the ratio of major axis / minor axis at the bottom was 1.1, and the number of particles per 1 g was 79.

[Example 78]
The pharmaceutical composition was 18.0 parts of benfresate (herbicidal active ingredient), Shirasu balloon (average particle diameter 70 to 90 μm) (floating carrier) 28.0 parts, alkyl naphthalene sulfonic acid Na 3.0 parts, alkyl naphthalene sulfonic acid formaldehyde condensate 3.0 parts of Na, 2.0 parts of acryl-methacrylic acid copolymer Na, 2.0 parts of carboxymethylcellulose Na, 39.0 parts of pearlite, 5.0 parts of clay, and 2.8 mm in particle diameter. Thus, a water-floating pesticide formulation was prepared. The particle size of the obtained preparation was 84% in the range of 2.80 to 1.70 mm, the ratio of major axis / minor axis at the bottom was 1.2, and the number of particles per 1 g was 75.

[Example 79]
The formulation was 18.0 parts benfresate (herbicidal active ingredient), fly ash balloon (average particle diameter 80 to 120 μm) (floating carrier) 30.0 parts, dialkyl succinate sulfonate Na 1.5 parts, partially desulfonated lignin 3.0 parts of sodium sulfonic acid, 2.0 parts of sodium polyacrylate, 2.0 parts of carboxymethyl cellulose, 10.0 parts of bentonite, 18.5 parts of pearlite, 10.0 parts of white carbon, 5.0 parts of clay, particle size A water-floating pesticide formulation was prepared in accordance with Example 69 with a thickness of 3.0 mm. The particle size of the obtained preparation was 83% in the range of 2.80 to 1.70 mm, and the ratio of major axis / minor axis at the bottom surface was 1.4, and the number of particles per gram was 98.

[Example 80]
The pharmaceutical composition was 18.0 parts of benfresate (herbicidal active ingredient), 30.0 parts of ceramic balloon (average particle size of 20 to 150 μm) (floating carrier), 3.0 parts of sodium alkylnaphthalenesulfonate, and Naphthalenesulfonic acid formaldehyde condensate Na3 2.0 parts, acryl-vinylsulfonic acid copolymer Na 3.0 parts, carboxymethyl cellulose Na 2.0 parts, bentonite 10.0 parts, diatomaceous earth 28.0 parts, clay 4.0 parts, and a particle size of 2.8 mm. A water-floating pesticide formulation was prepared according to Example 69. The particle size of the obtained preparation was 97% in the range of 2.80 to 1.70 mm, and the ratio of major axis / minor axis at the bottom surface was 1.4, and the number of particles per gram was 89.

[Example 81]
The formulation was 18.0 parts benfresate (herbicidally active ingredient), 2.0 parts of acrylonitrile resin balloon (average particle size of 20 to 40 μm) (floating carrier), 1.5 parts of sodium dialkylsuccinatesulfonate, partially desulfonated lignin Example 69: 3.0 parts of sodium sulfonic acid, 2.0 parts of acrylic acid-maleic acid copolymer Na, 3.0 parts of carboxymethylcellulose Na, 60.5 parts of diatomaceous earth, 10.0 parts of clay, and a particle size of 3.0 mm A water-floating pesticide formulation was prepared according to the standard. The particle size of the obtained preparation was 95% in the range of 2.80 to 1.70 mm, and the ratio of major axis / minor axis at the bottom surface was 1.3, and the number of particles per 1 g was 86.

[Example 82]
The formulation was 18.0 parts benfresate (herbicidal active ingredient), Shirasu balloon (average particle size 90 to 120 μm) (floating carrier) 28.0 parts, alkyl naphthalene sulfonic acid Na 3.0 parts, alkyl naphthalene sulfonic acid formaldehyde condensate 3.0 parts of Na, 3.0 parts of acryl-vinylsulfonic acid copolymer Na, 3.0 parts of carboxymethylcellulose Na, 10.0 parts of bentonite, 28.0 parts of pearlite, 4.0 parts of clay, and 2.8 mm in particle diameter. A water-floating pesticide formulation was prepared according to Example 69. The particle size of the obtained preparation was 83% in the range of 2.80 to 1.70 mm, and the ratio of major axis / minor axis at the bottom surface was 1.4, and the number of particles per gram was 98.

[Example 83]
The pharmaceutical composition was 18.0 parts of benfresate (herbicidal active ingredient), Shirasu balloon (average particle diameter 90 to 120 μm) (floating carrier) 30.0 parts, dialkyl succinate sulfonic acid Na 1.5 parts, naphthalene sulfonic acid formaldehyde condensate Na 3.0 parts, acrylic acid-methacrylic acid copolymer Na 3.0 parts, carboxymethyl cellulose Na 3.0 parts, bentonite 10.0 parts, perlite 15.0 parts, white carbon 12.0 parts, clay 4.5 parts, A water-susceptible pesticide formulation was prepared according to Example 69 with a particle diameter of 3.0 mm. The particle size of the obtained preparation was 84% in the range of 2.80 to 1.70 mm, the ratio of major axis / minor axis at the bottom was 1.1, and the number of particles per 1 g was 101.

[Example 84]
The pharmaceutical composition was 18.0 parts of benfresate (herbicidally active ingredient), Shirasu balloon (average particle diameter 90 to 120 μm) (floating carrier) 28.0 parts, alkylnaphthalenesulfonic acid Na 3.0 parts, partially desulfonated ligninsulfonic acid Na 3.0 parts, acrylic-maleic acid copolymer Na 3.0 parts, carboxymethylcellulose Na 3.0 parts, perlite 37.0 parts, clay 5.0 parts, particle size 3.0 mm. Thus, a water-floating pesticide formulation was prepared. The particle size of the obtained preparation was 95% in the range of 2.80 to 1.70 mm, and the ratio of major axis / minor axis at the bottom surface was 1.4, and the number of particles per 1 g was 96.

[Example 85]
The formulation was 18.0 parts of benfresate (herbicidal active ingredient), Shirasu balloon (average particle size 90 to 120 μm) (floating carrier) 30.0 parts, dialkyl succinate sulfonate Na 1.5 parts, alkylnaphthalene sulfonic acid formaldehyde condensation Product Na 3.0 parts, sodium polyacrylate 3.0 parts, carboxymethylcellulose Na 3.0 parts, diatomaceous earth 36.5 parts, clay 5.0 parts, particle diameter 2.8 mm. A pesticide formulation was prepared. The particle size of the obtained preparation was 93% in the range of 2.80 to 1.70 mm, and the ratio of major axis / minor axis at the bottom was 1.3, and the number of particles per 1 g was 93.

[Comparative Example 1]
The formulation composition was 24.0 parts of kasugamycin (bactericidal active ingredient), 25.0 parts of shirasu balloon (average particle size of 90 to 120 μm) (floating carrier), 3.0 parts of sodium alkylnaphthalenesulfonate, 2.0 parts of carboxymethylcellulose Na, 40.0 parts of perlite, 6.0 parts of clay, 3.0 mm of formed particle diameter, the sieves at the time of sieving were 3.35 mm and 0.85 mm sieve, and a water-floating pesticide formulation was prepared according to Example 1. did. The particle size of the obtained preparation is 72% in the range of 2.80 to 1.70 mm (the remainder is 28% below the particle size of 1.70 mm), and the ratio of major axis / minor axis at the bottom surface is 1.2 / g / g. The number was 179 and a formulation with many particles smaller than 1.70 mm in particle size was prepared.

[Comparative Example 2]
The pharmaceutical composition was 24.0 parts of kasugamycin (bactericidal active ingredient), 25.0 parts of shirasu balloon (average particle diameter of 90 to 120 μm) (floating carrier), 3.0 parts of sodium alkylnaphthalenesulfonic acid, and partially desulfonated ligninsulfonic acid. Example: 3.0 parts of Na, 2.0 parts of carboxymethylcellulose Na, 36.0 parts of perlite, 7.0 parts of clay, 1.7 mm in particle diameter 1.7 mm, and sieves used for sieving were 2.00 mm and 0.85 mm. A water-floating pesticide formulation was prepared according to 1. The particle size of the obtained preparation is 5% in the range of 2.80 to 1.70 mm (the rest is 95% below the particle size of 1.70 mm), and the ratio of major axis / minor axis at the bottom surface is 1.0 per 1 g. The number was 259, and a preparation having many small particles of 1.70 mm or less was prepared.

[Comparative Example 3]
The pharmaceutical composition was 24.0 parts of kasugamycin (bactericidal active ingredient), 25.0 parts of shirasu balloon (average particle size of 90 to 120 μm) (floating carrier), 3.0 parts of sodium alkylnaphthalenesulfonate, and condensate of alkylnaphthalenesulfonic acid formaldehyde Example: 3.0 parts of Na, 2.0 parts of carboxymethylcellulose Na, 35.0 parts of pearlite, 8.0 parts of clay, 4.0 mm of formed particle diameter, 4.76 mm and 2.36 mm sieves were used for screening. A water-floating pesticide formulation was prepared according to 1. The particle size of the obtained preparation is 23% in the range of 2.80 to 1.70 mm (the rest is 77% above 2.80 mm), and the ratio of major axis to minor axis at the bottom is 1.3, the number of grains per 1 g. Was 36, and a formulation with many grains larger than 2.80 mm was prepared.

[Comparative Example 4]
The pharmaceutical composition was 24.0 parts of kasugamycin (bactericidal active ingredient), 25.0 parts of shirasu balloon (average particle diameter of 90 to 120 μm) (floating carrier), 3.0 parts of sodium alkylnaphthalenesulfonic acid, and partially desulfonated ligninsulfonic acid. Na 3.0 parts, carboxymethyl cellulose Na 2.0 parts, perlite 37.0 parts, clay 6.0 parts, granulation particle size 3.0 mm And dried to prepare a water-floating pesticide formulation. The particle size of the obtained preparation was 83% in the range of 2.80 to 1.70 mm, the ratio of major axis / minor axis at the bottom surface was 1.0, and the number of particles per 1 g was 112.

[Comparative Example 5]
The formulation composition was 24.0 parts of kasugamycin (bactericidal active ingredient), 25.0 parts of shirasu balloon (average particle size of 90 to 120 μm) (floating carrier), 3.0 parts of sodium alkylnaphthalenesulfonate, 2.0 parts of carboxymethylcellulose Na, 38.0 parts of pearlite, 8.0 parts of clay, 8.0 mm of granulated particle diameter, 3.0 mm, and in addition to sizing with a drum sizing machine, further sizing in a plastic bag so as to be beaten up and down. A floating pesticide formulation was prepared. The particle size of the obtained preparation was 85% in the range of 2.80 to 1.70 mm, and the ratio of major axis / minor axis at the bottom surface was 1.6, and the number of particles per gram was 108.

[Comparative Example 6]
The pharmaceutical composition was 24.0 parts of kasugamycin (bactericidal active ingredient), 25.0 parts of shirasu balloon (average particle diameter of 90 to 120 μm) (floating carrier), 3.0 parts of sodium alkylnaphthalenesulfonic acid, and partially desulfonated ligninsulfonic acid. 3.0 parts of Na, 2.0 parts of carboxymethylcellulose Na, 33.0 parts of pearlite, 10.0 parts of clay, 3.0 mm in particle diameter, 3.0 mm in addition to sizing with a drum sizing machine, and further up and down in a plastic bag The sieved granules were dried to prepare a water-floating pesticide formulation. The particle size of the obtained preparation was 85% in the range of 2.80 to 1.70 mm, and the ratio of major axis / minor axis at the bottom surface was 1.8 and the number of particles per 1 g was 119.

[Comparative Example 7]
The composition of the formulation was 24.0 parts of kasugamycin (bactericidal active ingredient), 3.0 parts of sodium alkylnaphthalenesulfonate, 3.0 parts of partially desulfonated ligninsulfonic acid Na, 3.0 parts of carboxymethylcellulose Na, 60.0 parts of perlite, clay 7 0.0 parts, the particle size was 3.0 mm, and a water-floating pesticide formulation was prepared according to Example 1. The particle size of the obtained preparation was 82% in the range of 2.80 to 1.70 mm, the ratio of major axis / minor axis at the bottom was 1.2, and the number of particles per 1 g was 103.

[Comparative Example 8]
The pharmaceutical composition was 24.0 parts of kasugamycin (bactericidal active ingredient), 3.0 parts of sodium alkylnaphthalenesulfonate, 3.0 parts of partially desulfonated ligninsulfonic acid Na, 3.0 parts of carboxymethylcellulose Na, 18.0 parts of perlite, clay 49. 0.0 parts, the particle size was 3.0 mm, and a water-floating pesticide formulation was prepared according to Example 1. The particle size of the obtained preparation was 86% in the range of 2.80 to 1.70 mm, and the ratio of major axis / minor axis at the bottom surface was 1.4, and the number of particles per gram was 43.

[Comparative Example 9]
The pharmaceutical composition was 24.0 parts of kasugamycin (bactericidal active ingredient), 25.0 parts of shirasu balloon (average particle diameter of 90 to 120 μm) (floating carrier), 3.0 parts of partially desulfonated lignin sulfonic acid Na, 3.0 parts of carboxymethyl cellulose Na3. 0 parts, 39.0 parts of pearlite, 6.0 parts of clay and 3.0 mm in particle size were prepared, and a water-floating pesticide formulation was prepared according to Example 1. The particle size of the obtained preparation was 84% in the range of 2.80 to 1.70 mm, the ratio of major axis / minor axis at the bottom was 1.2, and the number of particles per 1 g was 108.

[Comparative Example 10]
The pharmaceutical composition was 24.0 parts of kasugamycin (bactericidal active ingredient), 25.0 parts of shirasu balloon (average particle size 90 to 120 μm) (floating carrier), 3.0 parts of partially desulfonated lignin sulfonic acid Na, 3.0 parts of alkyl sulfate Na. 0 parts, 3.0 parts of carboxymethylcellulose Na, 34.0 parts of perlite, 8.0 parts of clay, and 3.0 mm in particle diameter, and prepared a water-floating pesticide formulation according to Example 1. The particle size of the obtained preparation was 83% in the range of 2.80 to 1.70 mm, the ratio of major axis / minor axis at the bottom was 1.2, and the number of particles per gram was 98.

[Comparative Example 11]
The pharmaceutical composition was 24.0 parts of kasugamycin (bactericidal active ingredient), 25.0 parts of shirasu balloon (average particle size of 90 to 120 μm) (floating carrier), 3.0 parts of partially desulfonated lignin sulfonic acid Na, and 3 parts of alkylbenzene sulfonic acid Na 3 0.0 parts, 2.0 parts of carboxymethylcellulose Na, 38.0 parts of perlite, 5.0 parts of clay, 3.0 mm in particle diameter, and prepared a water-floating pesticide formulation according to Example 1. The particle size of the obtained preparation was 85% in the range of 2.80 to 1.70 mm, and the ratio of major axis / minor axis at the bottom surface was 1.4, and the number of particles per 1 g was 100.

[Comparative Example 12]
The composition of the formulation was 24.0 parts of kasugamycin (bactericidal active ingredient), 25.0 parts of shirasu balloon (average particle size of 90 to 120 μm) (floating carrier), 3.0 parts of alkylnaphthalenesulfonic acid formaldehyde condensate Na, polyoxyethylene alkyl 3.0 parts of ether, 2.0 parts of carboxymethylcellulose Na, 36.0 parts of perlite, 7.0 parts of clay, and 3.0 mm in particle diameter were prepared, and a water-floating pesticide formulation was prepared in accordance with Example 1. The particle size of the obtained preparation was 86% in the range of 2.80 to 1.70 mm, and the ratio of major axis / minor axis at the bottom surface was 1.3, and the number of particles per gram was 95.

[Comparative Example 13]
The pharmaceutical composition was 24.0 parts of kasugamycin (bactericidal active ingredient), 25.0 parts of shirasu balloon (average particle size of 90 to 120 μm) (floating carrier), 3.0 parts of polyoxyethylene arylphenyl ether, 3.0 parts of carboxymethylcellulose Na. Parts, 39.0 parts of perlite, 6.0 parts of clay, and a particle size of 3.0 mm, and a water-floating pesticide formulation was prepared in accordance with Example 1. The particle size of the obtained preparation was 83% in the range of 2.80 to 1.70 mm, the ratio of major axis / minor axis at the bottom was 1.2, and the number of particles per 1 g was 113.

[Comparative Example 14]
12.0 parts of pymetrozine (insecticidally active ingredient), 25.0 parts of shirasu balloon (average particle size of 90 to 120 μm) (floating carrier), 3.0 parts of sodium alkylnaphthalenesulfonate, 3.0 parts of carboxymethylcellulose Na, 47.0 parts of perlite, 10.0 parts of clay, particle size of 3.0 mm, sieves for sieving were 3.35 mm and 0.85 mm sieve, and a water-floating pesticide formulation was prepared according to Example 18. did. The particle size of the obtained preparation is 65% in the range of 2.80 to 1.70 mm (the remainder is 35% below 1.70 mm), and the ratio of major axis / minor axis at the bottom surface is 1.2, particles per 1 g. A formulation with a number of 195 and a large number of grains smaller than 1.70 mm was prepared.

[Comparative Example 15]
Formulation composition was 12.0 parts of pymetrozine (insecticidally active ingredient), Shirasu balloon (average particle diameter 90 to 120 μm) (floating carrier) 25.0 parts, alkylnaphthalenesulfonic acid Na 3.0 parts, partially desulfonated ligninsulfonic acid Example: 3.0 parts of Na, 3.0 parts of carboxymethylcellulose Na, 48.0 parts of pearlite, 6.0 parts of clay, 1.7 mm in particle diameter 1.7 mm, the sieves used for sieving were 2.00 mm and 0.85 mm. A water-floating pesticide formulation was prepared according to No. 18. The particle size of the obtained preparation is 1% in the range of 2.80 to 1.70 mm (the remainder is 99% below the particle size of 1.70 mm), and the ratio of major axis / minor axis at the bottom surface is 1.0 / g / g. The number was 283, and a preparation having many small particles of 1.70 mm or less was prepared.

[Comparative Example 16]
Formulation composition is 12.0 parts of pymetrozine (insecticidally active ingredient), 25.0 parts of shirasu balloon (average particle size of 90 to 120 μm) (floating carrier), 3.0 parts of sodium alkylnaphthalenesulfonate, formaldehyde condensate of alkylnaphthalenesulfonic acid Example: 3.0 parts of Na, 3.0 parts of carboxymethylcellulose Na, 47.0 parts of pearlite, 7.0 parts of clay, 4.0 mm in particle diameter 4.0 mm, and sieves for screening were 4.76 mm and 2.36 mm. A water-floating pesticide formulation was prepared according to No. 18. The particle size of the obtained preparation is 15% in the range of 2.80 to 1.70 mm (the rest is 85% above 2.80 mm), and the ratio of major axis / minor axis at the bottom surface is 1.2. Was 40, and a formulation with many grains larger than 2.80 mm was prepared.

[Comparative Example 17]
Formulation composition was 12.0 parts of pymetrozine (insecticidally active ingredient), Shirasu balloon (average particle diameter 90 to 120 μm) (floating carrier) 25.0 parts, alkylnaphthalenesulfonic acid Na 3.0 parts, partially desulfonated ligninsulfonic acid Na 3.0 parts, carboxymethyl cellulose Na 3.0 parts, perlite 47.0 parts, clay 7.0 parts, granulation particle size 3.0 mm And dried to prepare a water-floating pesticide formulation. The particle size of the obtained preparation was 86% in the range of 2.80 to 1.70 mm, the ratio of major axis / minor axis at the bottom surface was 1.0, and the number of particles per gram was 105.

