KR20210040400A - Sleep floating pesticide formulation - Google Patents

Abstract

An object of the present invention is to provide a surface-floating pesticide formulation that exhibits good flotation and diffusivity in freshwater treatment under natural water conditions, and maintains its performance even after long-term storage, a) a pesticide active ingredient, b ) A floating carrier, c) at least one selected from alkyl naphthalene sulfonic acid Na and dialkyl succinate sulfonic acid Na, and d) the long/short diameter ratio of the bottom of the particle is 1.1 to 1.4, e) the particle size is 2.80 mm ~ It provides a surface-floating pesticide formulation characterized in that the number of particles per 1 g is 50 to 150, f) 80% by weight or more in the range of 1.70 mm.

Description

Sleep floating pesticide formulation

The present invention exhibits good flotation and diffusivity in treatment to a faucet, particularly in freshwater treatment under shallow water conditions, and also maintains its performance even after long-term storage, diffusivity. And it relates to a surface-floating pesticide formulation excellent in preservation.

As a formulation of a pesticide formulation for rice paddy, granules, powders, wettable powders, tablets, packs, flowables, water-soluble agents, liquids, emulsions, and the like are known. In recent years, as a viability of pesticide spraying, pesticide formulations (jumbo agents, flowable agents for spraying undiluted fresh water, etc.) have been developed and used that can be sprayed by simply putting them in the field without entering the water field. However, since such a pesticide preparation locally sprays the pesticide active ingredient in a high concentration state, it requires a long time until the pesticide active ingredient is uniformly diffused into the paddy field, and the local ubiquity of the pesticide active ingredient. The weakening of rice fields or lack of effect according to the problem is becoming a problem. As a means to solve these problems, after the pesticide preparation is added to the faucet under fresh water, it is required that the pesticide active ingredient is rapidly and uniformly dispersed.

In response to the above request, various methods have been proposed, and for example, the following patent documents can be cited.

International Publication No. 2016-129466 pamphlet (Patent Document 1) contains agrochemical active ingredient, a surfactant, a hollow body, and a solid carrier, and a particle size distribution having a particle diameter of 3 mm or more of 80% or more, and a property of floating on the water surface In addition, as a method for producing a granular pesticide composition characterized in that it disintegrates on the water surface within 30 minutes, comprising: (a) a part of a pesticide active ingredient, a part of a surfactant, a part of a hollow body, a part of a solid carrier, and water. Kneading the contained mixture; (b) granulating the kneaded product obtained in step (a) using an extrusion granulator; (c) drying the granulated product obtained in step (b) to obtain particles; (d) disintegrating the particles obtained in the step (c); (e) kneading a mixture containing the disintegrated product obtained in step (d) above, the balance of the agricultural chemical active ingredient, the balance of the surfactant, the balance of the hollow body, the balance of the solid carrier, and water; (f) discharging the kneaded product obtained in step (e) from a screen having a pore diameter of 3 mm or more using an extrusion granulator and assembling; A granular pesticide composition comprising: (g) drying the granulated product obtained in the above step (f) is proposed.

In the pamphlet of International Publication No. 2016-114200 (Patent Document 2), one or two or more active pesticides and poorly water-soluble polysaccharides, surfactants, hollow bodies, and solids that have water-retaining properties and suppress swelling in water. It is obtained by extruding a carrier and a water-containing mixture containing water, followed by drying to remove moisture, and having a particle size distribution of 80% or more with a particle diameter of 3 mm or more, and a property of floating on the water surface, and 30 In a water-floating large-sized granular pesticide composition containing a water-containing raw material, by a pesticide granular composition that disintegrates on the surface of the water within minutes and a method for producing the same, a surface-floating large-sized granular pesticide composition having good quality and a method for producing the same have been proposed.

In the pamphlet of International Publication No. 2015-159906 (Patent Document 3), a pesticide active ingredient, a floating carrier, and water within the range of 0.3 to 3% by mass, a particle size distribution of 80% or more with a particle diameter of 3 mm or more, and the property of floating on the water surface And water-floating large granular pesticide formulations that disintegrate from the surface within 30 minutes of input in water, and the total n kinds of raw materials, which are all of the active pesticide ingredients and auxiliary ingredients (excluding water) constituting the pesticide formulation, formula A water-floating large granular pesticide formulation having a value X defined by (1) in the range of 0.5 to 2 and a method for producing the same have been proposed.

In Japanese Patent Laid-Open No. 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 alkyl naphthalene sulfonate, ( d) A surface-floating pesticide formulation using a combination of isoparaffin with a distillation point of 277°C to 353°C and (e) a surface-floating hollow body has been proposed.

In Japanese Patent Laid-Open No. 2012-116787 (Patent Document 5), (a) a herbicidal active ingredient, (b) a specific polyoxyethylene alkyl ether represented by the general formula (1), and (c) a specific sodium alkyl naphthalene sulfonate. , (d) a water-floating herbicidal preparation using a combination of isoparaffin and (e) a water-floating hollow body having a distillation point of 277°C to 353°C has been proposed.

In the pamphlet of International Publication No. 2005-29956 (Patent Document 6), non-destructive pesticide granules, surfactants and floating properties that do not disintegrate in water within 30 minutes containing an acidic pesticide active ingredient, a cationic surfactant, and a basic substance. A uniformly diffusible granule containing a component and having a particle size distribution in which the mass ratio of particles with a particle diameter of 3 mm or more is 80% by mass or more and a property to float on the water surface immediately after dropping on the water surface, but disintegrate on the water surface within 30 minutes. Pesticide formulations have been proposed.

In Japanese Unexamined Patent Application Publication No. 2002-179507 (Patent Document 7), it contains a pesticide active ingredient, has a particle size distribution of 80% of those having a particle diameter of 3 mm or more, and has a property to float on the water surface, and collapses on the water surface within 30 minutes. A uniformly diffusible granular pesticide formulation and a uniformly diffusible granular pesticide formulation in which the preparation is sprayed and sprayed over an area of 5% to 50% of the total area of the receiving field at a distance of 1 m or more from the paddy field under fresh water have been proposed.

In Japanese Patent Laid-Open No. 2002-128605 (Patent Document 8), a pesticide formulation for sleep application characterized by using an agricultural chemical active ingredient, a floating hollow body, and a specific polyoxyalkylene alkyl ether phosphate or a salt thereof. Is proposed.

In Japanese Patent Application Laid-Open No. 2000-351701 (Patent Document 9), one or two or more types of sleep amplifying agents and pesticides consisting of C2 to C4 alkylene oxide adducts of C4 to C10 alkyl alcohols and derivatives thereof are effective. A surface-floating pesticide solid formulation containing an ingredient has been proposed.

In Japanese Patent Application Laid-Open No. 2001-114603 (Patent Document 10), inorganic salts, organic salts, organic acids, sugars having a particle diameter of 1/10 to 1/2 with respect to the short diameter of the agrochemical active ingredient and the agrochemical solid composition, Pesticide solid compositions comprising one or two or more water-soluble substances selected from urea have been proposed.

In Japanese Patent Application Laid-Open No. 2000-319103 (Patent Document 11), an agricultural chemical active ingredient, a surfactant, a solid carrier, a surface-floating agent, and water are contained, and the water content after molding is 100 weight of a surface-floating granular pesticide formulation. A surface-floating granular pesticide formulation, characterized in that it is 0.3 to 6 parts per part, and a manufacturing method thereof have been proposed.

In Japanese Patent Laid-Open No. 2000-319102 (Patent Document 12), a surface-floating granular pesticide containing an active ingredient, a surfactant, a solid carrier, and a sleep-floating agent as a component, is used as the disintegration time of the surface-floating granular pesticide. A water-dropping pesticide formulation comprising a water-soluble film bag having a dissolution time of 1/5 or less is proposed.

In Japanese Patent Application Laid-Open No. 2000-302602 (Patent Document 13), it contains an agricultural chemical active ingredient, a surfactant, a solid carrier, a surface flotation imparting agent, water, and other auxiliary agents as necessary, and (1) weight per one particle 0.03 g to 0.3 g, and the density of one particle is greater than or equal to 0.4 and less than 1.0 (2) The ratio of the short diameter to the long diameter of one particle is 1 to 3, the outer shape consisting of a curved surface (3) Particles floating on the water surface A surface-floating granular pesticide formulation characterized in that the time until disintegration and dispersing is within 30 minutes and a method for producing the same have been proposed.

In Japanese Unexamined Patent Application Publication No. Hei 11-310503 (Patent Document 14), a pesticide powder formulation or granule that has a property of floating and spreading on the water surface and does not contain a foaming agent is divided into a water-soluble film with a hole and solidified over time. A pesticide pack agent for feeding faucets has been proposed.

Any of the prior art has improved diffusivity, but this is diffusivity under conditions where the water depth (amount) is guaranteed. On the other hand, there are paddy fields that can only be maintained in shallow water (less than 3 cm) due to water leakage or natural supervision. In such conditions, the distance between the water surface and the soil is close, so if the buoyancy is small, the formulation is stranded or buried in the soil during spraying and settled in a large amount at the spraying point. There is a risk of causing it. In addition, the shallow water depth (淺水深) is the same word as a small amount, and in a formulation in which the active ingredient is diffused through the water surface or underwater, the range that can be diffused is limited compared to the normal water depth (about 5 cm). In such a pavement, more excellent floatability and diffusivity are required, and it is difficult to say that it is sufficient in the prior art. Moreover, regarding maintaining these properties even after long-term storage, there is no mention in the prior art, and a formulation excellent in all of the floatability, diffusivity and storage stability is required.

Patent Document 1: International Publication No. 2016/129466 pamphlet Patent Document 2: International Publication No. 2016/114200 pamphlet Patent Document 3: Pamphlet of International Publication No. 2015/159906 Patent Document 4: Japanese Patent Laid-Open No. 2012-116788 Patent Document 5: Japanese Patent Laid-Open No. 2012-116787 Patent Document 6: Pamphlet of International Publication No. 2005/29956 Patent Document 7: Japanese Patent Laid-Open No. 2002-179507 Patent Document 8: Japanese Patent Laid-Open No. 2002-128605 Patent Document 9: Japanese Patent Laid-Open No. 2000-351701 Patent Document 10: Japanese Patent Laid-Open No. 2001-114603 Patent Document 11: Japanese Patent Laid-Open No. 2000-319103 Patent Document 12: Japanese Patent Laid-Open No. 2000-319102 Patent Document 13: Japanese Patent Laid-Open No. 2000-302602 Patent Document 14: Patent Publication No. Hei 11-310503

In view of the conventional disadvantages as described above, the present invention is a surface-floating pesticide formulation having excellent diffusibility in freshwater treatment under shallow water conditions, and more specifically, a surface-floating pesticide formulation having excellent floatability of the pesticide formulation, and below the surface of the water when spraying. Provides a surface-floating pesticide formulation that does not sediment and spreads on the water surface, and exhibits excellent diffusion properties in water even after the formulation disintegrates in water over time, and maintains its performance even after long-term storage. It is aimed at.

The present inventors studied in-depth to solve the above problems. As a result, it consists of at least one selected from Na alkyl naphthalene sulfonic acid and Na dialkyl succinate sulfonic acid as agrochemical active ingredient, floating carrier, and anionic surfactant, and the long diameter/short diameter ratio of the bottom surface of the particles is 1.1 to 1.4 , It was found that the surface-floating pesticide formulation, characterized in that 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 of 50 to 150, achieves the purpose.