[Comparative Example 18]
12.0 parts of pymetrozine (insecticidally active ingredient), 25.0 parts of shirasu balloon (average particle size of 90 to 120 μm) (floating carrier), 3.0 parts of sodium alkylnaphthalenesulfonate, 3.0 parts of carboxymethylcellulose Na, 51.0 parts of pearlite, 6.0 parts of clay, 3.0 mm of granulated particle size, in addition to sizing with a drum sizing machine, and further sizing in a plastic bag so as to be beaten up and down. A floating pesticide formulation was prepared. The particle size of the obtained preparation was 82% in the range of 2.80 to 1.70 mm, and the ratio of major axis / minor axis at the bottom surface was 1.6, and the number of particles per 1 g was 96.

[Comparative Example 19]
Formulation composition was 12.0 parts of pymetrozine (insecticidally active ingredient), 25.0 parts of shirasu balloon (average particle size of 90 to 120 μm) (floating carrier), 3.0 parts of sodium alkylnaphthalenesulfonic acid, and partially desulfonated ligninsulfonic acid. 3.0 parts of Na, 3.0 parts of carboxymethylcellulose Na, 47.0 parts of pearlite, 7.0 parts of clay, 3.0 mm in particle diameter, and in addition to sizing with a drum sizing machine, further up and down in a plastic bag The sieved granules were dried to prepare a water-floating pesticide formulation. The particle size of the obtained preparation was 84% in the range of 2.80 to 1.70 mm, and the ratio of major axis / minor axis at the bottom surface was 1.8 and the number of particles per gram was 108.

[Comparative Example 20]
Formulation composition was 12.0 parts of pymetrozine (insecticidal active ingredient), 3.0 parts of sodium alkylnaphthalenesulfonate, 3.0 parts of partially desulfonated ligninsulfonic acid Na, 3.0 parts of carboxymethylcellulose Na, 69.0 parts of perlite, clay 10 0.0 parts and a particle size of 3.0 mm were prepared according to Example 18 to prepare a water-floating pesticide formulation. The particle size of the obtained preparation was 85% in the range of 2.80 to 1.70 mm, the ratio of major axis / minor axis at the bottom was 1.2, and the number of particles per 1 g was 93.

[Comparative Example 21]
The formulation was composed of 12.0 parts of pymetrozine (an insecticidal active ingredient), 3.0 parts of sodium alkylnaphthalenesulfonic acid, 3.0 parts of partially desulfonated ligninsulfonic acid Na, 3.0 parts of carboxymethylcellulose Na, 21.0 parts of perlite, and clay 58. 0.0 part, the particle size was 3.0 mm, and a water-floating pesticide formulation was prepared according to Example 18. The particle size of the obtained preparation was 85% in the range of 2.80 to 1.70 mm, and the ratio of major axis / minor axis at the bottom surface was 1.4, and the number of particles per gram was 38.

[Comparative Example 22]
The formulation was composed of 12.0 parts of pymetrozine (insecticidally active ingredient), 25.0 parts of shirasu balloon (average particle diameter 90 to 120 μm) (floating carrier), 3.0 parts of partially desulfonated lignin sulfonic acid Na, and carboxymethyl cellulose Na2. 0 parts, 51.0 parts of perlite, 7.0 parts of clay, and 3.0 mm in particle size were prepared, and a water-floating pesticide formulation was prepared according to Example 18. The particle size of the obtained preparation was 83% in the range of 2.80 to 1.70 mm, the ratio of major axis / minor axis at the bottom was 1.2, and the number of particles per gram was 106.

[Comparative Example 23]
The formulation was composed of 12.0 parts of pymetrozine (insecticidally active ingredient), 25.0 parts of shirasu balloon (average particle size of 90 to 120 μm) (floating carrier), 3.0 parts of partially desulfonated lignin sulfonic acid Na, 3.0 parts of alkyl sulfate Na. 0 parts, 2.0 parts of carboxymethylcellulose Na, 48.0 parts of pearlite, 7.0 parts of clay, and a particle diameter of 3.0 mm, and a water-floating pesticide formulation was prepared according to Example 18. The particle size of the obtained preparation was 85% in the range of 2.80 to 1.70 mm, and the ratio of major axis / minor axis at the bottom surface was 1.4, and the number of particles per gram was 93.

[Comparative Example 24]
Formulation composition was 12.0 parts of pymetrozine (active insecticide), 25.0 parts of shirasu balloon (average particle size of 90 to 120 μm) (floating carrier), 3.0 parts of partially desulfonated ligninsulfonic acid Na, 3.0 parts of alkylbenzenesulfonic acid Na3 0.0 parts, 2.0 parts of carboxymethylcellulose Na, 46.0 parts of perlite, 9.0 parts of clay, and 3.0 mm in particle diameter, and prepared a water-floating pesticide formulation according to Example 18. The particle size of the obtained preparation was 84% in the range of 2.80 to 1.70 mm, the ratio of major axis / minor axis at the bottom was 1.2, and the number of particles per 1 g was 95.

[Comparative Example 25]
Formulation composition was 12.0 parts of pymetrozine (insecticidally active ingredient), 25.0 parts of shirasu balloon (average particle diameter of 90 to 120 μm) (floating carrier), 3.0 parts of alkylnaphthalenesulfonic acid formaldehyde condensate Na, polyoxyethylene alkyl 3.0 parts of ether, 3.0 parts of carboxymethylcellulose Na, 50.0 parts of perlite, 4.0 parts of clay, and 3.0 mm in particle diameter were prepared, and a water-floating pesticide formulation was prepared in accordance with Example 18. The particle size of the obtained preparation was 85% in the range of 2.80 to 1.70 mm, and the ratio of major axis / minor axis at the bottom surface was 1.4, and the number of particles per gram was 83.

[Comparative Example 26]
Formulation composition was 12.0 parts of pymetrozine (insecticidally active ingredient), Shirasu balloon (average particle size 90 to 120 μm) (floating carrier) 25.0 parts, polyoxyethylene aryl phenyl ether 3.0 parts, carboxymethyl cellulose Na 3.0. Parts, 49.0 parts of pearlite, 8.0 parts of clay, and 3.0 mm in particle diameter, and prepared a water-floating pesticide formulation according to Example 18. The particle size of the obtained preparation was 86% in the range of 2.80 to 1.70 mm, the ratio of major axis / minor axis at the bottom was 1.1, and the number of particles per 1 g was 99.

[Comparative Example 27]
The formulation was 10.0 parts of ipfencarbazone (herbicidally active ingredient), 25.0 parts of shirasu balloon (average particle size: 90 to 120 μm) (floating carrier), 3.0 parts of sodium alkylnaphthalenesulfonate, 2.0 parts of carboxymethylcellulose Na2. 0 parts, perlite 52.0 parts, clay 8.0 parts (of which the composition used for the slurry is 10.0 parts of ipfencarbazone, 1.0 part of sodium alkylnaphthalenesulfonate, 14.0 parts of water), granulation A sieve having a diameter of 3.0 mm and sieves at the time of sieving was 3.35 mm and 0.85 mm, and a water-floating pesticide preparation was prepared in accordance with Example 35. The particle size of the obtained preparation is 68% in the range of 2.80 to 1.70 mm (the remainder is 32% below 1.70 mm), and the ratio of major axis / minor axis at the bottom is 1.2, particles per 1 g. A formulation with a number of 175 and a large number of particles smaller than 1.70 mm in particle size was prepared.

[Comparative Example 28]
The pharmaceutical composition was 10.0 parts of ipfencarbazone (herbicidally active ingredient), 25.0 parts of shirasu balloon (average particle diameter of 90 to 120 μm) (floating carrier), 3.0 parts of sodium alkylnaphthalenesulfonate, and partially desulfonated. Lignin sulfonic acid Na 3.0 parts, carboxymethyl cellulose Na 2.0 parts, perlite 48.0 parts, clay 9.0 parts 0 parts, water 14.0 parts), a particle size of 1.7 mm, sieves at the time of sieving were 2.00 mm and 0.85 mm, and a water-floating pesticide formulation was prepared according to Example 35. The particle size of the obtained preparation is 10% in the range of 2.80 to 1.70 mm (the remainder is 90% below the particle size of 1.70 mm), and the ratio of major axis / minor axis on the bottom surface is 1.0 per 1 g. The number was 354 and a formulation with many small grains of 1.70 mm or less was prepared.

[Comparative Example 29]
Formulation composition is ipfencarbazone 10.0 parts (herbicidal active ingredient), Shirasu balloon (average particle size 90 to 120 μm) (floating carrier) 25.0 parts, alkyl naphthalene sulfonic acid Na 3.0 parts, alkyl naphthalene sulfonic acid 3.0 parts of formaldehyde condensate Na, 2.0 parts of carboxymethylcellulose Na, 51.0 parts of perlite, 6.0 parts of clay (of which the composition used for the slurry was 10.0 parts of ipfencarbazone, Na1 of alkylnaphthalenesulfonic acid). 0 parts, water 14.0 parts), a particle size of 4.0 mm, sieves at the time of sieving were 4.76 mm and 2.36 mm, and a water-floating pesticide formulation was prepared according to Example 35. The particle size of the obtained preparation is 38% in the range of 2.80 to 1.70 mm (the rest is 62% above 2.80 mm), and the ratio of major axis / minor axis on the bottom surface is 1.2. Was 41, and a formulation having many grains larger than 2.80 mm was prepared.

[Comparative Example 30]
The pharmaceutical composition was 10.0 parts of ipfencarbazone (herbicidally active ingredient), 25.0 parts of shirasu balloon (average particle diameter of 90 to 120 μm) (floating carrier), 3.0 parts of sodium alkylnaphthalenesulfonate, and partially desulfonated. 3.0 parts of ligninsulfonic acid Na, 3.0 parts of carboxymethylcellulose Na, 49.0 parts of perlite, 7.0 parts of clay (of which the composition used for the slurry was 10.0 parts of ipfencarbazone, Na1 of alkylnaphthalenesulfonic acid. (0 part, water 14.0 parts), granulation particle size 3.0 mm, without passing through a sizing by a drum sizing machine, drying in a state where the cross section is a perfect circle to prepare a water-floating pesticide formulation. . The particle size of the obtained preparation was 86% in the range of 2.80 to 1.70 mm, the ratio of major axis / minor axis at the bottom surface was 1.0, and the number of particles per gram was 98.

[Comparative Example 31]
The pharmaceutical composition was 10.0 parts of ipfencarbazone (herbicidally active ingredient), 25.0 parts of shirasu balloon (average particle size: 90 to 120 μm) (floating carrier), 3.0 parts of sodium alkylnaphthalenesulfonate, and 3.0 parts of carboxymethylcellulose Na3. 0 parts, perlite 52.0 parts, clay 7.0 parts (of which the composition used for the slurry is 10.0 parts of ipfencarbazone, 1.0 part of sodium alkylnaphthalenesulfonate, 14.0 parts of water), granulation The diameter was adjusted to 3.0 mm, and in addition to sizing with a drum sizing machine, the sieved granules were further smashed up and down in a plastic bag, and dried to prepare a water-floating pesticide formulation. The particle size of the obtained preparation was 83% in the range of 2.80 to 1.70 mm, and the ratio of major axis / minor axis at the bottom surface was 1.6, and the number of particles per gram was 89.

[Comparative Example 32]
The pharmaceutical composition was 10.0 parts of ipfencarbazone (herbicidally active ingredient), 25.0 parts of shirasu balloon (average particle diameter of 90 to 120 μm) (floating carrier), 3.0 parts of sodium alkylnaphthalenesulfonate, and partially desulfonated. 3.0 parts of ligninsulfonic acid Na, 3.0 parts of carboxymethylcellulose Na, 49.0 parts of perlite, 7.0 parts of clay (of which the composition used for the slurry was 10.0 parts of ipfencarbazone, Na1 of alkylnaphthalenesulfonic acid. 0 parts, water 14.0 parts), the granulation particle size is 3.0 mm, and in addition to sizing with a drum sizing machine, the sizing is performed by smashing up and down in a plastic bag, and then dried to obtain a water surface floating property. A pesticide formulation was prepared. The particle size of the obtained preparation was 84% in the range of 2.80 to 1.70 mm, and the ratio of major axis / minor axis at the bottom was 1.8, and the number of particles per gram was 83.

[Comparative Example 33]
The pharmaceutical composition was 10.0 parts of ipfencarbazone (herbicidally active ingredient), 3.0 parts of sodium alkylnaphthalenesulfonic acid, 3.0 parts of partially desulfonated ligninsulfonic acid Na, 2.0 parts of carboxymethylcellulose Na, and 65.0 parts of perlite. And 17.0 parts of clay (of which the composition used for the slurry was 10.0 parts of ipfencarbazone, 1.0 part of sodium alkylnaphthalenesulfonate, and 14.0 parts of water), and the particle size was 3.0 mm. A water-floating pesticide formulation was prepared according to 35. The particle size of the obtained preparation was 86% in the range of 2.80 to 1.70 mm, and the ratio of major axis / minor axis at the bottom surface was 1.3, and the number of particles per gram was 96.

[Comparative Example 34]
Formulation composition was 10.0 parts of ipfencarbazone (herbicidal active ingredient), 3.0 parts of sodium alkylnaphthalenesulfonate, 3.0 parts of partially desulfonated ligninsulfonic acid Na, 3.0 parts of carboxymethylcellulose Na, and 30.0 parts of perlite. And 51.0 parts of clay (of which the composition used for the slurry was 10.0 parts of ipfencarbazone, 1.0 part of sodium alkylnaphthalenesulfonate, 14.0 parts of water), and the particle size was 3.0 mm. A water-floating pesticide formulation was prepared according to 35. The particle size of the obtained preparation was 83% in the range of 2.80 to 1.70 mm, and the ratio of major axis / minor axis at the bottom surface was 1.4, and the number of particles per 1 g was 33.

[Comparative Example 35]
The formulation composition was 10.0 parts of ipfencarbazone (herbicidally active ingredient), 25.0 parts of shirasu balloon (average particle size of 90 to 120 μm) (floating carrier), 3.0 parts of partially desulfonated lignin sulfonic acid Na, and carboxy. 3.0 parts of methylcellulose Na, 50.0 parts of perlite, 9.0 parts of clay (of which the composition used for the slurry was 10.0 parts of ipfencarbazone, 1.0 part of partially desulfonated ligninsulfonic acid Na, 1.0 part of water). 0 part), the particle size was 3.0 mm, and a water-susceptible pesticide formulation was prepared according to Example 35. The particle size of the obtained preparation was 83% in the range of 2.80 to 1.70 mm, the ratio of major axis / minor axis at the bottom was 1.2, and the number of particles per 1 g was 105.

[Comparative Example 36]
Formulation composition was 10.0 parts of ipfencarbazone (herbicidally active ingredient), 25.0 parts of shirasu balloon (average particle diameter of 90 to 120 μm) (floating carrier), 3.0 parts of partially desulfonated lignin sulfonic acid Na, alkyl 3.0 parts of sodium sulfate, 2.0 parts of carboxymethylcellulose Na, 48.0 parts of perlite, 9.0 parts of clay (of which the composition used for the slurry is 10.0 parts of ipfencarbazone, partially desulfonated lignin sulfonic acid Na1) 2.0 parts, water 14.0 parts), the particle size was 3.0 mm, and a water-floating pesticide formulation was prepared according to Example 35. The particle size of the obtained preparation was 85% in the range of 2.80 to 1.70 mm, the ratio of major axis / minor axis at the bottom was 1.1, and the number of particles per 1 g was 90.

[Comparative Example 37]
The composition of the formulation was 10.0 parts of ipfencarbazone (herbicidally active ingredient), 25.0 parts of shirasu balloon (average particle diameter of 90 to 120 μm) (floating carrier), 3.0 parts of partially desulfonated ligninsulfonic acid Na, and alkylbenzene. 3.0 parts of sodium sulfonic acid, 3.0 parts of carboxymethylcellulose Na, 51.0 parts of perlite, 5.0 parts of clay (of which the composition used for the slurry is 10.0 parts of ipfencarbazone, partially desulfonated lignin sulfonic acid (1.0 part of Na, 14.0 parts of water), and the particle size was 3.0 mm. The particle size of the obtained preparation was 82% in the range of 2.80 to 1.70 mm, the ratio of major axis / minor axis at the bottom was 1.2, and the number of particles per 1 g was 110.

[Comparative Example 38]
The pharmaceutical composition was 10.0 parts of ipfencarbazone (herbicidally active ingredient), 25.0 parts of shirasu balloon (average particle size of 90 to 120 μm) (floating carrier), 3.0 parts of an alkylnaphthalenesulfonic acid formaldehyde condensate Na, 3.0 parts of oxyethylene alkyl ether, 3.0 parts of carboxymethylcellulose Na, 49.0 parts of perlite, 7.0 parts of clay (of which the composition used for the slurry was 10.0 parts of ipfencarbazone, polyoxyethylene alkyl ether 1.0 part, water 14.0 parts), and the particle size was 3.0 mm. The particle size of the obtained preparation was 87% in the range of 2.80 to 1.70 mm, the ratio of major axis / minor axis at the bottom was 1.2, and the number of particles per 1 g was 99.

[Comparative Example 39]
Formulation composition is ipfencarbazone 10.0 parts (herbicidal active ingredient), Shirasu balloon (average particle size 90 to 120 μm) (floating carrier) 25.0 parts, polyoxyethylene aryl phenyl ether 3.0 parts, carboxymethyl cellulose 2.0 parts of Na, 54.0 parts of perlite, 6.0 parts of clay (of which the composition used for the slurry was 10.0 parts of ipfencarbazone, 1.0 part of polyoxyethylene arylphenyl ether, 14.0 parts of water) ), The particle size was 3.0 mm, and a water-floating pesticide formulation was prepared according to Example 35. The particle size of the obtained preparation was 83% in the range of 2.80 to 1.70 mm, the ratio of major axis / minor axis at the bottom was 1.2, and the number of particles per 1 g was 86.

[Comparative Example 40]
12.0 parts of simethrin (herbicidal active ingredient), 25.0 parts of shirasu balloon (average particle size of 90 to 120 μm) (floating carrier), 3.0 parts of sodium alkylnaphthalenesulfonic acid, 3.0 parts of carboxymethylcellulose Na, 51.0 parts of pearlite, 6.0 parts of clay, 3.0 mm of formed particle size, the sieves at the time of sieving were 3.35 mm and 0.85 mm sieve, and a water-floating pesticide formulation was prepared according to Example 52. did. The particle size of the obtained preparation is 55% in the range of 2.80 to 1.70 mm (the remainder is 45% below 1.70 mm), and the ratio of major axis / minor axis at the bottom surface is 1.4 / g / g. The number was 203 and a formulation with many particles smaller than 1.70 mm in particle size was prepared.

[Comparative Example 41]
The composition was 12.0 parts of simethrin (herbicidal active ingredient), 25.0 parts of shirasu balloon (average particle size of 90 to 120 μm) (floating carrier), 3.0 parts of sodium alkylnaphthalenesulfonic acid, and partially desulfonated ligninsulfonic acid. Example: 3.0 parts of Na, 2.0 parts of carboxymethylcellulose Na, 47.0 parts of perlite, 8.0 parts of clay, 1.7 mm in particle diameter 1.7 mm, and sieves used for sieving were 2.00 mm and 0.85 mm. A water-floating pesticide formulation was prepared according to No.52. The particle size of the obtained preparation is 8% in the range of 2.80 to 1.70 mm (the remainder is 92% below the particle size of 1.70 mm), and the ratio of major axis / minor axis at the bottom surface is 1.0 / g / g. The number was 236, and a preparation with many small grains of 1.70 mm or less was prepared.

[Comparative Example 42]
12.0 parts of simethrin (herbicidal active ingredient), 25.0 parts of shirasu balloon (average particle size of 90 to 120 μm) (floating carrier), 3.0 parts of sodium alkylnaphthalenesulfonate, condensate of alkylnaphthalenesulfonic acid formaldehyde Example: 3.0 parts of Na, 3.0 parts of carboxymethylcellulose Na, 49.0 parts of perlite, 5.0 parts of clay, 4.0 mm in particle diameter, and 4.76 mm and 2.36 mm sieves for screening. A water-floating pesticide formulation was prepared in accordance with No.52. The particle size of the obtained preparation is 18% in the range of 2.80 to 1.70 mm (the remainder is 82% above 2.80 mm), and the ratio of major axis / minor axis at the bottom surface is 1.4, the number of particles per gram. Was 43, and a formulation having many grains larger than 2.80 mm was prepared.

[Comparative Example 43]
The composition was 12.0 parts of simethrin (herbicidal active ingredient), 25.0 parts of shirasu balloon (average particle size of 90 to 120 μm) (floating carrier), 3.0 parts of sodium alkylnaphthalenesulfonic acid, and partially desulfonated ligninsulfonic acid. Na 3.0 parts, carboxymethylcellulose Na 2.0 parts, perlite 49.0 parts, clay 6.0 parts, granulation particle size 3.0 mm. And dried to prepare a water-floating pesticide formulation. The particle size of the obtained preparation was 85% in the range of 2.80 to 1.70 mm, the ratio of major axis / minor axis at the bottom surface was 1.0, and the number of particles per 1 g was 90.

[Comparative Example 44]
12.0 parts of simethrin (herbicidal active ingredient), 25.0 parts of shirasu balloon (average particle size of 90 to 120 μm) (floating carrier), 3.0 parts of sodium alkylnaphthalenesulfonic acid, 3.0 parts of carboxymethylcellulose Na, 51.0 parts of pearlite, 6.0 parts of clay, 3.0 mm of granulated particle size, in addition to sizing with a drum sizing machine, and further sizing in a plastic bag so as to be beaten up and down. A floating pesticide formulation was prepared. The particle size of the obtained preparation was 83% in the range of 2.80 to 1.70 mm, and the ratio of major axis / minor axis at the bottom surface was 1.6, and the number of particles per gram was 84.

[Comparative Example 45]
The composition was 12.0 parts of simethrin (herbicidal active ingredient), 25.0 parts of shirasu balloon (average particle size of 90 to 120 μm) (floating carrier), 3.0 parts of sodium alkylnaphthalenesulfonic acid, and partially desulfonated ligninsulfonic acid. 3.0 parts of Na, 3.0 parts of carboxymethylcellulose Na, 47.0 parts of pearlite, 7.0 parts of clay, 3.0 mm in particle diameter, and in addition to sizing with a drum sizing machine, further up and down in a plastic bag The sieved granules were dried to prepare a water-floating pesticide formulation. The particle size of the obtained preparation was 86% in the range of 2.80 to 1.70 mm, and the ratio of major axis / minor axis at the bottom surface was 1.8, and the number of particles per gram was 95.

[Comparative Example 46]
The composition was 12.0 parts of simetryn (herbicidally active ingredient), 3.0 parts of sodium alkylnaphthalenesulfonate, 3.0 parts of partially desulfonated ligninsulfonic acid Na, 2.0 parts of carboxymethylcellulose Na, 68.0 parts of perlite, clay 12 0.0 part, the particle size was 3.0 mm, and a water-floating pesticide formulation was prepared according to Example 52. The particle size of the obtained preparation was 83% in the range of 2.80 to 1.70 mm, the ratio of major axis / minor axis at the bottom was 1.1, and the number of particles per 1 g was 99.

[Comparative Example 47]
The composition of the formulation was 12.0 parts of simethrin (herbicidal active ingredient), 3.0 parts of sodium alkylnaphthalenesulfonate, 3.0 parts of partially desulfonated ligninsulfonic acid Na, 2.0 parts of carboxymethylcellulose Na, 25.0 parts of perlite, and clay 55. 0.0 part, the particle size was 3.0 mm, and a water-floating pesticide formulation was prepared according to Example 52. The particle size of the obtained preparation was 82% in the range of 2.80 to 1.70 mm, the ratio of major axis / minor axis at the bottom was 1.2, and the number of particles per gram was 31.

[Comparative Example 48]
The formulation was composed of 12.0 parts of simetryn (herbicidal active ingredient), 25.0 parts of shirasu balloon (average particle size of 90 to 120 μm) (floating carrier), 3.0 parts of partially desulfonated lignin sulfonic acid Na, and 3.0 parts of carboxymethyl cellulose Na3. 0 parts, 49.0 parts of perlite, 8.0 parts of clay, and 3.0 mm in particle diameter, and a water-floating pesticide formulation was prepared according to Example 52. The particle size of the obtained preparation was 86% in the range of 2.80 to 1.70 mm, the ratio of major axis / minor axis at the bottom was 1.2, and the number of particles per gram was 98.

[Comparative Example 49]
The formulation was composed of 12.0 parts of simetryn (herbicidal active ingredient), 25.0 parts of shirasu balloon (average particle diameter of 90 to 120 μm) (floating carrier), 3.0 parts of partially desulfonated lignin sulfonic acid Na, and 3.0 parts of alkyl sulfate Na. 0 parts, 3.0 parts of carboxymethylcellulose Na, 48.0 parts of pearlite, 6.0 parts of clay, and a particle diameter of 3.0 mm were prepared according to Example 52 to prepare a water-floating pesticide formulation. The particle size of the obtained preparation was 85% in the range of 2.80 to 1.70 mm, and the ratio of major axis / minor axis at the bottom surface was 1.4, and the number of particles per 1 g was 107.

[Comparative Example 50]
The pharmaceutical composition was 12.0 parts of simetryn (herbicidally active ingredient), 25.0 parts of shirasu balloon (average particle diameter of 90 to 120 μm) (floating carrier), 3.0 parts of partially desulfonated lignin sulfonic acid Na, 3.0 parts of alkylbenzene sulfonic acid Na3 0.0 part, 3.0 parts of carboxymethylcellulose Na, 48.0 parts of pearlite, 6.0 parts of clay, and 3.0 mm in particle diameter, and prepared a water-floating pesticide formulation according to Example 52. The particle size of the obtained preparation was 84% in the range of 2.80 to 1.70 mm, the ratio of major axis / minor axis at the bottom was 1.2, and the number of particles per 1 g was 110.

[Comparative Example 51]
Formulation composition was 12.0 parts of simetryn (herbicidal active ingredient), 25.0 parts of shirasu balloon (average particle size of 90 to 120 μm) (floating carrier), 3.0 parts of sodium alkylnaphthalenesulfonic acid formaldehyde condensate, polyoxyethylene alkyl 3.0 parts of ether, 2.0 parts of carboxymethylcellulose Na, 47.0 parts of perlite, 8.0 parts of clay, and 3.0 mm in particle diameter were prepared, and a water-floating pesticide formulation was prepared in accordance with Example 52. The particle size of the obtained preparation was 84% in the range of 2.80 to 1.70 mm, and the ratio of major axis / minor axis at the bottom surface was 1.3, and the number of particles per 1 g was 106.

[Comparative Example 52]
The composition was 12.0 parts of simetryn (herbicidal active ingredient), 25.0 parts of shirasu balloon (average particle size of 90 to 120 μm) (floating carrier), 3.0 parts of polyoxyethylene aryl phenyl ether, carboxymethyl cellulose Na2.0 Parts, 50.0 parts of perlite, 8.0 parts of clay, and 3.0 mm in particle size, and a water-floating pesticide formulation was prepared according to Example 52. The particle size of the obtained preparation was 85% in the range of 2.80 to 1.70 mm, the ratio of major axis / minor axis at the bottom was 1.2, and the number of particles per 1 g was 114.

[Comparative Example 53]
18.0 parts of benfresate (herbicidal active ingredient), 25.0 parts of shirasu balloon (average particle diameter of 90 to 120 μm) (floating carrier), 3.0 parts of sodium alkylnaphthalenesulfonate, 2.0 parts of carboxymethylcellulose Na, 46.0 parts of pearlite, 6.0 parts of clay, 3.0 mm of formed particle size, the sieves at the time of sieving were 3.35 mm and 0.85 mm sieve, and a water-floating pesticide formulation was prepared according to Example 69. did. The particle size of the obtained preparation is 63% in the range of 2.80 to 1.70 mm (the remainder is 37% below 1.70 mm), and the ratio of major axis / minor axis at the bottom surface is 1.4 / g / g. A formulation with a number of 188 and many granules smaller than 1.70 mm in particle size was prepared.

[Comparative Example 54]
The pharmaceutical composition was 18.0 parts of benfresate (herbicidal active ingredient), Shirasu balloon (average particle diameter 90 to 120 μm) (floating carrier) 25.0 parts, alkylnaphthalenesulfonic acid Na 3.0 parts, partially desulfonated ligninsulfonic acid Example: 3.0 parts of Na, 3.0 parts of carboxymethylcellulose Na, 40.0 parts of perlite, 8.0 parts of clay, 1.7 mm in particle diameter 1.7 mm, the sieves used for sieving were 2.00 mm and 0.85 mm. A water-floating pesticide formulation was prepared according to 69. The particle size of the obtained preparation is 5% in the range of 2.80 to 1.70 mm (the rest is 95% below the particle size of 1.70 mm), and the ratio of major axis / minor axis at the bottom surface is 1.0 per 1 g. The number was 313, and a preparation having many small grains of 1.70 mm or less was prepared.

[Comparative Example 55]
The pharmaceutical composition was 18.0 parts of benfresate (herbicidally active ingredient), Shirasu balloon (average particle size 90 to 120 μm) (floating carrier) 25.0 parts, sodium alkylnaphthalenesulfonic acid 3.0 parts, alkylnaphthalenesulfonic acid formaldehyde condensate Example: 3.0 parts of Na, 3.0 parts of carboxymethylcellulose Na, 40.0 parts of perlite, 8.0 parts of clay, 4.0 mm of formed particle diameter, 4.76 mm and 2.36 mm sieves were used for screening. A water-floating pesticide formulation was prepared according to 69. The particle size of the obtained preparation is 13% in the range of 2.80 to 1.70 mm (the rest is 87% above 2.80 mm), and the ratio of major axis / minor axis at the bottom surface is 1.2. Was 39, and a formulation having many grains larger than 2.80 mm was prepared.

[Comparative Example 56]
The pharmaceutical composition was 18.0 parts benfresate (herbicidal active ingredient), Shirasu balloon (average particle size 90 to 120 μm) (floating carrier) 25.0 parts, alkylnaphthalenesulfonic acid Na 3.0 parts, partially desulfonated ligninsulfonic acid Na 3.0 parts, carboxymethylcellulose Na 3.0 parts, perlite 38.0 parts, clay 10.0 parts, granulation particle size 3.0 mm. And dried to prepare a water-floating pesticide formulation. The particle size of the obtained preparation was 82% in the range of 2.80 to 1.70 mm, the ratio of major axis / minor axis at the bottom was 1.0, and the number of particles per gram was 108.

[Comparative Example 57]
18.0 parts of benfresate (herbicidal active ingredient), 25.0 parts of shirasu balloon (average particle diameter of 90 to 120 μm) (floating carrier), 3.0 parts of sodium alkylnaphthalenesulfonate, 2.0 parts of carboxymethylcellulose Na, 45.0 parts of pearlite, 7.0 parts of clay, 3.0 mm of granulated particle size, in addition to sizing with a drum sizing machine, and further sizing in a plastic bag so as to be beaten up and down. A floating pesticide formulation was prepared. The particle size of the obtained preparation was 82% in the range of 2.80 to 1.70 mm, and the ratio of major axis / minor axis at the bottom surface was 1.6, and the number of particles per gram was 98.

[Comparative Example 58]
The pharmaceutical composition was 18.0 parts of benfresate (herbicidal active ingredient), Shirasu balloon (average particle diameter 90 to 120 μm) (floating carrier) 25.0 parts, alkylnaphthalenesulfonic acid Na 3.0 parts, partially desulfonated ligninsulfonic acid 3.0 parts of Na, 2.0 parts of carboxymethylcellulose Na, 39.0 parts of perlite, 10.0 parts of clay, 3.0 mm in particle diameter, 3.0 mm in diameter, and in addition to sizing with a drum sizing machine, further up and down in a plastic bag The sieved granules were dried to prepare a water-floating pesticide formulation. The particle size of the obtained preparation was 85% in the range of 2.80 to 1.70 mm, and the ratio of major axis / minor axis at the bottom surface was 1.8, and the number of particles per gram was 93.

[Comparative Example 59]
The pharmaceutical composition was 18.0 parts of benfresate (herbicidally active ingredient), 3.0 parts of sodium alkylnaphthalenesulfonate, 3.0 parts of partially desulfonated ligninsulfonic acid Na, 2.0 parts of carboxymethylcellulose Na, 67.0 parts of perlite, clay 7 0.0 parts, the particle size was 3.0 mm, and a water-floating pesticide formulation was prepared according to Example 69. The particle size of the obtained preparation was 84% in the range of 2.80 to 1.70 mm, and the ratio of major axis / minor axis at the bottom surface was 1.3, and the number of particles per gram was 102.

[Comparative Example 60]
The pharmaceutical composition was 18.0 parts of benfresate (herbicidally active ingredient), 3.0 parts of sodium alkylnaphthalenesulfonate, 3.0 parts of partially desulfonated sodium ligninsulfonate, 2.0 parts of carboxymethylcellulose Na, 19.0 parts of perlite, and clay 55. 0.0 parts, the particle size was 3.0 mm, and a water-floating pesticide formulation was prepared according to Example 69. The particle size of the obtained preparation was 86% in the range of 2.80 to 1.70 mm, the ratio of major axis / minor axis at the bottom was 1.1, and the number of particles per gram was 35.

[Comparative Example 61]
The pharmaceutical composition was 18.0 parts of benfresate (active herbicidal component), 25.0 parts of shirasu balloon (average particle diameter 90 to 120 μm) (floating carrier), 3.0 parts of partially desulfonated lignin sulfonic acid Na, 3.0 parts of carboxymethyl cellulose Na3. 0 parts, 42.0 parts of pearlite, 9.0 parts of clay, and a particle size of 3.0 mm were prepared according to Example 35 to prepare a water-floating pesticide formulation. The particle size of the obtained preparation was 83% in the range of 2.80 to 1.70 mm, the ratio of major axis / minor axis at the bottom was 1.2, and the number of particles per 1 g was 96.

[Comparative Example 62]
The pharmaceutical composition was 18.0 parts of benfresate (herbicidal active ingredient), 25.0 parts of shirasu balloon (average particle diameter of 90 to 120 μm) (floating carrier), 3.0 parts of partially desulfonated lignin sulfonic acid Na, 3.0 parts of alkyl sulfate. According to Example 69, 0 parts, 3.0 parts of carboxymethylcellulose Na, 41.0 parts of pearlite, 7.0 parts of clay, and 3.0 mm in particle diameter were prepared. The particle size of the obtained preparation was 85% in the range of 2.80 to 1.70 mm, the ratio of major axis / minor axis at the bottom was 1.2, and the number of particles per 1 g was 93.

[Comparative Example 63]
The pharmaceutical composition was 18.0 parts of benfresate (herbicidal active ingredient), Shirasu balloon (average particle size 90 to 120 μm) (floating carrier) 25.0 parts, partially desulfonated lignin sulfonic acid Na 3.0 parts, alkylbenzene sulfonic acid Na 3 0.0 parts, 2.0 parts of carboxymethylcellulose Na, 43.0 parts of perlite, 6.0 parts of clay, and 3.0 mm in particle diameter, and prepared a water-floating pesticide formulation according to Example 69. The particle size of the obtained preparation was 84% in the range of 2.80 to 1.70 mm, the ratio of major axis / minor axis at the bottom was 1.1, and the number of particles per 1 g was 83.

[Comparative Example 64]
The pharmaceutical composition was 18.0 parts of benfresate (herbicidal active ingredient), Shirasu balloon (average particle diameter 90 to 120 μm) (floating carrier) 25.0 parts, alkylnaphthalenesulfonic acid formaldehyde condensate Na 3.0 parts, polyoxyethylene alkyl 3.0 parts of ether, 2.0 parts of carboxymethylcellulose Na, 42.0 parts of pearlite, 7.0 parts of clay, and 3.0 mm in particle diameter were prepared, and a water-floating pesticide formulation was prepared according to Example 69. The particle size of the obtained preparation was 82% in the range of 2.80 to 1.70 mm, and the ratio of major axis / minor axis at the bottom surface was 1.3, and the number of particles per gram was 78.

[Comparative Example 65]
The pharmaceutical composition was 18.0 parts of benfresate (herbicidal active ingredient), Shirasu balloon (average particle diameter 90 to 120 μm) (floating carrier) 25.0 parts, polyoxyethylene aryl phenyl ether 3.0 parts, carboxymethyl cellulose Na 3.0. Parts, 43.0 parts of perlite, 8.0 parts of clay, and 3.0 mm in particle size, and prepared a water-floating pesticide formulation according to Example 69. The particle size of the obtained preparation was 83% in the range of 2.80 to 1.70 mm, and the ratio of major axis / minor axis at the bottom was 1.3, and the number of particles per gram was 88.

[Example 86]
Kasugamycin 24.0 parts (bactericidal active ingredient), polyoxyalkylene alkyl ether phosphate ester salt (alkylene group: carbon number 2, alkyl group: n-octyl, ester bond number: 1, cation: Na ⁺ ) 10.0 Parts, 2.0 parts of propylene glycol, 2.5 parts of sodium alkylnaphthalenesulfonate, 3.0 parts of methylcellulose, 25.0 parts of perlite, and 8.5 parts of clay with a hammer mill (Sample Mill KIIW-1, manufactured by Dalton). The mixture was ground and mixed to obtain a powder mixture. The obtained powder mixture and 25.0 parts of a shirasu balloon (average particle diameter 70 to 90 μm) (floating carrier) were mixed in a double-arm kneader (KDHJ, manufactured by Dalton) for 10 minutes, and then mixed and kneaded for 15 minutes. Next, this water-kneaded product was granulated by an extrusion granulator equipped with a basket type screen having a hole diameter of 3.0 mm. The obtained granules were pre-dried, sized with a drum type granulator, and dried with a fluidized bed drier. This was sieved at 3.35 mm to 2.00 mm to obtain a water-floating pesticide formulation. The particle size of the obtained preparation was 83% in the range of 2.80 to 1.70 mm, the ratio of major axis / minor axis at the bottom was 1.2, and the number of particles per 1 g was 113.