In addition, as agrochemical active ingredients, floating carriers, and anionic surfactants, those containing polyoxyalkylene alkyl ether phosphate salts together with water-soluble alkylene glycols such as propylene glycol, and additionally as anionic surfactants It was found that a water-floating pesticide formulation containing at least one selected from alkyl naphthalene sulfonic acid Na and dialkyl succinate sulfonic acid Na has excellent diffusivity. In addition, the long/short diameter ratio of the particle base of this formulation is 1.1 to 1.6, 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 1 g is 50 to 200. It has been found that the diffusivity is particularly good.

In addition, in the above water-floating pesticide formulation, the particle size is 90% by weight or more in the range of 2.80 mm to 1.70 mm, the floating carrier is a Shirasu balloon having an average particle diameter of 90 to 120 μm, additionally as an anionic surfactant In the case of containing alkylnaphthalene sulfonic acid formaldehyde condensate Na, naphthalene sulfonic acid formaldehyde condensate Na, and partially desulfonated lignin sulfonic acid Na (polyoxyalkylene alkyl ether phosphate ester salt and water-soluble alkylene glycol, lignin sulfonic acid Na ) Containing at least one selected from, and carboxymethylcellulose Na (polyoxyalkylene alkyl ether phosphate ester salt and water-soluble alkylene glycol, selected from carboxymethylcellulose Na and polyvinyl alcohol) as a binder. It has been found that it is more preferable to contain one or more), and thus the present invention has been completed.

That is, the present invention makes the following contents the gist.

[1] a) a pesticide active ingredient, b) a hollow body as a floating carrier, and c) a surface-floating pesticide containing at least one selected from alkyl naphthalene sulfonic acid Na and dialkyl succinate sulfonic acid Na as anionic surfactants A formulation, and a sleep-floating pesticide formulation having the following characteristics:

d) The long/short diameter ratio of the bottom of the particle is 1.1 to 1.4,

e) a particle size of at least 80% by weight in the range of 2.80 mm to 1.70 mm, and

f) The number of particles per 1 g is 50 to 150.

[2] e) The surface floating pesticide formulation according to [1], wherein the particle size is 90% by weight or more in the range of 2.80 mm to 1.70 mm.

[3] The sleep-floating pesticide formulation according to [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] In addition, as an anionic surfactant, it contains at least one selected from alkylnaphthalenesulfonic acid formaldehyde condensate Na, naphthalenesulfonic acid formaldehyde condensate Na, and partially desulfonated ligninsulfonic acid Na [ The sleep-floating pesticide formulation according to any one of 1] to [3].

[5] In addition, the water-floating agrochemical formulation according to any one of [1] to [4], which further contains carboxymethylcellulose Na as a binder.

[6] a) a pesticide active ingredient, b) a hollow body as a floating carrier, c) a polyoxyalkylene alkyl ether phosphate salt represented by the following general formula (I) and a water-soluble alkylene glycol, and d) anionic A surface-floating pesticide formulation comprising at least one selected from Na alkyl naphthalene sulfonic acid and Na dialkyl succinate sulfonic acid as a surfactant.

[Wherein, R represents a straight 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 p and q are p + q = 3 and p = 1 or 2 represents an integer, and M represents a hydrogen atom, an alkali metal atom, an ammonium group, or an organic ammonium group. On the other hand, when there are a plurality of R, A, and M, respectively, the types may be the same or different.]

[7] The water-soluble agrochemical formulation according to [6], wherein the water-soluble alkylene glycol is propylene glycol.

[8] The sleep-floating pesticide formulation according to [6] or [7] having the following characteristics:

e) The long/short diameter ratio of the bottom of the particle is 1.1 to 1.6,

f) a particle size of at least 80% by weight in the range of 2.80 mm to 1.70 mm, and

g) The number of particles per 1 g is 50 to 200.

[9] f) The surface floating pesticide formulation according to [8], wherein the particle size is 90% by weight or more in the range of 2.80 mm to 1.70 mm.

[10] The sleep-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] In addition, as anionic surfactants [6] to [6], characterized in that they contain at least one selected from Naphthalenesulfonic acid formaldehyde condensate Na, Naphthalenesulfonic acid formaldehyde condensate Na, and ligninsulfonic acid Na. The sleep-floating pesticide formulation according to any one of [10].

[12] In addition, the sleep-floating agrochemical formulation 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 flotation and diffusibility, even in freshwater sewage under shallow water conditions of less than 3 cm water depth, the formulation itself is excellent in surface movement and diffusion after disintegration of the formulation, and long-term storage It can maintain its performance afterwards. For this reason, a spraying machine such as a power spreader or a spraying tool such as a sprayer is not necessarily required at the time of spraying, and it is also possible to spray by hand. In addition, even if sprayed from one side of the ridge, it spreads, so the use environment is not limited. Moreover, since quality deterioration is suppressed even after long-term storage, it becomes possible to store and hold in advance. Accordingly, the sleep-floating pesticide formulation of the present invention is a viability formulation in which the physical, temporal, and economic burden of the spreader is reduced.

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

<A. About the composition ingredients>

As long as the pesticide active ingredient usable in the present invention is applicable to rice paddy, the following may be illustrated as such a pesticide active ingredient.

<< insecticidal active ingredient >>

For example, organic phosphorus-based (MEP, diazinone, etc.), carbamate-based (BPMC, carbosulfan, etc.), pyrethroid-based (cycloprothrin, etc.), neretoxin-based (thiocyclam, etc.) as an insecticidal active ingredient , Neonicotinoids (imidacloprid, thiamethoxam, clotianidine, dinotefuran, etc.), diamides (flubendiamide, chlorantraniliprole, cyantraniliprole, etc.), phenylpyra Sol-based (fipronil, etiprol, etc.), spinosine-based (spinosad, spinetoram, etc.) insecticides, insect growth control agents (tebufenozide, chromafenozide, methoxyfenozide, buprofezin, etc.) ), other synthetic pesticides (pimetrozine, triflumezopyrim, etc.), biological pesticides, and the like.

<< sterilization active ingredient >>

As bactericidal active ingredients, for example, inorganic copper, organic copper, inorganic sulfur, organic sulfur, organic phosphorus (IBP, etc.), melanin biosynthesis inhibitors (pyroquilon, tricyclazole, capropamide, di. Closimet, phenoxanil, etc.), benzoimidazole-based (benomyl, thiophanate methyl, dietophenecarb, etc.), amide-based (mepronil, flutolanil, furametpyr, fenflufen, fluxapyrok) THAAD, thifluzamide, thiadinil, isotianil, etc.), sterol biosynthesis inhibitors (pefurazoate, ifconazole, simeconazole, etc.), strobilurine (azoxystrobin, metominostrobin, orissa) Strobe), antibiotic fungicides (gasgamycin, validamycin, etc.), other synthetic fungicides, biological pesticides, and the like.

《Herbicidal active ingredient》

Examples of herbicidal active ingredients include phenoxy acid (MCPA thioethyl, MCPB ethyl, etc.), carbamate, acid amide (tenylchlor, butachlor, bromobutide, etc.), acetanilide, urea, Sulfonyl urea (bensulfuronmethyl, propysulfuron, etc.), benzofuranylalkyl sulfonic acid (benfursate, etc.), pyrimidyloxybenzoic acid (phenoxsulam, etc.), triazine (cymetrin, etc.), Diazine-based, diazole-based (pyrazolate, benzophenap, etc.), bipyridinium-based, dinitroaniline-based, aromatic carboxylic acid-based, imidazolinone-based, fatty acid-based, organic phosphorus-based, amino acid-based, tetrazolinone-based (pentrazamide Etc.), diphenyl ether-based (biphenox, etc.), oxazolidindione-based (pentoxazone, etc.), nitrile-based, phenylphthalimide-based, cineol-based, indandione-based, benzofuran-based, triazolopimididine-based, Oxazinone (oxazychromephone, etc.), allyltriazolinone, isourasol, pyrimidinylthiophthalide, triazolinone (iffencarbazone, etc.), triketone (tepuryltrione, mesotrione, etc.) On, benzobicyclone, etc.) inorganic herbicides, etc. are mentioned.

《Plant Growth Regulator》

Examples of the plant growth regulator include ethylene-based, auxin-based, cytokinin-based, gibberellin-based, and the like.

On the other hand, specific pesticide active ingredients contained in these are, for example, "Pesticide Handbook 2016 Edition" (published by the Japan Plant Prevention Association), "SHIBUYA INDEX 13th Edition" (Published by the Shibuya INDEX Research Society), and "The Pesticide Manual. Sixteenth Edition" (published by the British Crop Protection Council).

In addition, as the pesticide active ingredient used in the present invention, as long as it achieves the same object as the present invention and is applied as a sleep-floating pesticide formulation, a pesticide active ingredient other than the above known or later developed may also be applied.

The pesticide active ingredient may be used alone or in combination of two or more. In addition, the amount added is usually 0.01 to 60% by weight, preferably 0.05 to 50% by weight in the formulation.

《Floating carrier》

The floating carrier used in the present invention has a hollow body to generate buoyancy, so it can float on the water surface, and has a function of a disintegration aid because it creates a very small gap in the formulation, and has a function of a disintegration aid, in terms of floatability and disintegration. Contributes to diffusivity. Examples of the formulation include those having a hollow body such as a shirasu balloon, a fly ash balloon, a ceramic balloon, and a synthetic resin hollow body. In addition, since the hardness of the formulation tends to weaken when the average particle diameter of these components is excessively large, those having an average particle diameter of 200 μm or less are preferable.

In particular, considering the balance of floatability, disintegration, and formulation hardness, a Shirasu balloon having an average particle diameter of 90 to 120 μm is preferable.

The amount of the floating carrier usable in the present invention may be added as long as it is sufficient to make the formulation float on the water surface, and is usually 2.0 to 80% by weight, preferably 5.0 to 70% by weight. Moreover, you may use 1 type or 2 or more types among the above.

<< alkyl naphthalene sulfone Na and dialkyl succinate sulfonic acid Na >> (anionic surfactant)

Since the alkyl naphthalene sulfone Na and dialkyl succinate sulfonic acid Na used in the present invention are anionic surfactants with a good balance of wettability and dispersibility, by containing one or more of these anionic surfactants, it contributes to the disintegration and dispersibility of the formulation. And, this function maintains the above performance even after long-term storage. In addition, in terms of its wetting ability, a smaller amount of water in granulation is sufficient at the time of manufacture, and the effect of reducing the load at the time of granulation is also imparted.

The amount of alkylnaphthalene sulfone Na and dialkyl succinate sulfonic acid Na that can be used in the present invention is 0.5 to 30% by weight, preferably 1 to 20% by weight, in the formulation.

《Alkyl naphthalene sulfonic acid formaldehyde condensate Na, naphthalene sulfonic acid formaldehyde condensate Na, partially desulfonated lignin sulfonic acid Na, and lignin sulfonic acid Na” (additional anionic surfactant)

Diffusion and storage stability by additionally adding at least one selected from alkylnaphthalenesulfonic acid formaldehyde condensate Na, naphthalenesulfonic acid formaldehyde condensate Na, and partially desulfonated ligninsulfonic acid Na to the sleep-floating pesticide formulation of the present invention. Strengthen the function.

Any component or molecular weight is a polymer sulfonic acid-based surfactant having a molecular weight of about tens of thousands to tens of thousands, and dispersibility is enhanced by combination with Na alkyl naphthalene sulfonic acid and Na dialkyl succinate sulfonic acid, and the effect is maintained even after long-term storage.

On the other hand, in the case of containing a polyoxyalkylene alkyl ether phosphate salt and a water-soluble alkylene glycol described later, one selected from alkyl naphthalene sulfonic acid formaldehyde condensate Na, naphthalene sulfonic acid formaldehyde condensate Na, and lignin sulfonic acid Na By adding the above, diffusivity and storage stability functions are enhanced.