[Example 87]
The pharmaceutical composition was 24.0 parts of kasugamycin (a bactericidal active ingredient), 28.0 parts of fly ash balloon (average particle diameter: 80 to 120 μm) (floating carrier), polyoxyalkylene alkyl ether phosphate salt (alkylene group: carbon number) 2, 3, alkyl group: n-octyl, number of ester bonds: 2, cation: Na ⁺ ) 4.0 parts, propylene glycol 2.0 parts, alkylnaphthalenesulfonic acid Na 2.5 parts, acrylic acid-vinylsulfonic acid 2.0 parts of copolymer Na, 6.0 parts of dextrin, 20.0 parts of white carbon, 11.5 parts of bentonite and 2.8 mm in particle diameter were prepared, and a water-floating pesticide formulation was prepared according to Example 86. . The particle size of the obtained preparation was 86% in the range of 2.80 to 1.70 mm, and the ratio of major axis / minor axis at the bottom surface was 1.4, and the number of particles per 1 g was 103.

[Example 88]
The formulation composition was 24.0 parts of kasugamycin (bactericidal active ingredient), 25.0 parts of ceramic balloon (average particle size of 20 to 150 μm) (floating carrier), polyoxyalkylene alkyl ether phosphate salt (alkylene group having 2 carbon atoms). 3, alkyl group: 2-ethylhexyl, number of ester bonds: 1, cation: Na ⁺ ) 6.0 parts, propylene glycol 1.5 parts, dialkyl succinate sulfonic acid Na 2.5 parts, polyacrylic acid Na 2.0 Parts, 3.0 parts of methylcellulose, 25.0 parts of pearlite, 11.0 parts of bentonite, and a particle diameter of 3.0 mm. A water-floating pesticide formulation was prepared according to Example 86. The particle size of the obtained preparation was 85% in the range of 2.80 to 1.70 mm, and the ratio of major axis / minor axis at the bottom was 1.6, and the number of particles per gram was 175.

[Example 89]
The pharmaceutical composition was 24.0 parts of kasugamycin (bactericidal active ingredient), 2.5 parts of acrylonitrile resin balloon (average particle diameter of 20 to 40 μm) (floating carrier), polyoxyalkylene alkyl ether phosphate salt (alkylene group: carbon number) 2, 3, alkyl group: 2-ethylhexyl, number of ester bonds: 2, cation: Na ⁺ ) 12.0 parts, propylene glycol 3.0 parts, alkylnaphthalenesulfonic acid Na 2.5 parts, methylcellulose 3.0 parts, According to Example 86, 30.0 parts of white carbon, 23.0 parts of bentonite, and a particle size of 3.0 mm were used to prepare a water-floating pesticide formulation. The particle size of the obtained preparation was 83% in the range of 2.80 to 1.70 mm, the ratio of major axis / minor axis at the bottom was 1.5, and the number of particles per 1 g was 132.

[Example 90]
The pharmaceutical composition was 24.0 parts of kasugamycin (bactericidal active ingredient), 25.0 parts of ceramic balloon (average particle diameter of 20 to 150 μm) (floating carrier), polyoxyalkylene alkyl ether phosphate salt (alkylene group: having 2 carbon atoms). 4, alkyl group: n-decyl, number of ester bonds: 1, cation: H ⁺ ) 10.0 parts, propylene glycol 2.0 parts, dialkyl succinate sulfonate Na 2.5 parts, polyacrylic acid Na 2.0 Parts, dextrin 6.0 parts, perlite 20.0 parts, bentonite 8.5 parts, particle size 3.0 mm, and a water-floating pesticide formulation was prepared according to Example 86. The particle size of the obtained preparation was 85% in the range of 2.80 to 1.70 mm, and the ratio of major axis / minor axis at the bottom surface was 1.3, and the number of particles per gram was 115.

[Example 91]
The pharmaceutical composition was 24.0 parts of kasugamycin (bactericidal active ingredient), 2.5 parts of acrylonitrile resin balloon (average particle diameter of 20 to 40 μm) (floating carrier), polyoxyalkylene alkyl ether phosphate salt (alkylene group: carbon number) 2, 3, alkyl group: n-decyl, number of ester bonds: 2, cation: H ⁺ ) 10.0 parts, propylene glycol 2.0 parts, alkylnaphthalenesulfonic acid Na 2.5 parts, acrylic acid-vinylsulfonic acid 2.0 parts of copolymer Na, 6.0 parts of dextrin, 30.0 parts of white carbon, 23.0 parts of bentonite and 2.8 mm in particle diameter were prepared. . The particle size of the obtained preparation was 86% in the range of 2.80 to 1.70 mm, and the ratio of major axis / minor axis at the bottom surface was 1.4, and the number of particles per gram was 102.

[Example 92]
24.0 parts of kasugamycin (bactericidal active ingredient), fly ash balloon (average particle diameter 80 to 120 μm) (floating carrier) 25.0 parts, polyoxyalkylene alkyl ether phosphate salt (alkylene group: carbon number) 2, 3, alkyl group: isodecyl, number of ester bonds: 1, cation: K ⁺ ) 8.0 parts, butylene glycol 2.5 parts, dialkyl succinatesulfonic acid Na 2.5 parts, acrylic acid-vinylsulfonic acid Based on Example 86, 2.0 parts of polymer Na, 6.0 parts of dextrin, 17.0 parts of pearlite, 13.0 parts of clay, and a particle diameter of 3.0 mm were prepared. The particle size of the obtained preparation was 82% in the range of 2.80 to 1.70 mm, and the ratio of major axis / minor axis at the bottom surface was 1.3, and the number of particles per gram was 59.

[Example 93]
The pharmaceutical composition was 24.0 parts of kasugamycin (bactericidal active ingredient), 28.0 parts of shirasu balloon (average particle size of 70 to 90 μm) (floating carrier), polyoxyalkylene alkyl ether phosphate salt (alkylene group having 2 carbon atoms). 3, 4, alkyl group: isodecyl, number of ester bonds: 2, cation: K ⁺ ) 10.0 parts, propylene glycol 2.0 parts, alkylnaphthalenesulfonic acid Na 2.5 parts, acrylic acid-vinylsulfonic acid According to Example 86, 2.0 parts of polymer Na, 3.0 parts of methyl cellulose, 18.0 parts of white carbon, 10.5 parts of bentonite, and 2.8 mm in particle size were prepared. The particle size of the obtained preparation was 87% in the range of 2.80 to 1.70 mm, the ratio of major axis / minor axis at the bottom was 1.1, and the number of particles per 1 g was 121.

[Example 94]
The composition of the formulation was 24.0 parts of kasugamycin (bactericidal active ingredient), 25.0 parts of fly ash balloon (average particle diameter 80 to 120 μm) (floating carrier), polyoxyalkylene alkyl ether phosphate salt (alkylene group: carbon number) 2, 3, alkyl group: 2-ethylhexyl, number of ester bonds: 1, cation: Na ⁺ ) 5.0 parts, polyoxyalkylene alkyl ether phosphate salt (alkylene group: 2, 3 carbon atoms, alkyl group: 2-ethylhexyl, number of ester bonds: 2, cation: Na ⁺ ) 5.0 parts, propylene glycol 2.5 parts, alkylnaphthalenesulfonic acid Na 2.5 parts, acrylic acid-methacrylic acid copolymer Na 2.0 parts, Example 8: 3.0 parts of methylcellulose, 20.0 parts of diatomaceous earth, 11.0 parts of clay, and a particle size of 3.0 mm It was prepared water-floating agrochemical formulations in compliance with. The particle size of the obtained preparation was 82% in the range of 2.80 to 1.70 mm, the ratio of major axis / minor axis at the bottom was 1.5, and the number of particles per 1 g was 135.

[Example 95]
The formulation composition was 24.0 parts of kasugamycin (bactericidal active ingredient), 25.0 parts of shirasu balloon (average particle diameter 70 to 90 μm) (floating carrier), polyoxyalkylene alkyl ether phosphate salt (alkylene group: 2 carbon atoms). , Alkyl group: n-octyl, number of ester bonds: 1, cation: Na ⁺ ) 4.0 parts, polyoxyalkylene alkyl ether phosphate salt (alkylene group: 2, 3 carbon atoms, alkyl group: 2-ethylhexyl) , Number of ester bonds: 1, cation: Na ⁺ ) 4.0 parts, polyoxyalkylene alkyl ether phosphate ester salt (alkylene group: 2, 3, 4, carbon atoms, alkyl group: isodecyl, number of ester bonds: 2, ^cations: K +) 4.0 parts propylene glycol 2.0 parts, Na2.5 parts alkylnaphthalenesulfonate, Na3.0 parts Riakuriru acid, methyl cellulose, 3.0 parts of 20.0 parts of perlite, clay 8.5 parts, and Zotsubu径 3.0 mm, to prepare a water-floating agrochemical formulations in conformity with Example 86. The particle size of the obtained preparation was 82% in the range of 2.80 to 1.70 mm, and the ratio of major axis / minor axis at the bottom surface was 1.3, and the number of particles per 1 g was 127.

[Example 96]
The pharmaceutical composition was 24.0 parts of kasugamycin (bactericidal active ingredient), 25.0 parts of ceramic balloon (average particle diameter of 20 to 150 μm) (floating carrier), polyoxyalkylene alkyl ether phosphate salt (alkylene group: having 2 carbon atoms). 3, 4, alkyl group: n-octyl, number of ester bonds: 2, cation: Na ⁺ ) 6.0 parts, polyoxyalkylene alkyl ether phosphate salt (alkylene group: 2, 3 carbon atoms, alkyl group) : 2-ethylhexyl, number of ester bonds: 2, cation: Na ⁺ ) 6.0 parts, propylene glycol 2.5 parts, alkylnaphthalenesulfonic acid Na2.5 parts, acrylic acid-vinylsulfonic acid copolymer Na2.0 Parts, dextrin 6.0 parts, pearlite 20.0 parts, bentonite 6.0 parts, particle size 3.0 mm. It was prepared water-floating agrochemical formulations in compliance with 6. The particle size of the obtained preparation was 94% in the range of 2.80 to 1.70 mm, the ratio of major axis / minor axis at the bottom was 1.2, and the number of particles per gram was 161.

[Example 97]
The pharmaceutical composition was 24.0 parts of kasugamycin (bactericidal active ingredient), 28.0 parts of shirasu balloon (average particle diameter of 90 to 120 μm) (floating carrier), polyoxyalkylene alkyl ether phosphate (alkylene group: 2 carbon atoms) 3, alkyl group: n-decyl, number of ester bonds: 2, cation: H ⁺ ) 5.0 parts, polyoxyalkylene alkyl ether phosphate salt (alkylene group: 2, 3 carbon atoms, alkyl group: isodecyl) , Number of ester bonds: 1, cation: K ⁺ ) 5.0 parts, propylene glycol 1.5 parts, dialkyl succinate sulfonate Na 2.5 parts, polyacrylate Na 2.5 parts, methyl cellulose 3.0 parts, diatomaceous earth 18.0 parts, bentonite 10.5 parts, particle size 3.0 mm, prepared a water-floating pesticide formulation according to Example 86 It was. The particle size of the obtained preparation was 82% in the range of 2.80 to 1.70 mm, and the ratio of major axis / minor axis at the bottom surface was 1.3, and the number of particles per gram was 115.

[Example 98]
The formulation composition was 24.0 parts of kasugamycin (bactericidal active ingredient), 25.0 parts of shirasu balloon (average particle size of 90 to 120 μm) (floating carrier), polyoxyalkylene alkyl ether phosphate salt (alkylene group having 2 carbon atoms). 4, alkyl group: n-decyl, number of ester bonds: 1, cation: H ⁺ ) 8.0 parts, propylene glycol 2.0 parts, dialkyl succinatesulfonic acid Na 2.5 parts, acrylic acid-vinylsulfonic acid 2.0 parts of copolymer Na, 3.0 parts of methylcellulose, 25.0 parts of pearlite, 8.5 parts of bentonite, and a particle size of 2.8 mm were prepared. The particle size of the obtained preparation was 92% in the range of 2.80 to 1.70 mm, and the ratio of major axis / minor axis at the bottom surface was 1.4, and the number of particles per 1 g was 105.

[Example 99]
The pharmaceutical composition was 24.0 parts of kasugamycin (bactericidal active ingredient), 25.0 parts of ceramic balloon (average particle diameter of 20 to 150 μm) (floating carrier), polyoxyalkylene alkyl ether phosphate salt (alkylene group: having 2 carbon atoms). 3, alkyl group: isodecyl, number of ester bonds: 1, cation: K ⁺ ) 4.0 parts, polyoxyalkylene alkyl ether phosphate salt (alkylene group: 2, 3, 4, carbon atoms, alkyl group: isodecyl) , ester bonds: 2, ^cation: K +) 4.0 parts propylene glycol 2.5 parts, Na2.5 parts alkylnaphthalenesulfonate, Na5.0 parts naphthalenesulfonic acid formaldehyde condensates, polyacrylic acid Na3. 0 parts, dextrin 6.0 parts, diatomaceous earth 20.0 parts, clay 4.0 parts, particle size 3.0 mm. To prepare a water-floating agrochemical formulations in conformity with Example 86. The particle size of the obtained preparation was 86% in the range of 2.80 to 1.70 mm, the ratio of major axis / minor axis at the bottom was 1.2, and the number of particles per 1 g was 183.

[Example 100]
The pharmaceutical composition was 24.0 parts of kasugamycin (bactericidal active ingredient), 28.0 parts of shirasu balloon (average particle diameter of 90 to 120 μm) (floating carrier), polyoxyalkylene alkyl ether phosphate (alkylene group: 2 carbon atoms) 3, alkyl group: isodecyl, number of ester bonds: 1, cation: K ⁺ ) 10.0 parts, propylene glycol 2.0 parts, alkylnaphthalenesulfonic acid Na2.5 parts, alkylnaphthalenesulfonic acid formaldehyde condensate Na3. 0 parts, 2.0 parts of an acrylic acid-maleic acid copolymer Na, 6.0 parts of dextrin, 17.0 parts of pearlite, 5.5 parts of clay, and a particle size of 3.0 mm. A floating pesticide formulation was prepared. The particle size of the obtained preparation was 94% in the range of 2.80 to 1.70 mm, the ratio of major axis / minor axis at the bottom was 1.2, and the number of particles per 1 g was 127.

[Example 101]
The pharmaceutical composition was 24.0 parts of kasugamycin (bactericidal active ingredient), 25.0 parts of ceramic balloon (average particle diameter of 20 to 150 μm) (floating carrier), polyoxyalkylene alkyl ether phosphate salt (alkylene group: having 2 carbon atoms) 3, alkyl group: n-octyl, number of ester bonds: 2, cation: Na ⁺ ) 6.0 parts, polyoxyalkylene alkyl ether phosphate salt (alkylene group: 2, 3 carbon atoms, alkyl group: n) -Decyl, number of ester bonds: 2, cation: H ⁺ ) 6.0 parts, propylene glycol 2.5 parts, dialkyl succinatesulfonic acid Na 2.5 parts, acrylic acid-methacrylic acid copolymer Na 2.0 parts, Carboxymethylcellulose Na 3.0 parts, diatomaceous earth 20.0 parts, bentonite 9.0 parts, particle size 2.8 mm It was prepared water-floating agrochemical formulations in compliance with 6. The particle size of the obtained preparation was 82% in the range of 2.80 to 1.70 mm, and the ratio of major axis / minor axis at the bottom surface was 1.3, and the number of particles per gram was 118.

[Example 102]
The pharmaceutical composition was 24.0 parts of kasugamycin (bactericidal active ingredient), 25.0 parts of shirasu balloon (average particle size of 90 to 120 μm) (floating carrier), polyoxyalkylene alkyl ether phosphate (alkylene group: 2 carbon atoms) 3, alkyl group: 2-ethylhexyl, number of ester bonds: 2, cation: Na ⁺ ) 4.0 parts, polyoxyalkylene alkyl ether phosphate salt (alkylene group: 2, 4 carbon atoms, alkyl group: n) -Decyl, number of ester bonds: 1, cation: H ⁺ ) 4.0 parts, propylene glycol 3.0 parts, ligninsulfonic acid Na 3.0 parts, polyacrylic acid Na 2.0 parts, polyvinyl alcohol 3.0 parts, 20.0 parts of perlite, 9.5 parts of clay, and 3.0 mm in particle diameter were prepared, and a water-floating pesticide formulation was prepared according to Example 86. The particle size of the obtained preparation was 96% in the range of 2.80 to 1.70 mm, and the ratio of major axis / minor axis at the bottom surface was 1.3, and the number of particles per 1 g was 116.

[Example 103]
The formulation composition was 24.0 parts of kasugamycin (bactericidal active ingredient), 25.0 parts of shirasu balloon (average particle size of 90 to 120 μm) (floating carrier), polyoxyalkylene alkyl ether phosphate salt (alkylene group having 2 carbon atoms). 3, alkyl group: n-octyl, number of ester bonds: 2, cation: Na ⁺ ) 5.0 parts, polyoxyalkylene alkyl ether phosphate salt (alkylene group: 2, 3 carbon atoms, alkyl group: n) -Decyl, number of ester bonds: 2, cation: H ⁺ ) 5.0 parts, alkylnaphthalenesulfonic acid Na 2.5 parts, alkylnaphthalenesulfonic acid formaldehyde condensate Na 3.0 parts, polyacrylic acid Na 2.0 parts, carboxy 3.0 parts of methylcellulose Na, 12.5 parts of diatomaceous earth, 18.0 parts of bentonite, and a particle size of 3.0 mm To prepare a water-floating agrochemical formulations in conformity with Example 86. The particle size of the obtained preparation was 94% in the range of 2.80 to 1.70 mm, and the ratio of major axis / minor axis at the bottom was 1.3, and the number of particles per 1 g was 61.

[Example 104]
The formulation composition was 24.0 parts of kasugamycin (bactericidal active ingredient), 25.0 parts of shirasu balloon (average particle size of 90 to 120 μm) (floating carrier), 3.0 parts of propylene glycol, 2.5 parts of sodium alkylnaphthalenesulfonate, Naphthalenesulfonic acid formaldehyde condensate Na 3.0 parts, acrylic acid-vinylsulfonic acid copolymer Na 2.0 parts, carboxymethylcellulose Na 3.0 parts, diatomaceous earth 25.0 parts, bentonite 12.5 parts, particle size 3.0 mm A water-floating pesticide formulation was prepared according to Example 86. The particle size of the obtained preparation was 92% in the range of 2.80 to 1.70 mm, and the ratio of major axis / minor axis at the bottom surface was 1.4, and the number of particles per 1 g was 105.

[Example 105]
Pymetrozine 12.0 parts (pesticidal active ingredient), polyoxyalkylene alkyl ether phosphate ester salt (alkylene group: carbon number 2, alkyl group: n-octyl, ester bond number: 1, cation: Na ⁺ ) 10.0 Parts, 2.5 parts of propylene glycol, 2.5 parts of sodium alkylnaphthalenesulfonate, 6.0 parts of dextrin, 27.0 parts of perlite, and 15.0 parts of bentonite with a hammer mill (Sample Mill KIIW-1, manufactured by Dalton). The mixture was ground and mixed to obtain a powder mixture. The obtained powder mixture and 25.0 parts of a shirasu balloon (average particle diameter 70 to 90 μm) (floating carrier) were mixed in a double-arm kneader (KDHJ, manufactured by Dalton) for 10 minutes, and then mixed and kneaded for 15 minutes. Next, the kneaded mixture was granulated by an extrusion granulator equipped with a basket-type screen having a hole diameter of 2.8 mm. The obtained granules were pre-dried, sized with a drum type granulator, and dried with a fluidized bed drier. This was sieved at 3.35 mm to 2.00 mm to obtain a water-floating pesticide formulation. The particle size of the obtained preparation was 84% in the range of 2.80 to 1.70 mm, the ratio of major axis / minor axis at the bottom was 1.2, and the number of particles per 1 g was 138.

[Example 106]
Formulation composition was 12.0 parts of pymetrozine (insecticidally active ingredient), 25.0 parts of fly ash balloon (average particle size 80 to 120 μm) (floating carrier), polyoxyalkylene alkyl ether phosphate salt (alkylene group: carbon number) 2, 4, alkyl group: n-octyl, number of ester bonds: 2, cation: Na ⁺ ) 4.0 parts, propylene glycol 2.0 parts, dialkyl succinate sulfonate Na 2.5 parts, acrylic acid-vinyl sulfone 1.5 parts of acid copolymer Na, 6.0 parts of dextrin, 28.0 parts of diatomaceous earth, 19.0 parts of clay, and a particle diameter of 3.0 mm were prepared, and a water-floating pesticide formulation was prepared according to Example 105. . The particle size of the obtained preparation was 87% in the range of 2.80 to 1.70 mm, and the ratio of major axis / minor axis at the bottom surface was 1.4, and the number of particles per 1 g was 105.

[Example 107]
Formulation composition was 12.0 parts of pymetrozine (insecticidally active ingredient), 30.0 parts of fly ash balloon (average particle diameter of 80 to 120 μm) (floating carrier), polyoxyalkylene alkyl ether phosphate salt (alkylene group: carbon number) 2, 3, alkyl group: 2-ethylhexyl, number of ester bonds: 1, cation: Na ⁺ ) 6.0 parts, propylene glycol 2.0 parts, dialkyl succinate sulfonic acid Na 2.5 parts, acrylic acid-vinyl sulfone 2.0 parts of acid copolymer Na, 3.0 parts of methylcellulose, 25,0 parts of diatomaceous earth, 17.5 parts of bentonite, 3.0 mm in particle diameter were prepared, and a water-floating pesticide formulation was prepared according to Example 105. . The particle size of the obtained preparation was 85% in the range of 2.80 to 1.70 mm, the ratio of major axis / minor axis at the bottom was 1.2, and the number of particles per gram was 182.

[Example 108]
Formulation composition was 12.0 parts of pymetrozine (insecticidally active ingredient), 30.0 parts of fly ash balloon (average particle diameter of 80 to 120 μm) (floating carrier), polyoxyalkylene alkyl ether phosphate salt (alkylene group: carbon number) 2, alkyl group: 2-ethylhexyl, number of ester bonds: 2, cation: Na ⁺ ) 12.0 parts, hexylene glycol 2.5 parts, alkylnaphthalenesulfonic acid Na 2.5 parts, dextrin 7.0 parts, white A water-floating pesticide formulation was prepared according to Example 105, using 17.0 parts of carbon, 17.0 parts of bentonite, and a particle size of 3.0 mm. The particle size of the obtained preparation was 83% in the range of 2.80 to 1.70 mm, and the ratio of major axis / minor axis at the bottom surface was 1.4, and the number of particles per gram was 159.

[Example 109]
The formulation was composed of 12.0 parts of pymetrozine (active insecticide), 25.0 parts of ceramic balloon (average particle diameter of 20 to 150 μm) (floating carrier), polyoxyalkylene alkyl ether phosphate (alkylene group having 2 carbon atoms). , Alkyl group: n-decyl, number of ester bonds: 1, cation: H ⁺ ) 10.0 parts, propylene glycol 2.0 parts, alkylnaphthalenesulfonic acid Na2.5 parts, acrylic acid-methacrylic acid copolymer Na2 0.05 parts, 3.0 parts of methylcellulose, 25.0 parts of perlite, 18.5 parts of clay, and a particle diameter of 3.0 mm were prepared according to Example 105 to prepare a water-floating pesticide formulation. The particle size of the obtained preparation was 86% in the range of 2.80 to 1.70 mm, and the ratio of major axis / minor axis at the bottom surface was 1.3, and the number of particles per 1 g was 108.

[Example 110]
Formulation composition was 12.0 parts of pymetrozine (insecticidally active ingredient), 2.5 parts of acrylonitrile resin balloon (average particle diameter 20 to 40 μm) (floating carrier), polyoxyalkylene alkyl ether phosphate ester salt (alkylene group: carbon number) 2, 3, 4, alkyl group: n-decyl, number of ester bonds: 2, cation: H ⁺ ) 10.0 parts, propylene glycol 2.5 parts, dialkyl succinate sulfonate Na 2.5 parts, dextrin 6. 0 parts, 35.0 parts of diatomaceous earth, 29.5 parts of bentonite, and a particle diameter of 3.0 mm were prepared, and a water-floating pesticide formulation was prepared according to Example 105. The particle size of the obtained preparation was 85% in the range of 2.80 to 1.70 mm, and the ratio of major axis / minor axis at the bottom surface was 1.4, and the number of particles per gram was 125.

[Example 111]
Formulation composition was 12.0 parts of pymetrozine (insecticidally active ingredient), 30.0 parts of ceramic balloon (average particle size: 20 to 150 μm) (floating carrier), polyoxyalkylene alkyl ether phosphate ester salt (alkylene group: 2 carbon atoms) , Alkyl group: isodecyl, number of ester bonds: 1, cation: K ⁺ ) 10.0 parts, propylene glycol 2.5 parts, alkylnaphthalenesulfonic acid Na 2.5 parts, acrylic acid-methacrylic acid copolymer Na2.0 Parts, 3.0 parts of methylcellulose, 23.0 parts of white carbon, 15.0 parts of clay, and a particle size of 2.8 mm. A water-floating pesticide formulation was prepared according to Example 105. The particle size of the obtained preparation was 86% in the range of 2.80 to 1.70 mm, the ratio of major axis / minor axis at the bottom was 1.1, and the number of particles per 1 g was 113.

[Example 112]
Formulation composition was 12.0 parts of pymetrozine (insecticidal active ingredient), 25.0 parts of shirasu balloon (average particle diameter 70 to 90 μm) (floating carrier), polyoxyalkylene alkyl ether phosphate salt (alkylene group: 2 carbon atoms) , Alkyl group: isodecyl, number of ester bonds: 2, cation: K ⁺ ) 10.0 parts, propylene glycol 2.0 parts, dialkyl succinate sulfonate Na 2.5 parts, polyacrylate Na 1.0 parts, methyl cellulose 3 0.05 parts, 25.0 parts of diatomaceous earth, 19.5 parts of clay, and a particle diameter of 3.0 mm were prepared according to Example 105 to prepare a water-floating pesticide formulation. The particle size of the obtained preparation was 87% in the range of 2.80 to 1.70 mm, the ratio of major axis / minor axis at the bottom was 1.2, and the number of particles per 1 g was 113.

[Example 113]
Formulation composition was 12.0 parts of pymetrozine (insecticidally active ingredient), 25.0 parts of fly ash balloon (average particle size 80 to 120 μm) (floating carrier), polyoxyalkylene alkyl ether phosphate salt (alkylene group: carbon number) 2, 3, alkyl group: 2-ethylhexyl, number of ester bonds: 1, cation: Na ⁺ ) 5.0 parts, polyoxyalkylene alkyl ether phosphate salt (alkylene group: carbon number 2, alkyl group: 2-) Ethylhexyl, number of ester bonds: 2, cation: Na ⁺ ) 5.0 parts, propylene glycol 2.5 parts, alkylnaphthalenesulfonic acid Na 2.5 parts, acrylic acid-methacrylic acid copolymer Na 3.0 parts, methylcellulose 3 0.05 parts, diatomaceous earth 25.0 parts, clay 17.0 parts, particle size 3.0 mm. It was prepared water-floating agrochemical formulations and bases. The particle size of the obtained preparation was 85% in the range of 2.80 to 1.70 mm, the ratio of major axis / minor axis at the bottom was 1.1, and the number of particles per 1 g was 124.

[Example 114]
The formulation was composed of 12.0 parts of pymetrozine (an insecticidal active ingredient), 30.0 parts of a ceramic balloon (average particle diameter of 20 to 150 μm) (floating carrier), and a polyoxyalkylene alkyl ether phosphate ester salt (alkylene group: 2 carbon atoms). , Alkyl group: n-octyl, number of ester bonds: 1, cation: Na ⁺ ) 4.0 parts, polyoxyalkylene alkyl ether phosphate salt (alkylene group: 2, 3 carbon atoms, alkyl group: 2-ethylhexyl) , Number of ester bonds: 1, cation: Na ⁺ ) 4.0 parts, propylene glycol 2.0 parts, alkylnaphthalenesulfonic acid Na 2.5 parts, acrylic acid-maleic acid copolymer Na 3.0 parts, methyl cellulose 3.0 parts. Example 10: 0 parts, 23.0 parts of white carbon, 17.5 parts of bentonite, and a particle size of 3.0 mm. It was prepared water-floating agrochemical formulations in compliance with. The particle size of the obtained preparation was 83% in the range of 2.80 to 1.70 mm, and the ratio of major axis / minor axis at the bottom surface was 1.6, and the number of particles per gram was 105.

[Example 115]
Formulation composition was 12.0 parts of pymetrozine (insecticidally active ingredient), 2.5 parts of acrylonitrile resin balloon (average particle diameter 20 to 40 μm) (floating carrier), polyoxyalkylene alkyl ether phosphate ester salt (alkylene group: carbon number) 2, 4, alkyl group: n-octyl, number of ester bonds: 2, cation: Na ⁺ ) 6.0 parts, polyoxyalkylene alkyl ether phosphate salt (alkylene group: 2, 3 carbon atoms, alkyl group: 2-ethylhexyl, number of ester bonds: 1, cation: Na ⁺ ) 6.0 parts, propylene glycol 3.0 parts, dialkyl succinate sulfonic acid Na 2.5 parts, acrylic acid-vinyl sulfonic acid copolymer Na 1.5 Parts, dextrin 6.0 parts, perlite 30.0 parts, bentonite 30.5 parts, particle size 2.8 mm, It was prepared water-floating agrochemical formulations in compliance with 施例 105. The particle size of the obtained preparation was 94% in the range of 2.80 to 1.70 mm, the ratio of major axis / minor axis at the bottom was 1.2, and the number of particles per 1 g was 95.

[Example 116]
Formulation composition was 12.0 parts of pymetrozine (insecticidal active ingredient), 28.0 parts of shirasu balloon (average particle diameter 90 to 120 μm) (floating carrier), polyoxyalkylene alkyl ether phosphate ester (alkylene group: 2 carbon atoms) 3, 4, alkyl group: n-decyl, number of ester bonds: 2, cation: H ⁺ ) 10.0 parts, propylene glycol 1.5 parts, alkylnaphthalenesulfonic acid Na 2.5 parts, polyacrylic acid Na2. Based on Example 105, 0 parts, 3.0 parts of methylcellulose, 22.0 parts of diatomaceous earth, 19.0 parts of bentonite, and 3.0 mm in particle diameter were prepared. The particle size of the obtained preparation was 83% in the range of 2.80 to 1.70 mm, and the ratio of major axis / minor axis at the bottom surface was 1.3, and the number of particles per gram was 93.

[Example 117]
Formulation composition was 12.0 parts of pymetrozine (insecticidally active ingredient), 28.0 parts of shirasu balloon (average particle diameter of 90 to 120 μm) (floating carrier), polyoxyalkylene alkyl ether phosphate salt (alkylene group: having 2 carbon atoms) 4, alkyl group: n-octyl, number of ester bonds: 2, cation: Na ⁺ ) 4.0 parts, polyoxyalkylene alkyl ether phosphate ester salt (alkylene group: carbon number 2, alkyl group: 2-ethylhexyl) , ester bonds: 2, ^cations: Na +) 4.0 parts, 1.5 parts of propylene glycol, Na2.5 parts dialkyl succinate sulfonic acid, acrylic acid - vinyl sulfonic acid copolymer Na2.0 parts, methylcellulose 3.0 parts, 22.0 parts of diatomaceous earth, 21.0 parts of clay, and a particle size of 3.0 mm. The water-floating pesticide formulation was prepared. The particle size of the obtained preparation was 97% in the range of 2.80 to 1.70 mm, the ratio of major axis / minor axis at the bottom was 1.2, and the number of particles per 1 g was 109.

[Example 118]
Formulation composition was 12.0 parts of pymetrozine (insecticidal active ingredient), 25.0 parts of ceramic balloon (average particle diameter of 20 to 150 μm) (floating carrier), polyoxyalkylene alkyl ether phosphate ester (alkylene group: 2 carbon atoms) 3, 4, alkyl group: n-decyl, number of ester bonds: 2, cation: H ⁺ ) 12.0 parts, propylene glycol 3.0 parts, alkyl naphthalene sulfonic acid Na 2.5 parts, alkyl naphthalene sulfonic acid formaldehyde Condensate Na 3.0 parts, polyacrylic acid Na 3.0 parts, dextrin 6.0 parts, perlite 25.0 parts, bentonite 8.5 parts, particle size 2.8 mm, and floated on the water surface according to Example 105 A pesticide formulation was prepared. The particle size of the obtained preparation was 82% in the range of 2.80 to 1.70 mm, the ratio of major axis / minor axis at the bottom was 1.1, and the number of particles per 1 g was 111.

[Example 119]
Formulation composition was 12.0 parts of pymetrozine (insecticidally active ingredient), 25.0 parts of shirasu balloon (average particle size of 90 to 120 μm) (floating carrier), polyoxyalkylene alkyl ether phosphate salt (alkylene group: 2 carbon atoms) 3, alkyl group: 2-ethylhexyl, number of ester bonds: 1, cation: Na ⁺ ) 5.0 parts, polyoxyalkylene alkyl ether phosphate ester salt (alkylene group: carbon number 2, alkyl group: n-decyl) , ester bonds: 1 ^cation: H +) 5.0 parts, 1.5 parts of propylene glycol, Na2.5 parts alkylnaphthalenesulfonate, Na3.0 parts naphthalenesulfonic acid formaldehyde condensates, acrylic acid - methacrylic acid 15. Copolymer Na 2.5 parts, methyl cellulose 3.0 parts, perlite 25.0 parts, clay Parts, and Zotsubu径 3.0 mm, to prepare a water-floating agrochemical formulations in conformity with Example 105. The particle size of the obtained preparation was 96% in the range of 2.80 to 1.70 mm, the ratio of major axis / minor axis at the bottom was 1.1, and the number of particles per 1 g was 128.

[Example 120]
Formulation composition was 12.0 parts of pymetrozine (insecticidal active ingredient), 25.0 parts of shirasu balloon (average particle diameter 70 to 90 μm) (floating carrier), polyoxyalkylene alkyl ether phosphate salt (alkylene group: 2 carbon atoms) , Alkyl group: n-octyl, number of ester bonds: 1, cation: Na ⁺ ) 10.0 parts, propylene glycol 2.0 parts, dialkyl succinate sulfonic acid Na 2.5 parts, acrylic acid-vinyl sulfonic acid copolymer 2.0 parts of combined Na, 2.0 parts of carboxymethylcellulose Na, 25.0 parts of white carbon, 19.5 parts of bentonite, and a particle diameter of 3.0 mm were prepared. The particle size of the obtained preparation was 85% in the range of 2.80 to 1.70 mm, the ratio of major axis / minor axis at the bottom was 1.2, and the number of particles per 1 g was 110.

[Example 121]
Formulation composition was 12.0 parts of pymetrozine (insecticidally active ingredient), 25.0 parts of shirasu balloon (average particle size of 90 to 120 μm) (floating carrier), polyoxyalkylene alkyl ether phosphate (alkylene group: 2 carbon atoms) 4, alkyl group: n-octyl, number of ester bonds: 2, cation: Na ⁺ ) 10.0 parts, propylene glycol 2.5 parts, alkyl naphthalene sulfonic acid Na 2.5 parts, lignin sulfonic acid Na 2.5 parts 2.0 parts of sodium polyacrylate, 2.0 parts of polyvinyl alcohol, 26.0 parts of pearlite, 15.5 parts of bentonite, and a particle diameter of 2.8 mm. A water-floating pesticide preparation was prepared according to Example 105. did. The particle size of the obtained preparation was 97% in the range of 2.80 to 1.70 mm, and the ratio of major axis / minor axis at the bottom surface was 1.4, and the number of particles per 1 g was 119.

[Example 122]
Formulation composition was 12.0 parts of pymetrozine (insecticidally active ingredient), 25.0 parts of shirasu balloon (average particle size of 90 to 120 μm) (floating carrier), polyoxyalkylene alkyl ether phosphate salt (alkylene group: 2 carbon atoms) 3, alkyl group: 2-ethylhexyl, number of ester bonds: 1, cation: Na ⁺ ) 10.0 parts, alkyl naphthalene sulfonic acid Na 2.5 parts, alkyl naphthalene sulfonic acid formaldehyde condensate Na 2.5 parts, polyacryl 2.0 parts of sodium acid, 3.0 parts of carboxymethylcellulose Na, 23.0 parts of pearlite, 15.0 parts of bentonite, 5.0 parts of clay, 3.0 mm in particle diameter, 3.0 mm in particle size A formulation was prepared. The particle size of the obtained preparation was 93% in the range of 2.80 to 1.70 mm, the ratio of major axis / minor axis at the bottom was 1.2, and the number of particles per gram was 102.

[Example 123]
The pharmaceutical composition was composed of 12.0 parts of pymetrozine (insecticidally active ingredient), 25.0 parts of shirasu balloon (average particle size of 90 to 120 μm) (floating carrier), 3.0 parts of propylene glycol, 2.5 parts of sodium alkylnaphthalenesulfonate, Naphthalenesulfonic acid formaldehyde condensate Na2.5 parts, acrylic acid-vinylsulfonic acid copolymer Na3.0 parts, carboxymethylcellulose Na3.0 parts, perlite 26.0 parts, bentonite 10.0 parts, clay 13.0 parts, A water-susceptible pesticide formulation was prepared according to Example 105 with a particle diameter of 3.0 mm. The particle size of the obtained preparation was 91% in the range of 2.80 to 1.70 mm, the ratio of major axis / minor axis at the bottom was 1.2, and the number of particles per gram was 79.

[Example 124]
After mixing 10.0 parts of ipfencarbazone (herbicidally active ingredient), 1.0 part of sodium alkylnaphthalenesulfonate, and 14.0 parts of water, the average particle diameter becomes 1.0 μm with Dynomill (manufactured by Shinmaru Enterprises). To obtain a slurry. 8.0 parts of polyoxyalkylene alkyl ether phosphate ester salt (alkylene group: 2, 3 carbon atoms, alkyl group: n-octyl, number of ester bonds: 1, cation: H ⁺ ), propylene glycol 2.0 Parts, 1.5 parts of sodium alkylnaphthalenesulfonate, 3.0 parts of methylcellulose, 29.0 parts of pearlite, and 17.5 parts of bentonite are ground and mixed by a hammer mill (Sample Mill KIIW-1, manufactured by Dalton), and a powder mixture is obtained. I got The slurry, the powder mixture, and 28.0 parts of a shirasu balloon (average particle diameter of 70 to 90 μm) (floating carrier) were mixed in a double-arm kneader (KDHJ, manufactured by Dalton) for 10 minutes, and then mixed with water and kneaded for 15 minutes. Next, this water-kneaded product was granulated by an extrusion granulator equipped with a basket type screen having a hole diameter of 3.0 mm. The obtained granules were pre-dried, sized with a drum type granulator, and dried with a fluidized bed drier. This was sieved at 3.35 mm to 2.00 mm to obtain a water-floating pesticide formulation. The particle size of the obtained preparation was 83% in the range of 2.80 to 1.70 mm, the ratio of major axis / minor axis at the bottom was 1.2, and the number of particles per 1 g was 132.