Alkyl naphthalene sulfonic acid formaldehyde condensate Na, naphthalene sulfonic acid formaldehyde condensate Na, partially desulfonated lignin sulfonic acid Na, and lignin sulfonic acid Na are added in the formulation in an amount of 0.5 to 30% by weight, preferably 1 to 20% by weight. %to be.

<< polyoxyalkylene alkyl ether phosphoric acid ester salt >> (anionic surfactant)

The following general formula (I) used in the present invention

[Wherein, R represents a straight 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 p and q are p + q = 3 and p = 1 or 2 represents an integer, and M represents a hydrogen atom, an alkali metal atom, an ammonium group, or an organic ammonium group. On the other hand, when there are a plurality of R, A, and M, respectively, the types may be the same or different.]

The polyoxyalkylene alkyl ether phosphoric acid ester salt represented by has excellent spreading power, wettability, dispersibility, and ability to gel upon contact with water. When the formulation comes into contact with water, the ingredient is gelled in a form in which the agrochemical active ingredient or a floating carrier is contained, so that it becomes possible to diffuse the agrochemical active ingredient further far in a state in which buoyancy is strengthened by the floating carrier. In addition, when the gel is dissolved in water, since the ingredient is present in a high concentration around the pesticide active ingredient, the ingredient is efficiently adsorbed to the pesticide active ingredient, and the pesticide active ingredient diffuses even further after the gel state is released. In addition, since the gelling ability does not deteriorate, the effect of imparting spreading power, dispersing power, and floating support to the formulation continues 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.

In order to exhibit the spreading power and gelling ability in the present invention, the alkylene group preferably contains an ethylene group having 2 carbon atoms. The alkylene group represented by A may be only an ethylene group having 2 carbon atoms, and may contain a propylene group having 3 carbon atoms or a butylene group having 4 carbon atoms together with an ethylene group having 2 carbon atoms, or both.

In the present invention, the alkyl group represented by R in the phosphate ester salt represented by the general formula (I) is a linear or branched structure having 8 to 10 carbon atoms in order to balance the solubility in water and spread power in water. It is necessary to be, and examples of the alkyl group include n-octyl group, n-decyl group, isodecyl group, and 2-ethylhexyl group.

In the present invention, the phosphate ester salt represented by the general formula (I) is not particularly limited as long as the cation (in the formula M) used as a pair of phosphate ions is not particularly limited as long as the function of the present invention is not lost, and the atom represented by M is hydrogen Alkali metal atoms, such as an atom, a lithium atom, a sodium atom, or a potassium atom, are mentioned, As a substituent, an organic ammonium group, such as an ammonium group, a methyl ammonium group, or a dimethyl ammonium group, is mentioned.

On the other hand, in the present formulation, since a heat drying step enters the manufacturing step, it is preferable that it is ^{K +} , Na ⁺ , or H ^{+ that is difficult to volatilize even in a heat drying step with a cation (M in the formula).}

In the present invention, in order to balance the solubility in water and spread power in water, the phosphate ester salt represented by the general formula (I) is 1 (monoester) or 2 (diester). Need to be. When the phosphoric acid ester salt is a monoester, p = 1, q = 2, and in this case, the alkyl groups represented by R may be the same or different, and in the case of a diester, p = 2, q = 1 , 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 in combination.

The addition amount of the polyoxyalkylene alkyl ether phosphate salt usable in the present invention is 1 to 40% by weight, preferably 3 to 25% by weight in the formulation, and there is no problem even if one type or two or more types are used in combination.

<< water-soluble alkylene glycol >>

The water-soluble alkylene glycol used in the present invention is essential in order to exhibit the function of the polyoxyalkylene alkyl ether phosphate salt. The characteristics of water-soluble alkylene glycol having both hydrophilicity and lipophilicity, when used in combination with polyoxyalkylene alkyl ether, adjusts the water dissolution time of the gel that occurs when it comes into contact with water. Accordingly, not only the spreading power and dispersing power of the polyoxyalkylene alkyl ether phosphate salt are exhibited to the maximum, but also the secondary effect of imparting a floating auxiliary effect to the formulation is obtained by the gel supporting the floating carrier.

The water-soluble alkylene glycol usable in the present invention may be miscible with water, and may include ethylene glycol, propylene glycol, butylene glycol, pentylene glycol, and hexylene glycol, and one or two or more of them. There is no problem even if you use them together.

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

《Binder》

As auxiliary binders, dextrin (roasted dextrin and enzyme-modified dextrin, etc.), acid-decomposed starch, oxidized starch, gelatinized starch, etherified starch (carboxymethyl starch, hydroxyalkyl starch, etc.), esterified starch (acetic acid starch and Starch phosphate, etc.), processed starch such as crosslinked starch and grafted starch, such as sodium alginate, gum arabic, gelatin, gum tragacanth, locust bean gum, and natural substances such as casein, such as sodium carboxymethylcellulose Salt, hydroxyethylcellulose, hydroxypropylcellulose, hydroxypropylmethylcellulose, methylcellulose, ethylcellulose, and cellulose derivatives such as acetylcellulose, and, for example, polyvinyl alcohol and polyvinylpyrrolidone. , It is not limited to these, and there is no problem even if 1 type or 2 or more types of these are used together.

In addition, carboxymethylcellulose Na is preferable from the viewpoint of disintegration and dispersibility.

On the other hand, in the case of containing a polyoxyalkylene alkyl ether phosphate salt and a water-soluble alkylene glycol, carboxymethylcellulose Na or polyvinyl alcohol is preferable from the viewpoint of disintegration and dispersibility.

The content of the binder usable in the present invention is preferably 0.1 to 10% by weight.

《Other supplements》

The sleep-floating pesticide formulation of the present invention may be added as an auxiliary agent in addition to the above-described components, and the following components may be added as long as the effect of the present invention is not lost.

Examples of the surfactant include nonionic surfactants, anionic surfactants other than the above, cationic surfactants, and amphoteric surfactants.

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

Examples of anionic surfactants other than the above include dodecylbenzenesulfonate, alkylsulfonate, lauryl sulfate, α-olefin sulfonate, polyoxyethylenealkylsulfosuccinate, polyoxyethylenealkylether sulfate, polyoxyethylenealkylaryl Ether sulfate, polyoxyethylene arylphenyl ether phosphate, polyoxyethylene styrylphenyl ether phosphate, and carboxylic acid (co)polymers such as acrylic acid and maleic acid, or sodium and potassium salts of copolymers of styrene sulfonic acid or vinyl group with these And the like.

On the other hand, the (co)polymerization of carboxylic acid such as acrylic acid and maleic acid, and sodium salt and potassium salt of a copolymer of styrene sulfonic acid or vinyl group with these, can be expected to contribute to the disintegration and dispersibility of the formulation.

Examples of cationic surfactants include alkyltrimethylammonium salts, alkyldimethylbenzylammonium salts, and alkylpyridinium salts.

Examples of amphoteric surfactants include dialkylaminoethylbetaine and alkyldimethylbenzylbetaine.

The surfactant that can be used in the present invention is not limited to these examples, and may be used alone or in combination of two or more. The content of the surfactant in the formulation is preferably 0.1 to 20% by weight.

Examples of the solid carrier usable in the present invention include those exemplified below.

For example, clay, quartz, calcite, meerschaum, dolomite, chalk, kaolin, pyrophyllite, sericite, haloysite, metahaloysite, wood-cut clay, wamok clay, pottery stone, ziklite, arofen, shirasu, Fired products of natural minerals such as mica, talc, pumice, sepiolite, bentonite, hectorite, zeolite, and diatomaceous earth, such as calcined clay, pearlite, vermiculite, atapul gas clay, and calcined diatomaceous earth, For example, inorganic salts such as magnesium carbonate, calcium carbonate, sodium carbonate, sodium hydrogen chloride, ammonium sulfate, sodium sulfate, magnesium sulfate, diammonium hydrogen phosphate, ammonium dihydrogen phosphate, and potassium chloride, such as glucose, fructose, sucrose, And saccharides such as lactose, such as starch, powdered cellulose, and polysaccharides such as dextrin, and organic substances such as urea, urea derivatives, benzoic acid, and salts of benzoic acid, and, for example, wood flour, corn spikelets, walnut husks , And plants such as tobacco stems, and white carbon.

The amount of the solid carrier usable in the present invention is 3 to 95% by weight, preferably 5 to 90% by weight, in the formulation.

Examples of antiseptic and antimicrobial agents include potassium sorbate, p-chloro-m-xylenol, butyl p-oxybenzoate, 1,2-benzoisothiazolin-3-one, 5-chloro-2-methyl-4-isothiazoline As a pH adjuster such as -3-one and 2-methyl-4-isothiazolin-3-one, as a pH adjusting agent, hydrochloric acid, sulfuric acid, citric acid, phosphoric acid, and magnesium carbonate, etc., and as a stabilizer for agrochemical active ingredient, an antioxidant , An ultraviolet ray inhibitor, and an agent for preventing crystal precipitation, etc. may be added, but the present invention is not limited to the auxiliary agent exemplified.

The added amount of these auxiliary agents usable in the present invention is 0.01 to 15% by weight, preferably 0.1 to 10% by weight in the formulation.

<B. About the properties of the formulation>

In the water-floating agrochemical formulation of the present invention, in order to exhibit good flotation and diffusivity, as well as excellent preservation effects, not only the formulation components, but also the ``long diameter/short diameter ratio of the bottom of the particles'', which will be described below, Physical properties of pesticide formulations such as "particle size" and "the number of particles per 1 g" are required.

《Long diameter/short diameter ratio of particle base》

In the water-floating pesticide formulation of the present invention, the bottom surface of the particles refers to the surface originating from the screen hole at the time of assembly, and the long diameter and short diameter at the bottom surface are drawn by a straight line (diameter) passing through the center of the bottom surface. The maximum diameter at the time is set as the long diameter, and the minimum diameter is set as the short diameter.

Therefore, the long/short diameter ratio of the bottom of the particles is cut with a cutter so that the bottom of the formulation becomes a cross section, and then the maximum diameter (long diameter) and the minimum diameter (short diameter) of the cross section are measured with a microscope, and the short diameter It refers to a value obtained by calculating the ratio of the long diameter to the average value of 10 particles of the formulation.

In the water-floating pesticide formulation of the present invention, adjusting the long-diameter/short-diameter ratio at the bottom of the particles contributes to the floatability, diffusivity, and storage stability (reach distance to the formulation after long-term storage, diffusion distance) of the formulation. . In order to impart the effect of improving floatability and diffusivity, it is essential to adjust the long diameter/short diameter ratio in the range of 1.1 to 1.4. The long-diameter/short-diameter ratio is a parameter expressing the shape of the formulation, and 1.0 (minimum value) means that the shape of the bottom surface is round, and as the value increases, the particles become closer to the flat shape. When the long-diameter/short-diameter ratio is 1.0, the movement of the agent on the water surface is slow, resulting in a decrease in diffusibility, and when it exceeds 1.4, the movement on the water surface is accelerated, but rapidly disintegrating and dispersing, and as a result, the diffusion distance of the active ingredient is shortened.

On the other hand, in the case of containing polyoxyalkylene alkyl ether phosphate and propylene glycol, the disintegration time of the formulation in water increases due to the gel generated when contacted with water, so the upper limit of the long/short diameter ratio is 1.6 Until it becomes possible. In addition, when the long-diameter/short-diameter ratio is 1.1 or more with respect to the formulation reach and diffusion distance after long-term storage, deterioration of quality after long-term storage is suppressed. These factors are, as the long/short diameter ratio increases, the area of the agent in contact with the water surface increases, which makes it more susceptible to the buoyancy of water, or the disintegration and dispersion of the water surface due to the rapid release of the surfactant from the water surface. It is estimated that this is because the efficiency of is improved.