[Example 125]
The formulation composition was 10.0 parts of ipfencarbazone (herbicidally active ingredient), 25.0 parts of ceramic balloon (average particle diameter of 20 to 150 μm) (floating carrier), polyoxyalkylene alkyl ether phosphate ester salt (alkylene group: 2, 4 carbon atoms, alkyl group: n-octyl, number of ester bonds: 2, cation: H ⁺ ) 4.0 parts, propylene glycol 1.5 parts, dialkyl succinate sulfonic acid Na 2.5 parts, acrylic acid- Methacrylic acid copolymer Na 2.0 parts, dextrin 6.0 parts, perlite 30.0 parts, clay 19.0 parts (of which the composition used for the slurry was 10.0 parts of ipfencarbazone, dialkyl succinate sulfonic acid Na 1.0 part, water 14.0 parts), the particle size was 3.0 mm, and a water-floating pesticide formulation was prepared according to Example 124. . The particle size of the obtained preparation was 86% in the range of 2.80 to 1.70 mm, and the ratio of major axis / minor axis at the bottom surface was 1.3, and the number of particles per gram was 102.

[Example 126]
Formulation composition is 10.0 parts of ipfencarbazone (herbicidally active ingredient), 30.0 parts of fly ash balloon (average particle size: 20 to 150 μm) (floating carrier), polyoxyalkylene alkyl ether phosphate salt (alkylene group) : 2, 4 carbon atoms, alkyl group: 2-ethylhexyl, number of ester bonds: 1, cation: Na ⁺ ) 6.0 parts, propylene glycol 3.0 parts, dialkyl succinate sulfonic acid Na 2.5 parts, acrylic acid -Vinyl sulfonic acid copolymer Na 2.0 parts, methyl cellulose 3.0 parts, perlite 27.0 parts, clay 16.5 parts (the composition used for the slurry was 10.0 parts of ipfencarbazone, dialkyl succinate (Sulfonate Na: 1.0 part, water: 14.0 parts), particle size: 3.0 mm, floating on the water surface according to Example 124 A pesticide formulation was prepared. The particle size of the obtained preparation was 87% in the range of 2.80 to 1.70 mm, and the ratio of major axis / minor axis at the bottom surface was 1.4, and the number of particles per 1 g was 105.

[Example 127]
Formulation composition is 10.0 parts of ipfencarbazone (herbicidal active ingredient), 2.5 parts of acrylonitrile resin balloon (average particle diameter of 20 to 40 μm) (floating carrier), polyoxyalkylene alkyl ether phosphate salt (alkylene group) : C2, alkyl group: 2-ethylhexyl, number of ester bonds: 2, cation: Na ⁺ ) 10.0 parts, propylene glycol 2.0 parts, alkylnaphthalenesulfonic acid Na2.5 parts, acrylic acid-vinylsulfone 2.0 parts of acid copolymer Na, 3.0 parts of methylcellulose, 40.0 parts of perlite, 30.0 parts of bentonite (the composition used for the slurry was 10.0 parts of ipfencarbazone, Na1 of alkylnaphthalenesulfonic acid). 0 parts, water 14.0 parts), and the particle size is 3.0 mm. A pesticide formulation was prepared. The particle size of the obtained preparation was 86% in the range of 2.80 to 1.70 mm, the ratio of major axis / minor axis at the bottom was 1.2, and the number of particles per gram was 118.

[Example 128]
The formulation composition was 10.0 parts of ipfencarbazone (herbicidally active ingredient), 25.0 parts of ceramic balloon (average particle diameter of 20 to 150 μm) (floating carrier), polyoxyalkylene alkyl ether phosphate ester salt (alkylene group: 2, 4 carbon atoms, alkyl group: n-decyl, number of ester bonds: 1, cation: Na ⁺ ) 8.0 parts, butylene glycol 2.0 parts, alkylnaphthalenesulfonic acid Na 2.5 parts, acrylic acid-maleic 2.0 parts of acid copolymer Na, 6.0 parts of dextrin, 26.0 parts of diatomaceous earth, 18.5 parts of bentonite (the composition used for the slurry was 10.0 parts of ipfencarbazone, 1 part of alkylnaphthalenesulfonic acid Na1. 0, water 14.0 parts) and the particle size of 3.0 mm, and a water-floating pesticide formulation was prepared according to Example 124. The particle size of the obtained preparation was 84% in the range of 2.80 to 1.70 mm, the ratio of major axis / minor axis at the bottom was 1.2, and the number of particles per 1 g was 99.

[Example 129]
Formulation composition is 10.0 parts of ipfencarbazone (herbicidally active ingredient), 30.0 parts of fly ash balloon (average particle diameter: 80 to 120 μm) (floating carrier), polyoxyalkylene alkyl ether phosphate (alkylene group) : 2, 4 carbon atoms, alkyl group: n-decyl, number of ester bonds: 2, cation: Na ⁺ ) 12.0 parts, propylene glycol 3.0 parts, alkylnaphthalenesulfonic acid Na 2.5 parts, methyl cellulose 3. 0 parts, diatomaceous earth 26.0 parts, clay 13.5 parts (of which the composition used for the slurry is 10.0 parts of ipfencarbazone, 1.0 part of sodium alkylnaphthalenesulfonate, 14.0 parts of water), granulation A water-susceptible pesticide formulation having a diameter of 3.0 mm was prepared in accordance with Example 124. The particle size of the obtained preparation was 87% in the range of 2.80 to 1.70 mm, the ratio of major axis / minor axis at the bottom was 1.5, and the number of particles per 1 g was 143.

[Example 130]
The formulation composition was 10.0 parts of ipfencarbazone (herbicidally active ingredient), 25.0 parts of shirasu balloon (average particle diameter of 70 to 90 μm) (floating carrier), polyoxyalkylene alkyl ether phosphate salt (alkylene group: C2, C3, C4, alkyl group: isodecyl, number of ester bonds: 1, cation: K ⁺ ) 12.0 parts, propylene glycol 2.5 parts, dialkyl succinate sulfonic acid Na 2.5 parts, polyacrylic acid 2.0 parts of Na, 6.0 parts of dextrin, 25.0 parts of white carbon, 15.0 parts of bentonite (of which the composition used for the slurry was 10.0 parts of ipfencarbazone, 1.0 part of dialkylsuccinatesulfonic acid Na) , Water 14.0 parts) and a particle size of 2.8 mm, and a water-floating pesticide formulation was prepared according to Example 124. The particle size of the obtained preparation was 85% in the range of 2.80 to 1.70 mm, and the ratio of major axis / minor axis at the bottom surface was 1.3, and the number of particles per gram was 85.

[Example 131]
Formulation composition was 10.0 parts of ipfencarbazone (herbicidally active ingredient), 25.0 parts of fly ash balloon (average particle size: 80 to 120 μm) (floating carrier), polyoxyalkylene alkyl ether phosphate (alkylene group) : C2,4, alkyl group: isodecyl, number of ester bonds: 2, cation: K ⁺ ) 10.0 parts, propylene glycol 3.0 parts, alkylnaphthalenesulfonic acid Na 2.5 parts, acrylic acid-methacrylic acid 2.0 parts of copolymer Na, 6.0 parts of dextrin, 25.0 parts of diatomaceous earth, 16.5 parts of bentonite (of which the composition used for the slurry was 10.0 parts of ipfencarbazone, 1.0 part of alkylnaphthalenesulfonic acid Na1.0) Parts, water 14.0 parts), the particle size was 2.8 mm, and a water-floating pesticide formulation was prepared according to Example 124. The particle size of the obtained preparation was 84% in the range of 2.80 to 1.70 mm, and the ratio of major axis / minor axis at the bottom surface was 1.6, and the number of particles per gram was 180.

[Example 132]
The formulation composition was 10.0 parts of ipfencarbazone (herbicidally active ingredient), 25.0 parts of shirasu balloon (average particle diameter of 70 to 90 μm) (floating carrier), polyoxyalkylene alkyl ether phosphate salt (alkylene group: C2, C4, alkyl group: 2-ethylhexyl, number of ester bonds: 1, cation: Na ⁺ ) 6.0 parts, polyoxyalkylene alkyl ether phosphate salt (alkylene group: C2, alkyl group: 2-ethylhexyl, number of ester bonds: 2, cation: Na ⁺ ) 6.0 parts, propylene glycol 2.5 parts, alkylnaphthalenesulfonic acid Na 2.5 parts, acrylic acid-vinylsulfonic acid copolymer Na 2.0 parts , 3.0 parts of methylcellulose, 25.0 parts of perlite, 18.0 parts of clay (of which the composition used for the slurry was Flop Fen carbazone 10.0 parts, NA of 1.0 parts of alkylnaphthalene sulfonic acid, 14.0 parts of water), and Zotsubu径 3.0 mm, to prepare a water-floating agrochemical formulations in conformity with Example 124. The particle size of the obtained preparation was 82% in the range of 2.80 to 1.70 mm, the ratio of major axis / minor axis at the bottom was 1.1, and the number of particles per 1 g was 103.

[Example 133]
The formulation composition was 10.0 parts of ipfencarbazone (herbicidally active ingredient), 25.0 parts of ceramic balloon (average particle diameter of 20 to 150 μm) (floating carrier), polyoxyalkylene alkyl ether phosphate ester salt (alkylene group: 2, 3 carbon atoms, alkyl group: n-octyl, number of ester bonds: 1, cation: H ⁺ ) 3.0 parts, polyoxyalkylene alkyl ether phosphate salt (alkylene group: 2, 4 carbon atoms, alkyl) Group: 2-ethylhexyl, number of ester bonds: 1, cation: Na ⁺ ) 3.0 parts, polyoxyalkylene alkyl ether phosphate ester salt (alkylene group: 2,4 carbon atoms, alkyl group: isodecyl, number of ester bonds) : 2, ^cation: K +) 3.0 parts of propylene glycol, 3.0 parts of alkyl naphthalene sulfonate Na 0.5 parts, acrylic acid-methacrylic acid copolymer Na 2.5 parts, methyl cellulose 3.0 parts, white carbon 25.0 parts, bentonite 20.0 parts (the composition used for the slurry was ipfencarbazone 10.5 parts). 0 parts, 1.0 part of sodium alkylnaphthalenesulfonate, 14.0 parts of water) and a particle diameter of 3.0 mm, and a water-floating pesticide formulation was prepared according to Example 124. The particle size of the obtained preparation was 82% in the range of 2.80 to 1.70 mm, the ratio of major axis / minor axis at the bottom was 1.2, and the number of particles per 1 g was 93.

[Example 134]
The formulation composition was 10.0 parts of ipfencarbazone (herbicidally active ingredient), 25.0 parts of ceramic balloon (average particle diameter of 20 to 150 μm) (floating carrier), polyoxyalkylene alkyl ether phosphate ester salt (alkylene group: C2, C4, alkyl group: n-decyl, number of ester bonds: 1, cation: Na ⁺ ) 8.0 parts, polyoxyalkylene alkyl ether phosphate ester salt (alkylene group: C2, C4, alkyl) Group: n-decyl, number of ester bonds: 2, cation: Na ⁺ ) 4.0 parts, propylene glycol 2.0 parts, dialkyl succinate sulfonate 2.5 parts, polyacrylic acid Na 2.0 parts, dextrin 6 2.0 parts, perlite 25.0 parts, clay 15.5 parts (of which the composition used for the slurry was ipfencarbazone 10.0) , NA of 1.0 parts of dialkyl succinate sulfonic acid, 14.0 parts of water), and Zotsubu径 2.8 mm, to prepare a water-floating agrochemical formulations in conformity with Example 124. The particle size of the obtained preparation was 95% in the range of 2.80 to 1.70 mm, and the ratio of major axis / minor axis at the bottom surface was 1.3, and the number of particles per 1 g was 108.

[Example 135]
The formulation was composed of 10.0 parts of ipfencarbazone (herbicidally active ingredient), 25.0 parts of shirasu balloon (average particle size of 90 to 120 μm) (floating carrier), polyoxyalkylene alkyl ether phosphate salt (alkylene group: 2,3,4 carbon atoms, alkyl group: isodecyl, number of ester bonds: 1, cation: K ⁺ ) 10.0 parts, propylene glycol 2.0 parts, alkylnaphthalenesulfonic acid Na 2.5 parts, acrylic acid-maleic 2.0 parts of acid copolymer Na, 6.0 parts of dextrin, 25.0 parts of diatomaceous earth, 17.5 parts of bentonite (of which the composition used for the slurry was 10.0 parts of ipfencarbazone, 1 part of alkylnaphthalenesulfonic acid Na1. 0, water 14.0 parts) and a particle size of 2.8 mm, and a water-floating pesticide formulation was prepared according to Example 124. The particle size of the obtained preparation was 86% in the range of 2.80 to 1.70 mm, and the ratio of major axis / minor axis at the bottom surface was 1.4, and the number of particles per 1 g was 117.

[Example 136]
The formulation composition was 10.0 parts of ipfencarbazone (herbicidally active ingredient), 30.0 parts of shirasu balloon (average particle diameter of 90 to 120 μm) (floating carrier), polyoxyalkylene alkyl ether phosphate ester salt (alkylene group: 2, 4 carbon atoms, alkyl group: isodecyl, number of ester bonds: 2, cation: K ⁺ ) 8.0 parts, propylene glycol 2.0 parts, dialkyl succinate sulfonate Na 2.5 parts, polyacrylic acid Na2. 0 parts, dextrin 6.0 parts, perlite 23.0 parts, clay 16.5 parts (of which the composition used for the slurry was 10.0 parts of ipfencarbazone, 1.0 part of dialkyl succinate sulfonate Na, 14 parts of water 0.0 part), the particle size was 3.0 mm, and a water-floating pesticide formulation was prepared according to Example 124. The particle size of the obtained preparation was 96% in the range of 2.80 to 1.70 mm, the ratio of major axis / minor axis at the bottom was 1.2, and the number of particles per gram was 116.

[Example 137]
The formulation composition was 10.0 parts of ipfencarbazone (herbicidally active ingredient), 25.0 parts of ceramic balloon (average particle size: 20 to 150 μm) (floating carrier), polyoxyalkylene alkyl ether phosphate ester salt (alkylene group: C2, alkyl group: 2-ethylhexyl, number of ester bonds: 2, cation: Na ⁺ ) 10.0 parts, propylene glycol 2.0 parts, alkylnaphthalenesulfonic acid Na2.5 parts, alkylnaphthalenesulfonic acid formaldehyde condensation Product Na3.0 parts, acrylic acid-vinylsulfonic acid copolymer Na2.0 parts, methylcellulose 3.0 parts, perlite 25.0 parts, bentonite 17.5 parts (the composition used for the slurry was ipfencarbazone) 10.0 parts, 1.0 part of sodium alkylnaphthalenesulfonate, 14.0 parts of water ), The particle size was 3.0 mm, and a water-floating pesticide formulation was prepared according to Example 124. The particle size of the obtained preparation was 84% in the range of 2.80 to 1.70 mm, the ratio of major axis / minor axis at the bottom was 1.1, and the number of particles per 1 g was 108.

[Example 138]
The formulation was composed of 10.0 parts of ipfencarbazone (herbicidally active ingredient), 25.0 parts of shirasu balloon (average particle size of 90 to 120 μm) (floating carrier), polyoxyalkylene alkyl ether phosphate salt (alkylene group: 2, 3 carbon atoms, alkyl group: n-octyl, number of ester bonds: 1, cation: H ⁺ ) 6.0 parts, polyoxyalkylene alkyl ether phosphate ester salt (alkylene group: 2, 4 carbon atoms, alkyl) Group: 2-ethylhexyl, number of ester bonds: 1, cation: Na ⁺ ) 6.0 parts, propylene glycol 2.5 parts, alkylnaphthalenesulfonic acid Na2.5 parts, naphthalenesulfonic acid formaldehyde condensate Na3.0 parts, Acrylic acid-methacrylic acid copolymer Na 2.5 parts, dextrin 6.0 parts, diatomaceous earth 25.0 parts, clay 1.5 parts (of which the composition used for the slurry was 10.0 parts of ipfencarbazone, 1.0 part of sodium alkylnaphthalenesulfonate, 14.0 parts of water), and the particle size was 3.0 mm. A water-floating pesticide formulation was prepared according to the standard. The particle size of the obtained preparation was 95% in the range of 2.80 to 1.70 mm, and the ratio of major axis / minor axis at the bottom surface was 1.3, and the number of particles per gram was 156.

[Example 139]
The formulation composition was 10.0 parts of ipfencarbazone (herbicidally active ingredient), 25.0 parts of shirasu balloon (average particle diameter of 70 to 90 μm) (floating carrier), polyoxyalkylene alkyl ether phosphate salt (alkylene group: C2, C4, alkyl group: 2-ethylhexyl, number of ester bonds: 1, cation: Na ⁺ ) 5.0 parts, polyoxyalkylene alkyl ether phosphate salt (alkylene group: C2, alkyl group: 2-ethylhexyl, number of ester bonds: 2, cation: Na ⁺ ) 5.0 parts, propylene glycol 2.5 parts, alkylnaphthalenesulfonic acid Na 2.5 parts, acrylic acid-vinylsulfonic acid copolymer Na 2.0 parts , Polyvinyl alcohol 3.0 parts, white carbon 25.0 parts, bentonite 20.0 parts (including slurry The composition used was 10.0 parts of ipfencarbazone, 1.0 part of sodium alkylnaphthalenesulfonate, 14.0 parts of water), and the particle size was 2.8 mm. Was prepared. The particle size of the obtained preparation was 83% in the range of 2.80 to 1.70 mm, the ratio of major axis / minor axis at the bottom was 1.5, and the number of particles per gram was 178.

[Example 140]
The formulation was composed of 10.0 parts of ipfencarbazone (herbicidally active ingredient), 25.0 parts of shirasu balloon (average particle size of 90 to 120 μm) (floating carrier), polyoxyalkylene alkyl ether phosphate salt (alkylene group: 2, 4 carbon atoms, alkyl group: n-decyl, number of ester bonds: 1, cation: Na ⁺ ) 7.0 parts, polyoxyalkylene alkyl ether phosphate ester salt (alkylene group: 2, 4 carbon atoms, alkyl) Group: n-decyl, number of ester bonds: 2, cation: Na ⁺ ) 3.0 parts, propylene glycol 2.5 parts, dialkyl succinate sulfonic acid Na 2.5 parts, lignin sulfonic acid Na 3.0 parts, acrylic acid 15. Maleic acid copolymer Na 1.5 parts, carboxymethyl cellulose Na 2.0 parts, diatomaceous earth 25.0 parts, bentonite Parts (of which the composition used for the slurry was 10.0 parts of ipfencarbazone, 1.0 part of sodium dialkylsuccinatesulfonate, 14.0 parts of water), and the particle size was 3.0 mm. To prepare a water-floating pesticide formulation. The particle size of the obtained preparation was 95% in the range of 2.80 to 1.70 mm, the ratio of major axis / minor axis at the bottom was 1.2, and the number of particles per gram was 125.