As a method of adjusting the long/short diameter ratio, in the extrusion granulation process, the extrusion hole diameter at the time of granulation is adjusted, and then, in the sizing process, the particles such as a drum type sizing machine or a marmarizer are rotated. A method of rotating the granulated product before drying, controlling centrifugal force, and controlling the long-diameter/short-diameter ratio can be mentioned using a machine to be dried.

On the other hand, the granulated product before drying is soft because the binder contains moisture and is swollen, and if the granulation diameter (extrusion pore diameter) is large, its own weight is also affected. For this reason, when a rotational motion is applied, a centrifugal force and a self-weight act, and the cross section of the granulated product is flattened (generates of a long diameter and a short diameter).

《Particle size》

In the sleep-floating pesticide formulation of the present invention, the particle size is the formula below based on the weight of the formulation remaining on the sieve size 1.70 mm when 100 g of the formulation is sieved with a test sieve having a size of 2.80 mm and 1.70 mm. It is calculated from 1).

In the water-floating pesticide formulation of the present invention, adjusting the particle size contributes to the floatability and diffusivity of the formulation. From the viewpoint of balance of floatability and diffusivity, 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 terms of particle size, those smaller than the above particle size range tend to sink as the buoyancy decreases because there are fewer floating carriers, and those with larger particle sizes increase the weight per particle, resulting in slow motion on the water surface, and diffusibility. It gets worse.

As a method of adjusting the particle size, a method of adjusting the extrusion pore size at the time of granulation in the extrusion granulation step, then appropriately adjusting the length of the particles of the granulated product before drying in the sizing step, and controlling the particle size may be mentioned. The sizing group used for adjusting the particle size is not particularly limited, but a rotary sizing device such as a drum sizing device or a marmarizer, or a disintegrating sizing device such as a pin mill, oscillator, randel mill, or nebulizer can be used. From the viewpoint of economical efficiency and viability at the time of manufacture, a rotary sizing machine such as a drum sizing machine capable of simultaneously adjusting the long/short diameter ratio of the bottom of the particles is preferable.

<< number of particles per 1 g >>

In the water-floating pesticide formulation of the present invention, the number of particles per 1 g is measured by measuring the number of particles of 5.0 g of the weighed formulation with a particle number meter, and the measured value is expressed as a fifth value (the decimal point or less is rounded up). .

In the water-floating pesticide formulation of the present invention, adjusting the number of particles per 1 g contributes to the floatability and diffusivity of the formulation. In terms of balance of floatation and diffusivity, it is essential that the number of particles per gram is 50 to 150. For the same reason as the above-described particle size, those with more than 150 particles per gram tend to sink as the particles are smaller and less buoyant, and those with less than 50 increase the weight per particle, resulting in slow motion on the water surface. And diffusivity worsens.

On the other hand, in the case of containing polyoxyalkylene alkyl ether phosphate and propylene glycol, the upper limit of the number of particles per 1 g can be up to 200 because even particles with small buoyancy are diffused farther due to enhanced diffusivity. .

As a method of adjusting the number of particles per 1 g, a method of controlling the number of particles per 1 g is exemplified by disintegrating the granulated product before drying in the sizing step. The sizing group used for adjusting the number of particles is not particularly limited, but a rotary sizing device such as a drum sizing device or a marmarizer, or a disintegrating sizing device such as a pin mill, oscillator, randel mill, or nebulizer can be used. From the viewpoint of economical efficiency and viability at the time of manufacture, a rotary sizing machine such as a drum-type sizing machine capable of simultaneously adjusting the long/short diameter ratio of the bottom surface of the particles and the particle size is preferable.

<Method of manufacturing a water-floating pesticide formulation>

The water-floating pesticide formulation of the present invention is manufactured by extrusion granulation, and is advantageous in terms of economy and manufacturing efficiency.

In the manufacturing process, at least one selected from agrochemical active ingredients, floating carriers, alkyl naphthalene sulfonic acid Na and dialkyl succinate sulfonic acid Na, polyoxyalkylene alkyl ether phosphate ester salt, if necessary, alkyl naphthalene sulfonic acid Formaldehyde condensate Na, naphthalene sulfonic acid formaldehyde condensate Na, and at least one selected from partially desulfonated lignin sulfonic acid Na, and lignin sulfonic acid Na, and various auxiliary agents are added to the juice mixer, hammer mill, Lodige mixer, or Mix uniformly using a ribbon mixer or the like. Water is added to the mixture and kneaded using a double arm kneader or ribbon mixer. On the other hand, when adding a slurry by wet pulverizing the agricultural chemical active ingredient for reasons such as mixing precision, it is added together with water during kneading.

In the granulation step and the sizing step after the kneading step, the physical properties of the water-floating pesticide formulation of the present invention are adjusted. In the sizing process, the long/short diameter ratio, particle size, and number of particles of the bottom surface of the particles may be adjusted at once, or the long/short diameter ratio of the bottom surface of the particles may be adjusted, and then the particle size and the number of particles may be adjusted. It is desirable to omit the number of steps and to adjust at once from the viewpoint of improving economic efficiency in manufacturing.

In the granulation and sizing process, first, the mixture is granulated using an extrusion granulator such as a basket-type granulator or a screw-type granulator. The extrusion pore diameter at the time of 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. Given the extrusion pore size, the water-floating pesticide formulation of the present invention establishes the obtained granulated product with a machine in which a centrifugal force acts on particles such as a drum-type sizing machine and a marmarizer, so that the long/short diameter ratio at the bottom is 1.1 to In addition to 1.4, the particle size may be set to be 80% by weight or more in the range of 2.80 mm to 1.70 mm and the number of particles per 1 g of 50 to 150. After sizing, it is dried using a fluid bed dryer or a bed dryer, and then sieved to obtain a surface-floating pesticide formulation used in the present invention.

On the other hand, in the case of using a pesticide active ingredient intended to promote dissolution in combination, it is also possible to add a coating step within a range that does not lose the effect of the present invention.

<Forms of use of sleep-floating pesticide formulations>

The water-floating pesticide formulation of the present invention is sprayed directly without entering the faucet. Spraying methods include hand spraying, spraying in a container such as a cup, mechanical spraying by a powered sprayer, aerial spraying using radio-controlled helicopters, drones, etc., and water polo spray spraying on water flowing into a faucet . Considering the aspect of avoiding the exposure of the sprayer, a spraying method that does not come into direct contact with the formulation is preferable. In addition, the application amount is usually 50 to 500 g, preferably 75 to 300 g per 10 a.

[Example]

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

On the other hand, in the following Examples and Comparative Examples, "parts" means "parts by weight" and "%" means "% by weight".

In addition, in the following Examples and Comparative Examples, the devices (microscope, sieve shaker, particle number meter) used to measure the long/short diameter ratio, particle size, and number of particles of the surface-suspending pesticide formulation were VHX- 5000 (Keyence Co., Ltd.), low tap sieve shaker (Iida Seisakusho Co., Ltd.), multi auto counter KC-1M5 type (Fujiwara Seisakusho Co., Ltd.).

[Example 1]

Kasugamycin 24.0 parts (sterilizing active ingredient), Shirasu balloon (average particle diameter 70 to 90 μm) (floating carrier) 25.0 parts, alkylnaphthalenesulfonic acid Na 3.0 parts, dextrin 5.0 parts, bentonite 10.0 parts, pearlite 30.0 parts, clay 3.0 parts were pulverized and mixed with a hammer mill (sample mill KIIW-1, Dalton Corporation), and a powder mixture was obtained. The obtained powder mixture was put into a double arm kneader (KDHJ, Dalton Corporation), and kneaded for 15 minutes after adding water. Next, the kneaded water was assembled with an extrusion granulator equipped with a basket-type screen having a pore diameter of 3.0 mm. After pre-drying the obtained granulated product, it was sized with a drum-type sizer, and dried with a fluidized bed dryer. This was sieved to a size of 3.35 mm to 2.00 mm to obtain a surface-floating pesticide formulation. The particle size of the obtained formulation was 85% in the range of 2.80 to 1.70 mm, the long diameter/short diameter ratio at the bottom was 1.2, and the number of particles per 1 g was 98.

[Example 2]

Formulation composition of gasgamycin 24.0 parts (sterilizing active ingredient), fly ash balloon (average particle diameter 80 to 120 μm) (floating carrier) 30.0 parts, dialkyl succinate sulfonic acid Na 1.5 parts, carboxymethylcellulose Na 2.0 parts, pearlite With 35.0 parts, clay 7.5 parts, and a granulation diameter of 2.8 mm, in accordance with Example 1, a water-floating pesticide formulation was prepared. The particle size of the obtained formulation was 83% in the range of 2.80 to 1.70 mm, the long diameter/short diameter ratio at the bottom was 1.2, and the number of particles per 1 g was 105.

[Example 3]

Formulation composition is gasgamycin 24.0 parts (sterilizing active ingredient), acrylonitrile resin balloon (average particle diameter 20 to 40 μm) (floating carrier) 2.0 parts, alkylnaphthalenesulfonic acid Na 3.0 parts, polyacrylate Na 2.0 parts, carboxymethyl With 2.0 parts of cellulose Na, 57.0 parts of pearlite, 10.0 parts of clay, and 3.0 mm of granulated diameter, a water-floating pesticide formulation was prepared in accordance with Example 1. The particle size of the obtained formulation was 86% in the range of 2.80 to 1.70 mm, the long/short diameter ratio at the bottom was 1.3, and the number of particles per 1 g was 113.

[Example 4]

The formulation composition was gasgamycin 24.0 parts (sterilizing active ingredient), ceramic balloon (average particle diameter 20 to 150 μm) (floating carrier) 25.0 parts, alkylnaphthalenesulfonic acid Na 3.0 parts, carboxymethylcellulose Na 2.0 parts, diatomaceous earth 36.0 parts, The clay was 10.0 parts and the granulation diameter was 3.0 mm, and a surface-floating pesticide formulation was prepared in accordance with Example 1. The particle size of the obtained formulation was 93% in the range of 2.80 to 1.70 mm, the long/short diameter ratio at the bottom was 1.1, and the number of particles per 1 g was 83.

[Example 5]

The formulation composition was gasgamycin 24.0 parts (sterilizing active ingredient), Shirasu balloon (average particle diameter 70 to 90 μm) (floating carrier) 30.0 parts, dialkyl succinate sulfonic acid Na 1.5 parts, acrylic acid-maleic acid copolymer Na 2.0 parts, Carboxymethylcellulose Na 3.0 parts, bentonite 10.0 parts, pearlite 20.0 parts, white carbon 4.5 parts, clay 5.0 parts, granulation diameter 2.8 mm, according to Example 1, a water-floating pesticide formulation was prepared. The particle size of the obtained formulation was 95% in the range of 2.80 to 1.70 mm, the long/short diameter ratio at the bottom was 1.3, and the number of particles per 1 g was 88.

[Example 6]

The formulation composition was gasgamycin 24.0 parts (sterilizing active ingredient), Shirasu balloon (average particle diameter 90 to 120 μm) (floating carrier) 30.0 parts, alkyl naphthalene sulfonic acid Na 3.0 parts, acrylic-methacrylic acid copolymer Na 2.0 parts, Carboxymethylcellulose Na 3.0 parts, diatomaceous earth 33.0 parts, clay 5.0 parts, granulation diameter 2.8 mm, according to Example 1, a water-floating pesticide formulation was prepared. The particle size of the obtained formulation was 88% in the range of 2.80 to 1.70 mm, the long/short diameter ratio at the bottom was 1.2, and the number of particles per 1 g was 96.

[Example 7]

Formulation composition is gasgamycin 24.0 parts (sterilizing active ingredient), Shirasu balloon (average particle diameter 90 to 120 μm) (floating carrier) 25.0 parts, dialkyl succinate sulfonic acid Na 1.5 parts, polyacrylic acid Na 3.0 parts, carboxymethylcellulose With 3.0 parts of Na, 37.0 parts of diatomaceous earth, 6.5 parts of clay, and 3.0 mm of granulated diameter, a water-floating pesticide formulation was prepared in accordance with Example 1. The particle size of the obtained formulation was 87% in the range of 2.80 to 1.70 mm, the long diameter/short diameter ratio at the bottom was 1.4, and the number of particles per 1 g was 110.

[Example 8]

Formulation composition is gasgamycin 24.0 parts (sterilizing active ingredient), Shirasu balloon (average particle diameter 90 to 120 μm) (floating carrier) 30.0 parts, alkylnaphthalenesulfonic acid Na 3.0 parts, acrylic-maleic acid copolymer Na 3.0 parts, carboxymethyl With 3.0 parts of cellulose Na, 32.0 parts of pearlite, 5.0 parts of clay, and 3.0 mm of granulated diameter, a water-floating pesticide formulation was prepared in accordance with Example 1. The particle size of the obtained formulation was 96% in the range of 2.80 to 1.70 mm, the long/short diameter ratio at the bottom was 1.2, and the number of particles per 1 g was 98.

[Example 9]

Formulation composition is gasgamycin 24.0 parts (sterilizing active ingredient), Shirasu balloon (average particle diameter 90 to 120 μm) (floating carrier) 30.0 parts, dialkyl succinate sulfonic acid Na 1.5 parts, acrylic acid-vinyl sulfonic acid copolymer Na 2.0 parts , Carboxymethylcellulose Na 2.0 parts, pearlite 34.5 parts, clay 6.0 parts, granulation diameter 2.8 mm, according to Example 1, a water-floating pesticide formulation was prepared. The particle size of the obtained formulation was 97% in the range of 2.80 to 1.70 mm, the long/short diameter ratio at the bottom was 1.3, and the number of particles per 1 g was 87.

[Example 10]

The formulation composition was gasgamycin 24.0 parts (sterilizing active ingredient), Shirasu balloon (average particle diameter 70 to 90 μm) (floating carrier) 30.0 parts, alkylnaphthalenesulfonic acid Na 3.0 parts, alkylnaphthalenesulfonic acid formaldehyde condensate Na 3.0 parts, Acrylic-methacrylic acid copolymer Na 2.0 parts, carboxymethylcellulose Na 2.0 parts, pearlite 28.5 parts, clay 7.5 parts, granulation diameter 2.8 mm, according to Example 1, a water-floating pesticide formulation was prepared. The particle size of the obtained formulation was 85% in the range of 2.80 to 1.70 mm, the long/short diameter ratio at the bottom was 1.2, and the number of particles per 1 g was 76.

[Example 11]

Formulation composition is gasgamycin 24.0 parts (sterilizing active ingredient), fly ash balloon (average particle diameter 80 to 120 μm) (floating carrier) 30.0 parts, dialkyl succinate sulfonic acid Na 1.5 parts, partially desulfonated lignin sulfonic acid Na 3.0 parts , Polyacrylic acid Na 2.0 parts, carboxymethylcellulose Na 2.0 parts, bentonite 10.0 parts, pearlite 18.5 parts, white carbon 5.0 parts, clay 4.0 parts, granulation diameter 3.0 mm, according to Example 1, a water-floating pesticide formulation Prepared. The particle size of the obtained formulation was 87% in the range of 2.80 to 1.70 mm, the long diameter/short diameter ratio at the bottom was 1.3, and the number of particles per 1 g was 93.

[Example 12]

The formulation composition is gasgamycin 24.0 parts (sterilizing active ingredient), ceramic balloon (average particle diameter 20 to 150 μm) (floating carrier) 30.0 parts, alkyl naphthalene sulfonic acid Na 3.0 parts, naphthalene sulfonic acid formaldehyde condensate Na 3.0 parts, acrylic -Vinyl sulfonic acid copolymer Na 2.0 parts, carboxymethylcellulose Na 2.0 parts, bentonite 10.0 parts, diatomaceous earth 21.0 parts, clay 5.0 parts, granulation diameter 2.8 mm, according to Example 1, a surface-floating pesticide formulation was prepared. The particle size of the obtained formulation was 95% in the range of 2.80 to 1.70 mm, the long/short diameter ratio at the bottom was 1.1, and the number of particles per 1 g was 85.

[Example 13]

Formulation composition is gasgamycin 24.0 parts (sterilizing active ingredient), acrylonitrile resin balloon (average particle diameter 20 to 40 μm) (floating carrier) 2.0 parts, dialkyl succinate sulfonic acid Na 1.5 parts, partially desulfonated lignin sulfonic acid Na 3.0 parts, acrylic acid-maleic acid copolymer Na 2.0 parts, carboxymethylcellulose Na 2.0 parts, diatomaceous earth 55.5 parts, clay 10.0 parts, granulation diameter 3.0 mm, according to Example 1, a surface-floating pesticide formulation was prepared. The particle size of the obtained formulation was 95% in the range of 2.80 to 1.70 mm, the long diameter/short diameter ratio at the bottom was 1.3, and the number of particles per 1 g was 68.

[Example 14]

The formulation composition was gasgamycin 24.0 parts (sterilizing active ingredient), Shirasu balloon (average particle diameter 90 to 120 μm) (floating carrier) 30.0 parts, alkylnaphthalenesulfonic acid Na 3.0 parts, alkylnaphthalenesulfonic acid formaldehyde condensate Na 3.0 parts, Acrylic-vinyl sulfonic acid copolymer Na 3.0 parts, carboxymethylcellulose Na 2.0 parts, bentonite 10.0 parts, pearlite 22.0 parts, clay 3.0 parts, granulation diameter 2.8 mm, according to Example 1, a water surface floating pesticide formulation was prepared. . The particle size of the obtained formulation was 88% in the range of 2.80 to 1.70 mm, the long/short diameter ratio at the bottom was 1.3, and the number of particles per 1 g was 111.

[Example 15]

Formulation composition is gasgamycin 24.0 parts (sterilizing 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, carboxymethylcellulose Na 3.0 parts, bentonite 10.0 parts, pearlite 10.0 parts, white carbon 7.5 parts, clay 8.0 parts, granulation diameter 3.0 mm, according to Example 1 A floating pesticide formulation was prepared. The particle size of the obtained formulation was 86% in the range of 2.80 to 1.70 mm, the long/short diameter ratio at the bottom was 1.4, and the number of particles per 1 g was 105.

[Example 16]

Formulation composition is gasgamycin 24.0 parts (sterilizing active ingredient), Shirasu balloon (average particle diameter 90 to 120 μm) (floating carrier) 30.0 parts, alkyl naphthalene sulfonic acid Na 3.0 parts, partially desulfonated lignin sulfonic acid Na 3.0 parts, acrylic- Maleic acid copolymer Na 3.0 parts, carboxymethylcellulose Na 3.0 parts, pearlite 29.0 parts, clay 5.0 parts, granulation diameter was made into 3.0 mm, and the water-floating pesticide formulation was prepared according to Example 1. The particle size of the obtained formulation was 94% in the range of 2.80 to 1.70 mm, the long/short diameter ratio at the bottom was 1.3, and the number of particles per 1 g was 121.

[Example 17]

Formulation composition is gasgamycin 24.0 parts (sterilizing active ingredient), Shirasu balloon (average particle diameter 90 to 120 μm) (floating carrier) 30.0 parts, dialkyl succinate sulfonic acid Na 1.5 parts, alkylnaphthalene sulfonic acid formaldehyde condensate Na 3.0 Part, 3.0 parts of polyacrylate Na, 3.0 parts of carboxymethylcellulose Na, 30.5 parts of diatomaceous earth, 5.0 parts of clay, and a granulation diameter of 2.8 mm were used to prepare a water-floating pesticide formulation in accordance with Example 1. The particle size of the obtained formulation was 93% in the range of 2.80 to 1.70 mm, the long/short diameter ratio at the bottom was 1.4, and the number of particles per 1 g was 83.

[Example 18]

Pymetrozine 12.0 parts (insecticide active ingredient), Shirasu balloon (average particle diameter 70 to 90 μm) (floating carrier) 25.0 parts, alkyl naphthalene sulfonic acid Na 3.0 parts, polyvinyl alcohol 3.0 parts, pearlite 47.0 parts, clay 10.0 parts It pulverized and mixed with a hammer mill (sample mill KIIW-1, Dalton company), and obtained the powder mixture. The obtained powder mixture was put into a double arm kneader (KDHJ, Dalton Corporation), and kneaded for 15 minutes after adding water. Next, the kneaded water was assembled with an extrusion granulator equipped with a basket-type screen having a pore diameter of 3.0 mm. After pre-drying the obtained granulated product, it was sized with a drum-type sizer, and dried with a fluidized bed dryer. This was sieved to a size of 3.35 mm to 2.00 mm to obtain a surface-floating pesticide formulation. The particle size of the obtained formulation was 83% in the range of 2.80 to 1.70 mm, the long/short diameter ratio at the bottom was 1.3, and the number of particles per 1 g was 89.

[Example 19]

Formulation composition of pimetrozine 12.0 parts (insecticide active ingredient), fly ash balloon (average particle diameter 80 to 120 μm) (floating carrier) 25.0 parts, dialkyl succinate sulfonic acid Na 1.5 parts, carboxymethylcellulose Na 3.0 parts, pearlite With 48.5 parts, clay 10.0 parts, and a granulation diameter of 2.8 mm, in accordance with Example 16, a water-floating pesticide formulation was prepared. The particle size of the obtained formulation was 86% in the range of 2.80 to 1.70 mm, the long/short diameter ratio at the bottom was 1.4, and the number of particles per 1 g was 97.

[Example 20]

Formulation composition of pimetrozine 12.0 parts (insecticide active ingredient), acrylonitrile resin balloon (average particle diameter 20 to 40 μm) (floating carrier) 2.0 parts, alkyl naphthalene sulfonic acid Na 3.0 parts, polyacrylic acid Na 3.0 parts, carboxymethyl With 2.0 parts of cellulose Na, 60.0 parts of pearlite, 18.0 parts of clay, and 3.0 mm of granulated diameter, a water-floating pesticide formulation was prepared in accordance with Example 18. The particle size of the obtained formulation was 88% in the range of 2.80 to 1.70 mm, the long/short diameter ratio at the bottom was 1.3, and the number of particles per 1 g was 106.

[Example 21]

Formulation composition of pimetrozine 12.0 parts (insecticide active ingredient), ceramic balloon (average particle diameter 20 to 150 μm) (floating carrier) 30.0 parts, alkylnaphthalenesulfonic acid Na 3.0 parts, carboxymethylcellulose Na 2.0 parts, diatomaceous earth 43.0 parts, The clay was 10.0 parts and the granulation diameter was 3.0 mm, and a water-floating pesticide formulation was prepared in accordance with Example 18. The particle size of the obtained formulation was 93% in the range of 2.80 to 1.70 mm, the long/short diameter ratio at the bottom was 1.4, and the number of particles per 1 g was 82.