[Example 141]
The formulation was 10.0 parts of ipfencarbazone (herbicidally active ingredient), 25.0 parts of shirasu balloon (average particle size of 90 to 120 μm) (floating carrier), polyoxyalkylene alkyl ether phosphate ester salt (alkylene group: 2,4 carbon atoms, alkyl group: 2-ethylhexyl, number of ester bonds: 1, cation: Na ⁺ ) 10.0 parts, dialkyl succinate sulfonic acid Na 2.5 parts, alkylnaphthalene sulfonic acid formaldehyde condensate Na 3.0 Part, acrylic acid-maleic acid copolymer Na 1.5 parts, carboxymethyl cellulose Na 3.0 parts, diatomaceous earth 22.0 parts, bentonite 23.0 parts (the composition used for the slurry was 10.0 parts of ipfencarbazone) , 1.0 part of sodium dialkyl succinatesulfonate, 14.0 parts of water), particle size 3.0 m m, and a water-floating pesticide formulation was prepared according to Example 124. The particle size of the obtained preparation was 95% in the range of 2.80 to 1.70 mm, and the ratio of major axis / minor axis at the bottom was 1.3, and the number of particles per gram was 58.

[Example 142]
The formulation composition was 10.0 parts of ipfencarbazone (herbicidally active ingredient), 25.0 parts of shirasu balloon (average particle size of 90 to 120 μm) (floating carrier), 2.5 parts of propylene glycol, Na2 dialkyl succinate sulfonate. 0.5 parts, alkyl naphthalene sulfonic acid formaldehyde condensate Na 3.0 parts, acrylic acid-vinyl sulfonic acid copolymer Na 2.0 parts, carboxymethyl cellulose Na 3.0 parts, diatomaceous earth 35.0 parts, bentonite 17.0 parts (including The composition used for the slurry was 10.0 parts of ipfencarbazone, 1.0 part of sodium dialkylsuccinatesulfonate, 14.0 parts of water), the particle size was 3.0 mm, and the water surface was floated according to Example 124. A pesticide formulation was prepared. The particle size of the obtained preparation was 91% in the range of 2.80 to 1.70 mm, the ratio of major axis / minor axis at the bottom was 1.2, and the number of particles per gram was 112.

[Example 143]
After mixing 10.0 parts of ipfencarbazone (herbicidally active ingredient), 1.0 part of sodium dialkylsuccinatesulfonate, and 14.0 parts of water, the mixture was adjusted to an average particle diameter of 1.0 μm with Dynomill (manufactured by Shinmaru Enterprises). Wet pulverization was carried out until a slurry was obtained. In addition, 18.0 parts of benfresate (herbicidal active ingredient), polyoxyalkylene alkyl ether phosphate ester salt (alkylene group: 2, 3 carbon atoms, alkyl group: n-octyl, number of ester bonds: 1, cation: Na ⁺ ) 12.0 parts, propylene glycol 2.5 parts, dialkyl succinate sulfonate Na 1.5 parts, methyl cellulose 3.0 parts, white carbon 18.0 parts, bentonite 9.0 parts were prepared with a hammer mill (Sample Mill KIIW-1). And Dalton Co., Ltd.) to obtain a powder mixture. 25.0 parts of the slurry, the powder mixture, and the fly ash balloon (average particle size: 80 to 120 μm) (floating carrier) were mixed for 10 minutes in a double-arm kneader (KDHJ, manufactured by Dalton), and then kneaded with water for 15 minutes. Next, this water-kneaded product was granulated by an extrusion granulator equipped with a basket type screen having a hole diameter of 3.0 mm. The obtained granules were pre-dried, sized with a drum type granulator, and dried with a fluidized bed drier. This was sieved at 3.35 mm to 2.00 mm to obtain a water-floating pesticide formulation. The particle size of the obtained preparation was 86% in the range of 2.80 to 1.70 mm, the ratio of major axis / minor axis at the bottom was 1.1, and the number of particles per 1 g was 78.

[Example 144]
The formulation composition was 10.0 parts of ipfencarbazone (herbicidally active ingredient), 18.0 parts of benfresate (herbicidally active ingredient), 28.0 parts of shirasu balloon (average particle diameter 70 to 90 μm) (floating carrier), polyoxy Alkylene alkyl ether phosphate salt (alkylene group: 2, 3, 4, carbon atoms, alkyl group: n-octyl, ester bond number: 2, cation: Na ⁺ ) 6.0 parts, hexylene glycol 2.0 parts , 2.5 parts of sodium alkylnaphthalenesulfonate, 2.0 parts of sodium polyacrylate, 6.0 parts of dextrin, 15.0 parts of calcium silicate, 10.5 parts of bentonite (the composition used for the slurry was ipfencarbazone) 10.0 parts, 1.0 part of sodium alkylnaphthalenesulfonate, 14.0 parts of water), 2.8 mm in particle diameter, and according to Example 143. A waterborne pesticide formulation was prepared. The particle size of the obtained preparation was 87% in the range of 2.80 to 1.70 mm, and the ratio of major axis / minor axis at the bottom surface was 1.3, and the number of particles per gram was 89.

[Example 145]
The formulation was composed of 10.0 parts of ipfencarbazone (herbicidally active ingredient), 18.0 parts of benfresate (herbicidally active ingredient), 28.0 parts of ceramic balloon (average particle diameter of 20 to 150 μm) (floating carrier), polyoxy Alkylene alkyl ether phosphate ester salt (alkylene group: 2,4 carbon atoms, alkyl group: 2-ethylhexyl, number of ester bonds: 1, cation: K ⁺ ) 6.0 parts, propylene glycol 3.0 parts, alkylnaphthalene 2.5 parts of sodium sulfonic acid, 1.5 parts of acrylic acid-vinyl sulfonic acid copolymer Na, 6.0 parts of dextrin, 18.0 parts of calcium silicate, 7.0 parts of clay (of which the composition used for the slurry is ip 10.0 parts of phencarbazone, 1.0 part of sodium alkylnaphthalenesulfonate, 14.0 parts of water), and a particle size of 2.8 mm. A water-floating pesticide formulation was prepared according to Example 143. The particle size of the obtained preparation was 83% in the range of 2.80 to 1.70 mm, the ratio of major axis / minor axis at the bottom was 1.5, and the number of particles per 1 g was 96.

[Example 146]
The formulation was 10.0 parts of ipfencarbazone (herbicidal active ingredient), 18.0 parts of benfresate (herbicidal active ingredient), 25.0 parts of fly ash balloon (average particle diameter of 80 to 120 μm) (floating carrier), Oxyalkylene alkyl ether phosphate ester salt (alkylene group: carbon number 2, alkyl group: 2-ethylhexyl, ester bond number: 2, cation: K ⁺ ) 10.0 parts, propylene glycol 2.0 parts, dialkyl succinate 2.5 parts of sodium sulfonate, 3.0 parts of methylcellulose, 18.0 parts of white carbon, 11.5 parts of bentonite (of which the composition used for the slurry was 10.0 parts of ipfencarbazone, Na1 of dialkyl succinate sulfonate) 0 parts, water 14.0 parts), the particle size is 3.0 mm, and the water surface floats according to Example 143. A pesticide formulation was prepared. The particle size of the obtained preparation was 85% in the range of 2.80 to 1.70 mm, and the ratio of major axis / minor axis at the bottom was 1.3, and the number of particles per gram was 105.

[Example 147]
The formulation was composed of 10.0 parts of ipfencarbazone (herbicidally active ingredient), 18.0 parts of benfresate (herbicidally active ingredient), 28.0 parts of ceramic balloon (average particle diameter of 20 to 150 μm) (floating carrier), polyoxy Alkylene alkyl ether phosphate salt (alkylene group: 2, 3, 4, carbon atoms, alkyl group: n-decyl, number of ester bonds: 1, cation: Na ⁺ ) 10.0 parts, propylene glycol 2.0 parts, 2.5 parts of sodium dialkylsuccinatesulfonate, 1.0 part of Na of acrylic acid-vinylsulfonic acid copolymer, 3.0 parts of methylcellulose, 18.0 parts of white carbon, 7.5 parts of bentonite (the composition used for the slurry was , 10.0 parts of ipfencarbazone, 1.0 part of sodium dialkylsuccinatesulfonate, 14.0 parts of water), particle size A water-floating pesticide formulation was prepared according to Example 143, with the thickness being 3.0 mm. The particle size of the obtained preparation was 84% in the range of 2.80 to 1.70 mm, and the ratio of major axis / minor axis at the bottom surface was 1.4, and the number of particles per gram was 118.

[Example 148]
The formulation composition was 10.0 parts of ipfencarbazone (herbicidally active ingredient), 18.0 parts of benfresate (herbicidally active ingredient), 25.0 parts of shirasu balloon (average particle diameter of 70 to 90 μm) (floating carrier), polyoxy 12.0 parts of an alkylene alkyl ether phosphate salt (alkylene group: 2, 3, 4, carbon atoms, alkyl group: n-decyl, number of ester bonds: 2, cation: Na ⁺ ), 2.5 parts of propylene glycol, 2.5 parts of sodium alkylnaphthalenesulfonate, 3.0 parts of methylcellulose, 20.0 parts of calcium silicate, 7.0 parts of clay (the composition used for the slurry was 10.0 parts of ipfencarbazone, alkylnaphthalenesulfonic acid (1.0 part of Na, 14.0 parts of water), the particle size was 3.0 mm, and a water-floating pesticide formulation was prepared according to Example 143. The particle size of the obtained preparation was 86% in the range of 2.80 to 1.70 mm, the ratio of major axis / minor axis at the bottom was 1.2, and the number of particles per 1 g was 93.

[Example 149]
The formulation was 10.0 parts of ipfencarbazone (herbicidal active ingredient), 18.0 parts of benfresate (herbicidal active ingredient), 25.0 parts of fly ash balloon (average particle diameter of 80 to 120 μm) (floating carrier), Oxyalkylene alkyl ether phosphate ester salt (alkylene group: 2, 3, 4, carbon atoms, alkyl group: isodecyl, number of ester bonds: 1, cation: H ⁺ ) 12.0 parts, propylene glycol 3.0 parts, dialkyl 2.5 parts of sodium succinatesulfonate, 2.0 parts of acrylic acid-maleic acid copolymer Na, 3.0 parts of methylcellulose, 18.0 parts of white carbon, 6.5 parts of clay (the composition used for the slurry was ip Phencarbazone 10.0 parts, dialkyl succinatesulfonate Na 1.0 part, water 14.0 parts), particle size 3.0 mm In accordance with Example 143, a water-floating pesticide formulation was prepared. The particle size of the obtained preparation was 83% in the range of 2.80 to 1.70 mm, and the ratio of major axis / minor axis at the bottom was 1.3, and the number of particles per gram was 82.

[Example 150]
Formulation composition was 10.0 parts of ipfencarbazone (herbicidally active ingredient), 18.0 parts of benfresate (herbicidally active ingredient), 2.5 parts of acrylonitrile resin balloon (average particle diameter of 20 to 40 μm) (floating carrier), Oxyalkylene alkyl ether phosphate salt (alkylene group: 2, 3, 4, carbon atoms, alkyl group: isodecyl, ester bond number: 2, cation: H ⁺ ) 12.0 parts, propylene glycol 2.0 parts, alkyl Naphthalenesulfonic acid Na 2.5 parts, acrylic acid-methacrylic acid copolymer Na 2.0 parts, dextrin 6.0 parts, calcium silicate 20.0 parts, bentonite 25.0 parts (the composition used for the slurry was ip Phencarbazone 10.0 parts, alkylnaphthalenesulfonate Na 1.0 part, water 14.0 parts), particle size 2.8 mm In accordance with Example 143, a water-floating pesticide formulation was prepared. The particle size of the obtained preparation was 85% in the range of 2.80 to 1.70 mm, and the ratio of major axis / minor axis at the bottom surface was 1.4, and the number of particles per 1 g was 73.

[Example 151]
The formulation composition was 10.0 parts of ipfencarbazone (herbicidal active ingredient), 18.0 parts of benfresate (herbicidal active ingredient), 25.0 parts of ceramic balloon (average particle diameter of 20 to 150 μm) (floating carrier), polyoxy 10.0 parts of alkylene alkyl ether phosphate salt (alkylene group: 2,4 carbon atoms, alkyl group: 2-ethylhexyl, number of ester bonds: 1, cation: K ⁺ ) 10.0 parts, polyoxyalkylene alkyl ether phosphate salt (Alkylene group: carbon number 2, alkyl group: 2-ethylhexyl, ester bond number: 2, cation: K ⁺ ) 2.0 parts, propylene glycol 2.0 parts, dialkyl succinate sulfonic acid Na 2.5 parts, acrylic Acid-vinyl sulfonic acid copolymer Na 1.5 parts, methyl cellulose 3.0 parts, white carbon 18 0 parts, bentonite 8.0 parts (of which the composition used for the slurry was 10.0 parts of ipfencarbazone, 1.0 part of sodium dialkylsuccinatesulfonate, 14.0 parts of water), and the particle size was 3.0 mm. A water-floating pesticide formulation was prepared according to Example 143. The particle size of the obtained preparation was 84% in the range of 2.80 to 1.70 mm, the ratio of major axis / minor axis at the bottom was 1.2, and the number of particles per 1 g was 75.

[Example 152]
The formulation composition was 10.0 parts of ipfencarbazone (herbicidal active ingredient), 18.0 parts of benfresate (herbicidal active ingredient), 25.0 parts of ceramic balloon (average particle diameter of 20 to 150 μm) (floating carrier), polyoxy 3.0 parts of alkylene alkyl ether phosphate salt (alkylene group: 2, 3 carbon atoms, alkyl group: n-octyl, number of ester bonds: 1, cation: Na ⁺ ), 3.0 parts of polyoxyalkylene alkyl ether phosphate salt (Alkylene group: 2,4 carbon atoms, alkyl group: 2-ethylhexyl, number of ester bonds: 1, cation: K ⁺ ) 3.0 parts, polyoxyalkylene alkyl ether phosphate salt (alkylene group: 2 carbon atoms) , 3,4, alkyl group: isodecyl ester bonds: 2, ^cations: H +) 3.0 parts of propylene glycol 3.0 parts, sodium alkylnaphthalenesulfonate 2.5 parts, acrylic acid-maleic acid copolymer Na 1.0 part, methylcellulose 3.0 parts, white carbon 18.0 parts, bentonite 10.5 parts (including slurry The composition used was 10.0 parts of ipfencarbazone, 1.0 part of sodium alkylnaphthalenesulfonate, 14.0 parts of water), the particle size was 3.0 mm, and the water-floating pesticide formulation according to Example 143. Was prepared. The particle size of the obtained preparation was 82% in the range of 2.80 to 1.70 mm, and the ratio of major axis / minor axis at the bottom surface was 1.6, and the number of particles per gram was 78.

[Example 153]
The formulation was 10.0 parts of ipfencarbazone (herbicidal active ingredient), 18.0 parts of benfresate (herbicidal active ingredient), 25.0 parts of fly ash balloon (average particle diameter of 80 to 120 μm) (floating carrier), Oxyalkylene alkyl ether phosphate ester salt (alkylene group: 2, 3, 4 carbon atoms, alkyl group: n-octyl, number of ester bonds: 2, cation: Na ⁺ ) 10.0 parts, propylene glycol 1.5 parts 2.5 parts of sodium alkylnaphthalenesulfonate, 2.0 parts of sodium polyacrylate, 6.0 parts of dextrin, 18.0 parts of white carbon, 7.0 parts of clay (of which the composition used for the slurry was ipfencarbazone 10 2.0 parts, 1.0 part of sodium alkylnaphthalenesulfonate, 14.0 parts of water), and a particle diameter of 3.0 mm, according to Example 143. Thus, a water-floating pesticide formulation was prepared. The particle size of the obtained preparation was 93% in the range of 2.80 to 1.70 mm, the ratio of major axis / minor axis at the bottom was 1.1, and the number of particles per 1 g was 83.

[Example 154]
The formulation composition was 10.0 parts of ipfencarbazone (herbicidally active ingredient), 18.0 parts of benfresate (herbicidally active ingredient), 28.0 parts of shirasu balloon (average particle size of 90 to 120 μm) (floating carrier), polyoxy 4.0 parts of an alkylene alkyl ether phosphate salt (alkylene group: 2,4 carbon atoms, alkyl group: 2-ethylhexyl, number of ester bonds: 1, cation: K ⁺ ) 4.0 parts, polyoxyalkylene alkyl ether phosphate salt (Alkylene group: 2, 3, 4, carbon atoms, alkyl group: n-decyl, number of ester bonds: 2, cation: Na ⁺ ) 6.0 parts, propylene glycol 1.5 parts, alkylnaphthalenesulfonic acid Na2.5 Parts, acrylic acid-vinyl sulfonic acid copolymer Na 2.0 parts, methyl cellulose 3.0 parts, calcium silicate 18.0 parts, Example 143 was prepared with 7.0 parts of tontonite (of which the composition used for the slurry was 10.0 parts of ipfencarbazone, 1.0 part of sodium alkylnaphthalenesulfonate, 14.0 parts of water), and the particle size was 3.0 mm. A water-floating pesticide formulation was prepared according to the standard. The particle size of the obtained preparation was 83% in the range of 2.80 to 1.70 mm, the ratio of major axis / minor axis at the bottom was 1.2, and the number of particles per 1 g was 86.

[Example 155]
The formulation composition was 10.0 parts of ipfencarbazone (herbicidally active ingredient), 18.0 parts of benfresate (herbicidally active ingredient), 25.0 parts of shirasu balloon (average particle size of 90 to 120 μm) (floating carrier), polyoxy 5.0 parts of alkylene alkyl ether phosphate salt (alkylene group: 2, 3 carbon atoms, alkyl group: n-octyl, number of ester bonds: 1, cation: Na ⁺ ), 5.0 parts, polyoxyalkylene alkyl ether phosphate salt (Alkylene group: 2, 3, 4 carbon atoms, alkyl group: n-decyl, number of ester bonds: 1, cation: Na ⁺ ) 2.5 parts, polyoxyalkylene alkyl ether phosphate salt (alkylene group: carbon number 2,3,4, alkyl group: isodecyl ester bonds: 2, ^cations: H +) 2.5 parts propylene glycol 2 0 parts, 2.5 parts of sodium alkylnaphthalenesulfonate, 2.5 parts of sodium polyacrylate, 3.0 parts of methylcellulose, 18.0 parts of calcium silicate, 9.0 parts of clay (the composition used for the slurry was ipfen) 10.0 parts of carbazone, 1.0 part of sodium alkylnaphthalenesulfonate, 14.0 parts of water) and a particle diameter of 2.8 mm were prepared according to Example 143 to prepare a water-floating pesticide formulation. The particle size of the obtained preparation was 95% in the range of 2.80 to 1.70 mm, the ratio of major axis / minor axis at the bottom was 1.1, and the number of particles per 1 g was 85.