[Example 22]

Formulation composition of pimetrozine 12.0 parts (insecticide active ingredient), Shirasu balloon (average particle diameter 70 to 90 μm) (floating carrier) 30.0 parts, dialkyl succinate sulfonic acid Na 1.5 parts, acrylic acid-maleic acid copolymer Na 2.0 parts, Carboxymethylcellulose Na 2.0 parts, bentonite 10.0 parts, pearlite 30.0 parts, white carbon 5.0 parts, clay 7.5 parts, granulation diameter 2.8 mm, according to Example 18, a water-floating pesticide formulation was prepared. The particle size of the obtained formulation was 96% in the range of 2.80 to 1.70 mm, the long/short diameter ratio at the bottom was 1.3, and the number of particles per 1 g was 88.

[Example 23]

Formulation composition of pimetrozine 12.0 parts (insecticide active ingredient), Shirasu balloon (average particle diameter 90 to 120 μm) (floating carrier) 30.0 parts, alkyl naphthalene sulfonic acid Na 3.0 parts, acrylic-methacrylic acid copolymer Na 2.0 parts, Carboxymethylcellulose Na 3.0 parts, diatomaceous earth 40.0 parts, clay 10.0 parts, granulation diameter 2.8 mm, according to Example 18, to prepare a water-floating pesticide formulation. The particle size of the obtained formulation was 84% in the range of 2.80 to 1.70 mm, the long/short diameter ratio at the bottom was 1.4, and the number of particles per 1 g was 93.

[Example 24]

Formulation composition of pimetrozine 12.0 parts (insecticide active ingredient), Shirasu balloon (average particle diameter 90 to 120 μm) (floating carrier) 30.0 parts, dialkyl succinate sulfonic acid Na 1.5 parts, polyacrylic acid Na 2.0 parts, carboxymethylcellulose With 3.0 parts of Na, 45.0 parts of diatomaceous earth, 6.5 parts of clay, and 3.0 mm of granulated diameter, a water-floating pesticide formulation was prepared in accordance with Example 18. The particle size of the obtained formulation was 83% in the range of 2.80 to 1.70 mm, the long/short diameter ratio at the bottom was 1.3, and the number of particles per 1 g was 97.

[Example 25]

Formulation composition of pimetrozine 12.0 parts (insecticide active ingredient), Shirasu balloon (average particle diameter 90 to 120 μm) (floating carrier) 25.0 parts, alkyl naphthalene sulfonic acid Na 3.0 parts, acrylic-maleic acid copolymer Na 3.0 parts, carboxymethyl With 2.0 parts of cellulose Na, 45.0 parts of pearlite, 10.0 parts of clay, and 3.0 mm of granulated diameter, a water-floating pesticide formulation was prepared in accordance with Example 18. The particle size of the obtained formulation was 94% in the range of 2.80 to 1.70 mm, the long diameter/short diameter ratio at the bottom was 1.4, and the number of particles per 1 g was 95.

[Example 26]

Formulation composition of pimetrozine 12.0 parts (insecticide 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 copolymer Na 3.0 parts , Carboxymethylcellulose Na 3.0 parts, pearlite 48.5 parts, clay 7.0 parts, granulation diameter 2.8 mm, according to Example 18, to prepare a water-floating pesticide formulation. The particle size of the obtained formulation was 97% in the range of 2.80 to 1.70 mm, the long/short diameter ratio at the bottom was 1.4, and the number of particles per 1 g was 107.

[Example 27]

Formulation composition of pimetrozine 12.0 parts (insecticide 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 Na 3.0 parts, Acrylic-methacrylic acid copolymer Na 3.0 parts, carboxymethylcellulose Na 3.0 parts, pearlite 38.0 parts, clay 10.0 parts, granulation diameter 2.8 mm, according to Example 18 to prepare a water-floating pesticide formulation. The particle size of the obtained formulation was 83% in the range of 2.80 to 1.70 mm, the long/short diameter ratio at the bottom was 1.4, and the number of particles per 1 g was 91.

[Example 28]

Formulation composition of pimetrozine 12.0 parts (insecticide active ingredient), fly ash balloon (average particle diameter 80 to 120 μm) (floating carrier) 28.0 parts, dialkyl succinate sulfonic acid Na 1.5 parts, partially desulfonated lignin sulfonic acid Na 3.0 parts , Polyacrylic acid Na 3.0 parts, carboxymethylcellulose Na 2.0 parts, bentonite 10.0 parts, pearlite 30.0 parts, white carbon 5.0 parts, clay 5.5 parts, granulation diameter 3.0 mm, according to Example 18, a water-floating pesticide formulation Prepared. The particle size of the obtained formulation was 87% in the range of 2.80 to 1.70 mm, the long/short diameter ratio at the bottom was 1.3, and the number of particles per 1 g was 83.

[Example 29]

Formulation composition of pimetrozine 12.0 parts (insecticide active ingredient), ceramic balloon (average particle diameter 20 to 150 μm) (floating carrier) 25.0 parts, alkyl naphthalene sulfonic acid Na 3.0 parts, naphthalene sulfonic acid formaldehyde condensate Na 3.0 parts, acrylic -Vinyl sulfonic acid copolymer Na 3.0 parts, carboxymethylcellulose Na 3.0 parts, bentonite 10.0 parts, diatomaceous earth 36.0 parts, clay 5.0 parts, granulation diameter 2.8 mm, according to Example 18, a water surface floating pesticide formulation was prepared. The particle size of the obtained formulation was 98% in the range of 2.80 to 1.70 mm, the long/short diameter ratio at the bottom was 1.4, and the number of particles per 1 g was 86.

[Example 30]

The formulation composition was 12.0 parts of pymetrozine (an insecticidal active ingredient), an acrylonitrile resin balloon (average particle diameter of 20 to 40 μm) (a floating carrier) 2.0 parts, a dialkyl succinate sulfonic acid Na 1.5 parts, and a partially desulfonated lignin sulfonic acid Na 3.0 parts, acrylic acid-maleic acid copolymer Na 2.0 parts, carboxymethylcellulose Na 2.0 parts, pearlite 35.0 parts, diatomaceous earth 35.0 parts, clay 7.5 parts, granulation diameter 3.0 mm, according to Example 18, a water-floating pesticide formulation Prepared. The particle size of the obtained formulation was 93% in the range of 2.80 to 1.70 mm, the long diameter/short diameter ratio at the bottom was 1.3, and the number of particles per 1 g was 95.

[Example 31]

The formulation composition was 12.0 parts of pymetrozine (insecticide active ingredient), Shirasu balloon (average particle diameter 90 to 120 μm) (floating carrier) 28.0 parts, alkylnaphthalenesulfonic acid Na 3.0 parts, alkylnaphthalenesulfonic acid formaldehyde condensate Na 3.0 parts, Acrylic-vinylsulfonic acid copolymer Na 3.0 parts, carboxymethylcellulose Na 2.0 parts, bentonite 10.0 parts, pearlite 30.0 parts, clay 9.0 parts, granulation diameter 2.8 mm, according to Example 18, a water-floating pesticide formulation was prepared . The particle size of the obtained formulation was 84% in the range of 2.80 to 1.70 mm, the long/short diameter ratio at the bottom was 1.4, and the number of particles per 1 g was 108.

[Example 32]

Formulation composition of pimetrozine 12.0 parts (insecticide 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, carboxymethylcellulose Na 2.0 parts, bentonite 10.0 parts, pearlite 19.5 parts, white carbon 15.0 parts, clay 4.0 parts, granulation diameter 3.0 mm, according to Example 18 water surface A floating pesticide formulation was prepared. The particle size of the obtained formulation was 83% in the range of 2.80 to 1.70 mm, the long/short diameter ratio at the bottom was 1.2, and the number of particles per 1 g was 90.

[Example 33]

Formulation composition of pimetrozine 12.0 parts (insecticide active ingredient), Shirasu balloon (average particle diameter 90 to 120 μm) (floating carrier) 30.0 parts, alkyl naphthalene sulfonic acid Na 3.0 parts, partially desulfonated lignin sulfonic acid Na 3.0 parts, acrylic- Maleic acid copolymer Na 2.0 parts, carboxymethylcellulose Na 2.0 parts, pearlite 40.0 parts, clay 8.0 parts, granulation diameter 3.0 mm, according to Example 18, to prepare a water-floating pesticide formulation. The particle size of the obtained formulation was 95% in the range of 2.80 to 1.70 mm, the long/short diameter ratio at the bottom was 1.4, and the number of particles per 1 g was 88.

[Example 34]

Formulation composition of pimetrozine 12.0 parts (insecticide active ingredient), Shirasu balloon (average particle diameter 90 to 120 μm) (floating carrier) 30.0 parts, dialkyl succinate sulfonic acid Na 1.5 parts, alkyl naphthalene sulfonic acid formaldehyde condensate Na 3.0 Part, 2.0 parts of polyacrylate Na, 2.0 parts of carboxymethylcellulose Na, 44.5 parts of diatomaceous earth, 5.0 parts of clay, and a granulation diameter of 2.8 mm were used to prepare a water-floating pesticide formulation based on Example 18. The particle size of the obtained formulation was 96% in the range of 2.80 to 1.70 mm, the long/short diameter ratio at the bottom was 1.2, and the number of particles per 1 g was 99.

[Example 35]

After mixing 10.0 parts of iffencarbazone (herbicidal active ingredient), 1.0 part of alkylnaphthalenesulfonic acid, and 14.0 parts of water, wet grinding with a Dino Mill (Shinmaru Enterprises) until the average particle diameter is 1.0 μm, and slurry Got it. In addition, Shirasu balloon (average particle diameter 70 to 90 μm) (floating carrier) 25.0 parts, alkyl naphthalene sulfonic acid Na 2.0 parts, polyvinyl alcohol 2.0 parts, bentonite 5.0 parts, pearlite 42.0 parts, clay 13.0 parts hammer mill (sample mill KIIW-1, Dalton Corporation) pulverized and mixed, and a powder mixture was obtained. The obtained slurry and powder mixture were put in a double arm kneader (KDHJ, Dalton Corporation), and kneaded for 15 minutes after watering. Next, the kneaded water was assembled with an extrusion granulator equipped with a basket-type screen having a pore diameter of 3.0 mm. After pre-drying the obtained granulated product, it was sized with a drum-type sizer, and dried with a fluidized bed dryer. This was sieved to a size of 3.35 mm to 2.00 mm to obtain a surface-floating pesticide formulation. The particle size of the obtained formulation was 84% in the range of 2.80 to 1.70 mm, the long/short diameter ratio at the bottom was 1.4, and the number of particles per 1 g was 109.

[Example 36]

The formulation composition was 10.0 parts of iffencarbazone (herbicidal active ingredient), fly ash balloon (average particle diameter of 80 to 120 μm) (floating carrier) 28.0 parts, dialkyl succinate sulfonic acid Na 1.5 parts, carboxymethylcellulose Na 2.0 parts, Pearlite 51.5 parts, clay 7.0 parts (the composition used in the slurry is 10.0 parts of iffencarbazone, 1.0 parts of dialkyl succinate sulfonic acid Na, 14.0 parts of water), a granulation diameter of 2.8 mm, and water surface according to Example 35 A floating pesticide formulation was prepared. The particle size of the obtained formulation was 86% in the range of 2.80 to 1.70 mm, the long/short diameter ratio at the bottom was 1.2, and the number of particles per 1 g was 115.

[Example 37]

Formulation composition is 10.0 parts of iffencarbazone (herbicidal active ingredient), acrylonitrile resin balloon (average particle diameter 20 to 40 μm) (floating carrier) 2.0 parts, alkylnaphthalenesulfonic acid Na 3.0 parts, polyacrylic acid Na 2.0 parts, carboxy Methylcellulose Na 3.0 parts, pearlite 70.0 parts, clay 10.0 parts (the composition used in the slurry is 10.0 parts iffencarbazone, alkylnaphthalene sulfonic acid Na 1.0 parts, water 14.0 parts), a granulation diameter of 3.0 mm, Example 35 A water-floating pesticide formulation was prepared in accordance with the following. The particle size of the obtained formulation was 88% in the range of 2.80 to 1.70 mm, the long/short diameter ratio 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 iffencarbazone (herbicidal active ingredient), ceramic balloon (average particle diameter of 20 to 150 μm) (floating carrier) 28.0 parts, alkylnaphthalenesulfonic acid Na 3.0 parts, polyacrylic acid Na 2.0 parts, carboxymethylcellulose Na 3.0 parts, diatomaceous earth 48.0 parts, clay 8.0 parts (the composition used in the slurry is 10.0 parts of iffencarbazone, 1.0 parts of alkylnaphthalenesulfonic acid Na, 14.0 parts of water), a granulation diameter of 3.0 mm, according to Example 35 A water-floating pesticide formulation was prepared. The particle size of the obtained formulation was 92% in the range of 2.80 to 1.70 mm, the long diameter/short diameter ratio at the bottom was 1.3, and the number of particles per 1 g was 103.

[Example 39]

Formulation composition is 10.0 parts of iffencarbazone (herbicidal active ingredient), Shirasu balloon (average particle diameter of 70 to 90 μm) (floating carrier) 25.0 parts, dialkyl succinate sulfonic acid Na 1.5 parts, acrylic acid-maleic acid copolymer Na 2.0 parts , Carboxymethylcellulose Na 3.0 parts, bentonite 10.0 parts, pearlite 33.5 parts, white carbon 10.0 parts, clay 5.0 parts (the composition used in the slurry is iffencarbazone 10.0 parts, dialkyl succinate sulfonic acid Na 1.0 parts, water 14.0 Part), the granulation diameter was 2.8 mm, and a water-floating pesticide formulation was prepared in accordance with Example 35. The particle size of the obtained formulation was 95% in the range of 2.80 to 1.70 mm, the long diameter/short diameter ratio at the bottom was 1.4, and the number of particles per 1 g was 100.

[Example 40]

Formulation composition: 10.0 parts of iffencarbazone (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 Na 2.0 parts , Carboxymethylcellulose Na 2.0 parts, diatomaceous earth 43.0 parts, clay 10.0 parts (the composition used in the slurry is 10.0 parts of iffencarbazone, 1.0 parts of alkylnaphthalenesulfonic acid Na, 14.0 parts of water), and a granulation diameter of 2.8 mm. According to Example 35, a surface-floating pesticide formulation was prepared. The particle size of the obtained formulation was 87% in the range of 2.80 to 1.70 mm, the long/short diameter ratio at the bottom was 1.1, and the number of particles per 1 g was 123.

[Example 41]

Formulation composition is 10.0 parts of iffencarbazone (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, polyacrylate Na 3.0 parts, carboxymethyl 3.0 parts of cellulose Na, 50.0 parts of diatomaceous earth, 7.5 parts of clay (the composition used in the slurry is 10.0 parts of iffencarbazone, 1.0 parts of dialkyl succinate sulfonic acid Na, 14.0 parts of water), and a granulation diameter of 3.0 mm. In accordance with 35, a surface-floating pesticide formulation was prepared. The particle size of the obtained formulation was 84% in the range of 2.80 to 1.70 mm, the long/short diameter ratio at the bottom was 1.3, and the number of particles per 1 g was 109.

[Example 42]

The formulation composition was 10.0 parts of iffencarbazone (herbicidal active ingredient), Shirasu balloon (average particle diameter 90 to 120 μm) (floating carrier) 30.0 parts, alkylnaphthalenesulfonic acid Na 3.0 parts, acrylic-maleic acid copolymer Na 3.0 parts, carboxy Methylcellulose Na 2.0 parts, pearlite 45.0 parts, clay 7.0 parts (the composition used in the slurry is 10.0 parts of iffencarbazone, 1.0 parts of alkylnaphthalene sulfonic acid Na, 14.0 parts of water), a granulation diameter of 3.0 mm, and Example 35 A water-floating pesticide formulation was prepared in accordance with the following. The particle size of the obtained formulation was 96% in the range of 2.80 to 1.70 mm, the long/short diameter ratio at the bottom was 1.3, and the number of particles per 1 g was 103.

[Example 43]

The formulation composition was 10.0 parts of iffencarbazone (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, acrylic acid-vinyl sulfonic acid copolymer Na 3.0 Parts, carboxymethylcellulose Na 3.0 parts, pearlite 50.0 parts, clay 4.5 parts (the composition used in the slurry is 10.0 parts iffencarbazone, dialkyl succinate sulfonic acid Na 1.0 parts, water 14.0 parts), a granulation diameter of 2.8 mm Then, in accordance with Example 35, a surface-floating pesticide formulation was prepared. The particle size of the obtained formulation was 95% in the range of 2.80 to 1.70 mm, the long diameter/short diameter ratio at the bottom was 1.2, and the number of particles per 1 g was 126.

[Example 44]

Formulation composition is 10.0 parts of iffencarbazone (herbicidal active ingredient), Shirasu balloon (average particle diameter 70 to 90 μm) (floating carrier) 28.0 parts, alkylnaphthalenesulfonic acid Na 3.0 parts, alkylnaphthalenesulfonic acid formaldehyde condensate Na 3.0 parts , Acrylic-methacrylic acid copolymer Na 3.0 parts, carboxymethylcellulose Na 2.0 parts, pearlite 46.0 parts, clay 5.0 parts (the composition used in the slurry is iffencarbazone 10.0 parts, alkylnaphthalenesulfonic acid Na 1.0 part, water 14.0) Part), the granulation diameter was 2.8 mm, and a water-floating pesticide formulation was prepared in accordance with Example 35. The particle size of the obtained formulation was 86% in the range of 2.80 to 1.70 mm, the long/short diameter ratio at the bottom was 1.2, and the number of particles per 1 g was 113.

[Example 45]

The formulation composition was 10.0 parts of iffencarbazone (herbicidal active ingredient), fly ash balloon (average particle diameter 80 to 120 μm) (floating carrier) 28.0 parts, dialkyl succinate sulfonic acid Na 1.5 parts, partially desulfonated lignin sulfonic acid Na 3.0 Parts, polyacrylic acid Na 2.0 parts, carboxymethylcellulose Na 2.0 parts, bentonite 10.0 parts, pearlite 20.0 parts, white carbon 15.0 parts, clay 8.5 parts (the composition used in the slurry is iffencarbazone 10.0 parts, dialkyl succinate Sulfonic acid Na 1.0 part, water 14.0 parts), granulation diameter 3.0 mm, according to Example 35, the water surface floating pesticide preparation was prepared. The particle size of the obtained formulation was 84% in the range of 2.80 to 1.70 mm, the long/short diameter ratio at the bottom was 1.4, and the number of particles per 1 g was 99.

[Example 46]

The formulation composition was 10.0 parts of iffencarbazone (herbicidal active ingredient), 28.0 parts of ceramic balloon (average particle diameter 20 to 150 μm) (floating carrier), 3.0 parts of alkylnaphthalenesulfonic acid Na, 3.0 parts of naphthalenesulfonic acid formaldehyde condensate Na, Acrylic-vinylsulfonic acid copolymer Na 2.0 parts, carboxymethylcellulose Na 3.0 parts, bentonite 10.0 parts, diatomaceous earth 38.0 parts, clay 6.0 parts (the composition used in the slurry is iffencarbazone 10.0 parts, alkyl naphthalene sulfonic acid Na 1.0 parts, 14.0 parts of water) and a granulation diameter of 2.8 mm, according to Example 35, a water-floating pesticide formulation was prepared. The particle size of the obtained formulation was 96% in the range of 2.80 to 1.70 mm, the long diameter/short diameter ratio at the bottom was 1.1, and the number of particles per 1 g was 108.

[Example 47]

Formulation composition is 10.0 parts of iffencarbazone (herbicidal active ingredient), acrylonitrile resin balloon (average particle diameter 20 to 40 μm) (floating carrier) 2.0 parts, dialkyl succinate sulfonic acid Na 1.5 parts, partially desulfonated lignin sulfonic acid Na 3.0 parts, acrylic acid-maleic acid copolymer Na 2.0 parts, carboxymethylcellulose Na 2.0 parts, pearlite 10.0 parts, diatomaceous earth 61.5 parts, clay 8.0 parts (the composition used in the slurry is iffencarbazone 10.0 parts, dialkyl succinate Sulfonic acid Na 1.0 part, water 14.0 parts), granulation diameter 3.0 mm, according to Example 35, the water surface floating pesticide preparation was prepared. The particle size of the obtained formulation was 93% in the range of 2.80 to 1.70 mm, the long/short diameter ratio at the bottom was 1.4, and the number of particles per 1 g was 103.

[Example 48]

Formulation composition is 10.0 parts of iffencarbazone (herbicidal active ingredient), Shirasu balloon (average particle diameter 90-120 μm) (floating carrier) 25.0 parts, alkylnaphthalenesulfonic acid Na 3.0 parts, alkylnaphthalenesulfonic acid formaldehyde condensate Na 3.0 parts , Acrylic-vinylsulfonic acid copolymer Na 2.0 parts, carboxymethylcellulose Na 3.0 parts, bentonite 10.0 parts, pearlite 38.0 parts, clay 6.0 parts (the composition used in the slurry is iffencarbazone 10.0 parts, alkyl naphthalene sulfonic acid Na 1.0 part , 14.0 parts of water), and a granulation diameter of 2.8 mm, to prepare a water-floating pesticide formulation in accordance with Example 35. The particle size of the obtained formulation was 84% in the range of 2.80 to 1.70 mm, the long/short diameter ratio at the bottom was 1.2, and the number of particles per 1 g was 113.

[Example 49]

Formulation composition is 10.0 parts of iffencarbazone (herbicidal active ingredient), Shirasu balloon (average particle diameter 90-120 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, carboxymethylcellulose Na 3.0 parts, bentonite 10.0 parts, pearlite 25.0 parts, white carbon 10.0 parts, clay 7.5 parts (the composition used in the slurry is iffencarbazone 10.0 parts , Dialkyl succinate sulfonic acid Na 1.0 part, water 14.0 parts), granulation diameter 3.0 mm, according to Example 35, the water surface floating pesticide preparation was prepared. The particle size of the obtained formulation was 83% in the range of 2.80 to 1.70 mm, the long/short diameter ratio at the bottom was 1.1, and the number of particles per 1 g was 96.

[Example 50]

The formulation composition was 10.0 parts of iffencarbazone (herbicidal active ingredient), Shirasu balloon (average particle diameter 90-120 μm) (floating carrier) 25.0 parts, alkylnaphthalenesulfonic acid Na 3.0 parts, partially desulfonated lignin sulfonic acid Na 3.0 parts, acrylic -Maleic acid copolymer Na 3.0 parts, carboxymethylcellulose Na 2.0 parts, pearlite 45.0 parts, clay 9.0 parts (the composition used in the slurry is iffencarbazone 10.0 parts, alkylnaphthalenesulfonic acid Na 1.0 parts, water 14.0 parts), granulated With a diameter of 3.0 mm, a water-floating pesticide formulation was prepared in accordance with Example 35. The particle size of the obtained formulation was 94% in the range of 2.80 to 1.70 mm, the long diameter/short diameter ratio at the bottom was 1.3, and the number of particles per 1 g was 97.