[Example 156]
The formulation composition was 10.0 parts of ipfencarbazone (herbicidally active ingredient), 18.0 parts of benfresate (herbicidally active ingredient), 25.0 parts of shirasu balloon (average particle diameter of 70 to 90 μm) (floating carrier), polyoxy Alkylene alkyl ether phosphate salt (alkylene group: 2,4 carbon atoms, alkyl group: 2-ethylhexyl, number of ester bonds: 1, cation: K ⁺ ) 10.0 parts, propylene glycol 2.5 parts, alkylnaphthalene 2.5 parts of sodium sulfonic acid, 3.0 parts of naphthalenesulfonic acid formaldehyde condensate Na, 1.5 parts of acrylic acid-maleic acid copolymer Na, 3.0 parts of methylcellulose, 18.0 parts of white carbon, 6.5 parts of bentonite ( The composition used for the slurry was 10.0 parts of ipfencarbazone, alkylnaphthalene sulfone (Acid Na: 1.0 part, water: 14.0 parts), the particle size was 3.0 mm, and a water-floating pesticide formulation was prepared according to Example 143. The particle size of the obtained preparation was 86% in the range of 2.80 to 1.70 mm, the ratio of major axis / minor axis at the bottom was 1.2, and the number of particles per 1 g was 93.

[Example 157]
The formulation composition was 10.0 parts of ipfencarbazone (herbicidally active ingredient), 18.0 parts of benfresate (herbicidally active ingredient), 25.0 parts of shirasu balloon (average particle size of 90 to 120 μm) (floating carrier), polyoxy Alkylene alkyl ether phosphate salt (alkylene group: 2, 3, 4, carbon atoms, alkyl group: n-octyl, number of ester bonds: 2, cation Na ⁺ ) 8.0 parts, propylene glycol 3.0 parts, dialkyl 2.5 parts of sodium succinatesulfonate, 3.0 parts of Na of alkylnaphthalenesulfonic acid formaldehyde condensate, 1.0 part of acrylic acid-methacrylic acid copolymer Na, 3.0 parts of methylcellulose, 18.0 parts of white carbon, and bentonite 5 parts (of which the composition used for the slurry was 10.0 parts of ipfencarbazone, 1.0 part of sodium sinate sulfonate, 14.0 parts of water) and a particle size of 3.0 mm were prepared according to Example 143 to prepare a water-floating pesticide formulation. The particle size of the obtained preparation was 94% in the range of 2.80 to 1.70 mm, and the ratio of major axis / minor axis at the bottom surface was 1.3, and the number of particles per 1 g was 120.

[Example 158]
The formulation was 10.0 parts of ipfencarbazone (herbicidal active ingredient), 18.0 parts of benfresate (herbicidal active ingredient), 25.0 parts of fly ash balloon (average particle diameter of 80 to 120 μm) (floating carrier), 5.0 parts of oxyalkylene alkyl ether phosphoric acid ester salt (alkylene group: 2, 3, 4 carbon atoms, alkyl group: n-octyl, number of ester bonds: 2, cation Na ⁺ ), polyoxyalkylene alkyl ether phosphoric acid Ester salt (alkylene group: 2,4 carbon atoms, alkyl group: 2-ethylhexyl, ester bond number: 1, cation K ⁺ ) 5.0 parts, propylene glycol 3.0 parts, alkylnaphthalenesulfonic acid Na 2.5 parts , Acrylic acid-vinyl sulfonic acid copolymer Na 3.0 parts, polyvinyl alcohol 3.0 parts, white carbon 1 2.0 parts, clay 7.5 parts (of which the composition used for the slurry is 10.0 parts of ipfencarbazone, 1.0 part of sodium alkylnaphthalenesulfonate, 14.0 parts of water), and the particle size is 3.0 mm. A water-floating pesticide formulation was prepared according to Example 143. The particle size of the obtained preparation was 84% in the range of 2.80 to 1.70 mm, the ratio of major axis / minor axis at the bottom was 1.2, and the number of particles per 1 g was 100.

[Example 159]
The formulation composition was 10.0 parts of ipfencarbazone (herbicidally active ingredient), 18.0 parts of benfresate (herbicidally active ingredient), 25.0 parts of shirasu balloon (average particle size of 90 to 120 μm) (floating carrier), polyoxy 4.5 parts of an alkylene alkyl ether phosphate salt (alkylene group: having 2 carbon atoms, alkyl group: 2-ethylhexyl, number of ester bonds: 2, cation K ⁺ ), polyoxyalkylene alkyl ether phosphate salt (alkylene group) : C2, 3, 4, alkyl group: n-decyl, number of ester bonds: 1, cation Na ⁺ ) 4.5 parts, propylene glycol 2.0 parts, alkylnaphthalenesulfonic acid Na2.5 parts, lignin sulfone Acid 3.0 parts, acrylic acid-methacrylic acid copolymer Na 2.0 parts, carboxymethyl cellulose Na3. Part, white carbon 18.0 parts, bentonite 7.5 parts (of which the composition used for the slurry was 10.0 parts of ipfencarbazone, 1.0 part of sodium alkylnaphthalenesulfonate, 14.0 parts of water), granulation A water-floating pesticide formulation was prepared according to Example 143 with a diameter of 3.0 mm. The particle size of the obtained preparation was 97% in the range of 2.80 to 1.70 mm, the ratio of major axis / minor axis at the bottom was 1.2, and the number of particles per 1 g was 90.

[Example 160]
The formulation composition was 10.0 parts of ipfencarbazone (herbicidally active ingredient), 18.0 parts of benfresate (herbicidally active ingredient), 25.0 parts of shirasu balloon (average particle size of 90 to 120 μm) (floating carrier), polyoxy Alkylene alkyl ether phosphate ester salt (alkylene group: 2, 3, 4 carbon atoms, alkyl group: n-decyl, number of ester bonds: 2, cation Na ⁺ ) 10.0 parts, alkyl naphthalene sulfonic acid Na 2.5 parts , Naphthalenesulfonic acid formaldehyde condensate Na 3.0 parts, acrylic acid-vinylsulfonic acid copolymer Na 2.0 parts, carboxymethylcellulose Na 3.0 parts, white carbon 17.0 parts, bentonite 9.5 parts (used for slurry The composition thus obtained was 10.0 parts of ipfencarbazone, and 1.0 part of sodium alkylnaphthalenesulfonate. Parts, water 14.0 parts) and the particle size 3.0 mm, and a water-floating pesticide formulation was prepared according to Example 143. The particle size of the obtained preparation was 93% in the range of 2.80 to 1.70 mm, and the ratio of major axis / minor axis at the bottom surface was 1.4, and the number of particles per gram was 102.

[Example 161]
The pharmaceutical composition was 10.0 parts of ipfencarbazone (herbicidally active ingredient), 18.0 parts of benfresate (herbicidally active ingredient), 25.0 parts of shirasu balloon (average particle size of 90 to 120 μm) (floating carrier), propylene glycol 3.0 parts, alkylnaphthalenesulfonic acid Na2.5 parts, naphthalenesulfonic acid formaldehyde condensate Na3.0 parts, acrylic acid-methacrylic acid copolymer Na2.0 parts, carboxymethylcellulose Na3.0 parts, white carbon 21.5 Parts, clay 12.0 parts (of which the composition used for the slurry was 10.0 parts of ipfencarbazone, 1.0 part of sodium alkylnaphthalenesulfonate, 14.0 parts of water), and the particle size was 3.0 mm. A water-floating pesticide formulation was prepared according to Example 143. The particle size of the obtained preparation was 95% in the range of 2.80 to 1.70 mm, and the ratio of major axis / minor axis at the bottom surface was 1.3, and the number of particles per 1 g was 86.

Next, the usefulness of the water-floating pesticide formulation of the present invention is shown by test examples.
<Diffusion test 1 (confirmation of diffusivity under shallow water depth and tailwind conditions)>
Paddy fields after paddy rice transplantation were separated by corrugated sheet so that the area of one section would be 100 square meters (4m x 25m, flooding depth 2cm). Example, comparative example from one side of 4m side under tail wind 2-3m / s. 25 g of a sample prepared according to the above-mentioned method was processed, and the following three items were investigated.
(1) The longest visual reach of the preparation 15 minutes after application (2) Presence or absence of sediment at the application point 15 minutes after application The sediment was evaluated according to the following standard table.

(3) Next, 48 hours after the treatment, the formulation sample was placed in a sampled water sampled at a sampling point of 20 mL at 1 m intervals starting from the spraying point in the test plot, and in a 1 m 2 (1 mx 1 m, flooded depth 2 cm) test plot created separately. The active ingredient concentration in the sampled liquid 48 hours after the 0.25 g was uniformly sprayed was quantified by high performance liquid chromatography (HPLC) or gas chromatography (GC). The amount of the substance was also quantified, converted to the concentration of the pesticidal active ingredient, and summed), and the diffusion rate (%) at each point was calculated by the following equation (2).

拡散 The maximum distance of the point where the diffusion rate was 90% or more was defined as the diffusion distance, and the diffusivity was evaluated. In addition, this test was performed on a product immediately after preparation and a product stored at 40 ° C. for 90 days (equivalent to storage at room temperature for 3 years).

<Diffusion test 2 (confirmation of diffusivity under shallow water depth and no wind conditions)>
Separate with a corrugated sheet so that the area of one section is 120 square meters (4 mx 30 m, immersion depth 2 cm), and treat 30 g of a sample prepared according to the example from one side of 4 m side under no wind conditions under the following conditions. The items were surveyed.
(1) The longest visual reach of the preparation 15 minutes after spraying (2) Presence or absence of sediment at the spraying point 15 minutes after spraying The sediment was evaluated according to the above standard table.
(3) Next, 24 hours after the treatment, the above-mentioned test solution was applied to a sampled water sampled at a spraying point of the test plot of 20 mL at 1.5 m intervals and a 1 m 2 (1 m × 1 m, flooded depth 2 cm) test plot prepared separately. 0.25 g of the preparation sample was evenly sprayed, and the concentration of the active ingredient in the sampled liquid 24 hours later was quantified by high performance liquid chromatography (HPLC) or gas chromatography (GC). , Decomposed products were also quantified, converted to the concentration of the pesticidal active ingredient, and added up), and the diffusivity (%) at each point was calculated by the above equation (2).

拡散 The maximum distance of the point where the diffusion rate was 90% or more was defined as the diffusion distance, and the diffusivity was evaluated. In addition, this test was performed on a product immediately after preparation and a product stored at 40 ° C. for 150 days (equivalent to storage at room temperature for 5 years).

As a result of the diffusivity test, it can be evaluated that the formulation with less sediment at the application point and the longer the reach of the formulation and the longer the point where the diffusion rate is 90% or more is extended, the more excellent the floating property and the diffusivity. .
The test results are shown in Tables 2-1 to 2-9 (Examples) and Tables 3-1 to 3-5 (Comparative Examples).

<Explanation of table>
(1) Diffusivity test 1 (confirmation of diffusivity under shallow water depth and tailwind conditions)
The sediment was affected by the buoyant carrier, the sodium alkylnaphthalenesulfonate or the sodium dialkylsuccinatesulfonate, the particle size, the ratio of the major axis / minor axis of the bottom of the grains, and the number of grains per gram. In Tables 2-1 to 2-5, in Examples 1 to 85 satisfying all of the requirements, the sediment, the reaching distance of the preparation, and the diffusion distance were within the range in which there was no practical problem. On the other hand, in Comparative Examples in which one of the constituent elements was removed or replaced with a substitute, sediment during preparation or after storage at 40 ° C. for 90 days resulted in a practically problematic result.
In addition, about the Example, the preparation which added any of the alkyl naphthalene sulfonic acid formaldehyde condensate Na, the naphthalene sulfonic acid formaldehyde condensate Na, or the partially desulfonated lignin sulfonic acid Na, the performance after 90 days of 40 degreeC. (Sediment, formulation reach distance, diffusion distance) were suppressed. In addition, the preparation containing sodium carboxymethylcellulose as a binder had improved sediment and diffusion distance as compared with the examples using other binders. The overall diffusivity is as follows: a floating carrier is a Shirasu balloon having an average particle diameter of 90 to 120 μm, sodium alkylnaphthalenesulfonate or sodium dialkylsuccinatesulfonate, and alkylnaphthalenesulfonic acid formaldehyde condensate Na, naphthalenesulfonic acid formaldehyde condensate Na or partially desulfonated lignin sulfonic acid Na, containing carboxymethylcellulose Na as a binder, and having a particle size of at least 90% by weight in the range of 2.80 mm to 1.70 mm; Examples 16, 17, 33, 34, 50, 51, 67, 68, 84, and 85, in which the ratio of major axis / minor axis was 1.1 to 1.4, and the number of particles per 1 g was 50 to 150, immediately after preparation, It was the best including 90 days after 40 ° C.

From the above, in order for the water-floating pesticide formulation to fully demonstrate the diffusivity of the sediment, the formulation reach distance, and the diffusion distance not only immediately after preparation but also after long-term storage, the pesticide active ingredient, floating carrier, alkyl Na naphthalene sulfonate or dialkyl succinate sulfonate, 80% by weight or more in a particle size range of 2.80 mm to 1.70 mm, and a ratio of major axis / minor axis of the bottom surface of the particles of 1.1 to 1.4 per 1 g It is an effective means that the number of particles is from 50 to 150, and further, a shirasu balloon having a particle size of at least 90% by weight in the range of 2.80 mm to 1.70 mm and a floating carrier having an average particle size of 90 to 120 μm is used. That the alkylnaphthalenesulfonic acid formaldehyde condensate Na, the naphthalenesulfonic acid formaldehyde condensate Na, or the partially desulfonated ligninsulfonic acid N It is a more effective means to contain any of a and to contain Na carboxymethylcellulose as a binder.

(2) Diffusivity test 2 (confirmation of diffusivity under shallow water depth and no wind conditions)
Examples 86 to 102, 105 to 121, 124 to 140, and 143 to 159 containing a polyoxyalkylene alkyl ether phosphate ester and a water-soluble alkylene glycol such as propylene glycol are Examples 16 and 17 containing no such component. , 33, 34, 50, 51, 67, 68, 84, 85, 103, 104, 122, 123, 141, 142, 160, 161. As a result, the diffusion distance was more excellent, and the diffusivity was further improved (Tables 2-1 to 2-9).
Further, in the examples containing the polyoxyalkylene alkyl ether phosphate ester salt and propylene glycol, the particle size is particularly 90% by weight or more in the range of 2.80 mm to 1.70 mm, and the floating carrier has an average particle size of 90 to 120 μm. Formulation using shirasu balloon, formulation containing any of alkyl naphthalene sulfonic acid formaldehyde condensate Na, naphthalene sulfonic acid formaldehyde condensate Na or lignin sulfonate, and carboxymethyl cellulose Na or polyvinyl alcohol as binder The preparation was found to have more excellent sediment, preparation reach distance, and diffusion distance at the time of preparation or storage at 40 ° C. for 150 days. The overall diffusivity is as follows: a floating carrier is a Shirasu balloon having an average particle diameter of 90 to 120 μm, sodium alkylnaphthalenesulfonate or sodium dialkylsuccinatesulfonate, and alkylnaphthalenesulfonic acid formaldehyde condensate Na; Na or lignin sulfonate, containing carboxymethylcellulose Na or polyvinyl alcohol as a binder, having a particle size of at least 90% by weight in the range of 2.80 mm to 1.70 mm, and the major axis of the bottom of the grain Examples 102, 121, 140, and 159 having a ratio of minor axis of 1.1 to 1.6 were the most excellent immediately after preparation, including after 150 days at 40 ° C.

From the above, in order for the water-floating pesticide formulation to exhibit the diffusivity combining the sediment, formulation reach distance, and diffusion distance more effectively not only immediately after preparation but also after long-term storage, the pesticide active ingredient, Carrier, polyoxyalkylene alkyl ether phosphoric acid ester salt, and sodium alkylnaphthalenesulfonate or dialkylsuccinatesulfonate, having a particle size of at least 80% by weight in the range of 2.80 mm to 1.70 mm, and the major axis / short axis of the bottom of the particle It is an effective means that the diameter ratio is 1.1 to 1.6, and the number of particles per 1 g is 50 to 200, and further, the particle size is in the range of 2.80 mm to 1.70 mm and 90% by weight or more. That the floating carrier is a shirasu balloon having an average particle diameter of 90 to 120 μm, and that an alkylnaphthalenesulfonic acid formaldehyde condensate Na, naphthalene It is more effective means to contain either the sodium sulfonate formaldehyde condensate or the sodium ligninsulfonate, and to contain sodium carboxymethylcellulose or polyvinyl alcohol as a binder.

Claims

A water-floating pesticide formulation comprising: a) a pesticidal active ingredient; b) a hollow body as a floating carrier; and c) one or more selected from sodium alkylnaphthalenesulfonate and sodium dialkylsuccinatesulfonate as an anionic surfactant. And a water-floating pesticide formulation having the following characteristics:
d) the ratio of major axis / minor axis of the bottom surface of the grains is 1.1 to 1.4;
e) The particle size is at least 80% by weight in the range of 2.80 mm to 1.70 mm, and f) The number of particles per gram is 50 to 150.
E) The water-floating pesticide formulation according to claim 1, wherein the particle size is 90% by weight or more in a range of 2.80 mm to 1.70 mm.
(3) The water-floating pesticide preparation according to any one of (1) and (2), wherein the hollow body as the flotation carrier is a shirasu balloon having an average particle diameter of 90 to 120 μm.
Further, it contains at least one selected from the group consisting of an alkyl naphthalene sulfonic acid formaldehyde condensate Na, a naphthalene sulfonic acid formaldehyde condensate Na, and a partially desulfonated sodium lignin sulfonate as an anionic surfactant. Item 4. The water-floating pesticide preparation according to any one of Items 1 to 3.
(5) The water-floating pesticide preparation according to any one of (1) to (4), further comprising carboxymethylcellulose Na as a binder.
a) an agrochemical active ingredient, b) a hollow body as a floating carrier, c) a polyoxyalkylene alkyl ether phosphate salt and a water-soluble alkylene glycol represented by the following general formula (I), and d) an anionic interface A water-floating pesticide formulation comprising, as an activator, at least one selected from sodium alkylnaphthalenesulfonate and sodium dialkylsuccinatesulfonate.

[Wherein, R represents a linear or branched alkyl group having 8 to 10 carbon atoms, A represents an alkylene group having 2 to 4 carbon atoms, n represents an integer of 1 to 20; And q represent an integer in which p + q = 3 and p = 1 or 2, and M represents a hydrogen atom, an alkali metal atom, an ammonium group, or an organic ammonium group. When there are a plurality of R, A, and M, the types may be the same or different. ]
7. The water-floating pesticide preparation according to claim 6, wherein the water-soluble alkylene glycol is propylene glycol.
The water-floating pesticide formulation according to claim 6 or 7, having the following characteristics.
e) the ratio of major axis / minor axis of the bottom surface of the grains is 1.1 to 1.6;
f) 80% by weight or more in a particle size range of 2.80 mm to 1.70 mm, and g) 50 to 200 particles per gram.
(F) The water-susceptible pesticide formulation according to claim 8, wherein the particle size is 90% by weight or more in a range of 2.80 mm to 1.70 mm.
The water-floating pesticide preparation according to any one of claims 6 to 9, wherein the hollow body as the floating carrier is a shirasu balloon having an average particle diameter of 90 to 120 µm.
10. The composition according to claim 6, further comprising, as an anionic surfactant, at least one selected from the group consisting of an alkylnaphthalenesulfonic acid formaldehyde condensate Na, a naphthalenesulfonic acid formaldehyde condensate Na, and sodium ligninsulfonate. 4. The water-floating pesticide preparation according to any one of the above.
12. The water-floating pesticide formulation according to any one of claims 6 to 11, further comprising one or more selected from carboxymethylcellulose Na and polyvinyl alcohol as a binder.