[Example 51]

Formulation composition is 10.0 parts of iffencarbazone (herbicidal active ingredient), Shirasu balloon (average particle diameter 90-120 μm) (floating carrier) 28.0 parts, dialkyl succinate sulfonic acid Na 1.5 parts, alkylnaphthalene sulfonic 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 in the slurry is 10.0 parts of iffencarbazone, dialkyl succinate sulfonic acid Na 1.0 part, water 14.0 parts ), the granulation diameter was 2.8 mm, and a water-floating pesticide formulation was prepared in accordance with Example 35. The particle size of the obtained formulation was 97% in the range of 2.80 to 1.70 mm, the long diameter/short diameter ratio at the bottom was 1.2, and the number of particles per 1 g was 90.

[Example 52]

Cymethrin 12.0 parts (herbicidal active ingredient), Shirasu balloon (average particle diameter 70 to 90 μm) (floating carrier) 30.0 parts, alkylnaphthalenesulfonic acid Na 3.0 parts, dextrin 5.0 parts, bentonite 10.0 parts, pearlite 38.0 parts, clay 2.0 parts were pulverized and mixed with a hammer mill (sample mill KIIW-1, Dalton Corporation), and a powder mixture was obtained. The obtained powder mixture was put in a double arm kneader (KDHJ, Dalton Corporation), and kneaded for 15 minutes after adding water. Next, the kneaded water was assembled with an extrusion granulator equipped with a basket-type screen having a pore diameter of 3.0 mm. After pre-drying the obtained granulated product, it was sized with a drum-type sizer and dried with a fluidized bed dryer. This was sieved to a size of 3.35 mm to 2.00 mm to obtain a surface-floating pesticide formulation. The particle size of the obtained formulation was 83% in the range of 2.80 to 1.70 mm, the long/short diameter ratio at the bottom was 1.4, and the number of particles per 1 g was 93.

[Example 53]

Formulation composition was 12.0 parts of cymethrin (herbicidal active ingredient), fly ash balloon (average particle diameter 80 to 120 μm) (floating carrier) 28.0 parts, dialkyl succinate sulfonic acid Na 1.5 parts, carboxymethylcellulose Na 3.0 parts, pearlite With 43.0 parts, clay 12.5 parts, and a granulation diameter of 2.8 mm, in accordance with Example 50, a water-floating pesticide formulation was prepared. The particle size of the obtained formulation was 85% in the range of 2.80 to 1.70 mm, the long diameter/short diameter ratio at the bottom was 1.2, and the number of particles per 1 g was 88.

[Example 54]

The formulation composition was 12.0 parts of cymethrin (herbicidal active ingredient), acrylonitrile resin balloon (average particle diameter 20 to 40 μm) (floating carrier) 2.0 parts, alkylnaphthalenesulfonic acid Na 3.0 parts, polyacrylate Na 2.0 parts, carboxymethyl With 2.0 parts of cellulose Na, 65.0 parts of pearlite, 14.0 parts of clay, and 3.0 mm of granulation diameter, a water-floating pesticide formulation was prepared in accordance with Example 52. The particle size of the obtained formulation was 87% in the range of 2.80 to 1.70 mm, the long/short diameter ratio at the bottom was 1.4, and the number of particles per 1 g was 97.

[Example 55]

The formulation composition was 12.0 parts of cymethrin (herbicidal active ingredient), 28.0 parts of ceramic balloon (average particle diameter 20 to 150 μm) (floating carrier), 3.0 parts of alkylnaphthalenesulfonic acid Na, 3.0 parts of carboxymethylcellulose Na, and 45.0 parts of diatomaceous earth, With 9.0 parts of clay and 3.0 mm in granulation diameter, a water-floating pesticide formulation was prepared in accordance with Example 52. The particle size of the obtained formulation was 93% in the range of 2.80 to 1.70 mm, the long/short diameter ratio at the bottom was 1.3, and the number of particles per 1 g was 96.

[Example 56]

The formulation composition was 12.0 parts of cymethrin (herbicidal active ingredient), 28.0 parts of Shirasu balloon (average particle diameter 70-90 μm) (floating carrier), 1.5 parts of dialkyl succinate sulfonic acid Na, 2.0 parts of acrylic acid-maleic acid copolymer Na, Carboxymethylcellulose Na 3.0 parts, bentonite 10.0 parts, pearlite 30.0 parts, white carbon 8.0 parts, clay 5.5 parts, granulation diameter 2.8 mm, according to Example 52, to prepare a water-floating pesticide formulation. The particle size of the obtained formulation was 96% in the range of 2.80 to 1.70 mm, the long/short diameter ratio at the bottom was 1.4, and the number of particles per 1 g was 108.

[Example 57]

The formulation composition was 12.0 parts of cymethrin (herbicidal active ingredient), 28.0 parts of Shirasu balloon (average particle diameter 90-120 μm) (floating carrier), 3.0 parts of alkylnaphthalenesulfonic acid Na, 2.0 parts of acrylic-methacrylic acid copolymer Na, Carboxymethylcellulose Na 3.0 parts, diatomaceous earth 47.0 parts, clay 5.0 parts, granulation diameter 2.8 mm, according to Example 52, to prepare a water-floating pesticide formulation. The particle size of the obtained formulation was 87% in the range of 2.80 to 1.70 mm, the long/short diameter ratio at the bottom was 1.2, and the number of particles per 1 g was 95.

[Example 58]

The formulation composition was 12.0 parts of cymethrin (herbicidal active ingredient), 30.0 parts of Shirasu balloon (average particle diameter 90 to 120 μm) (floating carrier), 1.5 parts of dialkyl succinate sulfonic acid Na, 3.0 parts of polyacrylate Na, and carboxymethylcellulose. With 3.0 parts of Na, 45.0 parts of diatomaceous earth, 5.5 parts of clay, and 3.0 mm of granulated diameter, a water-floating pesticide formulation was prepared in accordance with Example 52. The particle size of the obtained formulation was 84% in the range of 2.80 to 1.70 mm, the long/short diameter ratio at the bottom was 1.4, and the number of particles per 1 g was 97.

[Example 59]

The formulation composition was 12.0 parts of cymethrin (herbicidal active ingredient), 30.0 parts of Shirasu balloon (average particle diameter 90 to 120 μm) (floating carrier), 3.0 parts of alkylnaphthalenesulfonic acid Na, 3.0 parts of acrylic-maleic acid copolymer Na, carboxymethyl With 2.0 parts of cellulose Na, 46.0 parts of pearlite, 4.0 parts of clay, and 3.0 mm of granulated diameter, a water-floating pesticide formulation was prepared in accordance with Example 52. The particle size of the obtained formulation was 96% in the range of 2.80 to 1.70 mm, the long/short diameter ratio at the bottom was 1.2, and the number of particles per 1 g was 93.

[Example 60]

The formulation composition was 12.0 parts of cymethrin (herbicidal active ingredient), 30.0 parts of Shirasu balloon (average particle diameter 90-120 μm) (floating carrier), 1.5 parts of dialkyl succinate sulfonic acid Na, 2.0 parts of acrylic acid-vinylsulfonic acid copolymer Na , Carboxymethylcellulose Na 2.0 parts, pearlite 47.5 parts, clay 5.0 parts, granulation diameter 2.8 mm, and according to Example 52, a water-floating pesticide formulation was prepared. The particle size of the obtained formulation was 94% in the range of 2.80 to 1.70 mm, the long/short diameter ratio at the bottom was 1.4, and the number of particles per 1 g was 98.

[Example 61]

The formulation composition was 12.0 parts of cymethrin (herbicidal active ingredient), 30.0 parts of Shirasu balloon (average particle diameter 70-90 μm) (floating carrier), 3.0 parts of alkylnaphthalenesulfonic acid Na, 3.0 parts of alkylnaphthalenesulfonic acid formaldehyde condensate Na, Acrylic-methacrylic acid copolymer Na 2.0 parts, carboxymethylcellulose Na 2.0 parts, pearlite 40.0 parts, clay 8.0 parts, granulation diameter 2.8 mm, according to Example 52, to prepare a water-floating pesticide formulation. The particle size of the obtained formulation was 84% in the range of 2.80 to 1.70 mm, the long/short diameter ratio at the bottom was 1.3, and the number of particles per 1 g was 108.

[Example 62]

Formulation composition was 12.0 parts of cymethrin (herbicidal active ingredient), fly ash balloon (average particle diameter 80 to 120 μm) (floating carrier) 28.0 parts, dialkyl succinate sulfonic acid Na 1.5 parts, partially desulfonated lignin sulfonic acid Na 3.0 parts , Polyacrylic acid Na 3.0 parts, carboxymethylcellulose Na 2.0 parts, bentonite 10.0 parts, pearlite 25.0 parts, white carbon 10.0 parts, clay 5.5 parts, granulation diameter 3.0 mm, according to Example 52, a water-floating pesticide formulation Prepared. The particle size of the obtained formulation was 83% in the range of 2.80 to 1.70 mm, the long/short diameter ratio at the bottom was 1.4, and the number of particles per 1 g was 100.

[Example 63]

The formulation composition was 12.0 parts of cymethrin (herbicidal active ingredient), 30.0 parts of ceramic balloon (average particle diameter 20 to 150 μm) (floating carrier), 3.0 parts of alkylnaphthalenesulfonic acid Na, 3.0 parts of naphthalenesulfonic acid formaldehyde condensate Na, acrylic -Vinyl sulfonic acid copolymer Na 3.0 parts, carboxymethylcellulose Na 2.0 parts, bentonite 10.0 parts, diatomaceous earth 30.0 parts, clay 7.0 parts, granulation diameter 2.8 mm, according to Example 52, a water-floating pesticide formulation was prepared. The particle size of the obtained formulation was 95% in the range of 2.80 to 1.70 mm, the long/short diameter ratio at the bottom was 1.2, and the number of particles per 1 g was 97.

[Example 64]

The formulation composition was 12.0 parts of cymethrin (herbicidal active ingredient), acrylonitrile resin balloon (average particle diameter 20 to 40 μm) (floating carrier) 2.0 parts, dialkyl succinate sulfonic acid Na 1.5 parts, partially desulfonated lignin sulfonic acid Na 3.0 parts, acrylic acid-maleic acid copolymer Na 2.0 parts, carboxymethylcellulose Na 2.0 parts, diatomaceous earth 67.5 parts, clay 10.0 parts, granulation diameter 3.0 mm, according to Example 52, a water-floating pesticide formulation was prepared. The particle size of the obtained formulation was 94% in the range of 2.80 to 1.70 mm, the long/short diameter ratio at the bottom was 1.2, and the number of particles per 1 g was 96.

[Example 65]

The formulation composition was 12.0 parts of cymethrin (herbicidal active ingredient), 30.0 parts of Shirasu balloon (average particle diameter 90-120 μm) (floating carrier), 3.0 parts of alkylnaphthalenesulfonic acid Na, 3.0 parts of alkylnaphthalenesulfonic acid formaldehyde condensate Na, Acrylic-vinyl sulfonic acid copolymer Na 3.0 parts, carboxymethylcellulose Na 2.0 parts, bentonite 10.0 parts, pearlite 30.0 parts, clay 7.0 parts, granulation diameter 2.8 mm, according to Example 52, a water-floating pesticide formulation was prepared. . The particle size of the obtained formulation was 86% in the range of 2.80 to 1.70 mm, the long/short diameter ratio at the bottom was 1.4, and the number of particles per 1 g was 93.

[Example 66]

The formulation composition was 12.0 parts of cymethrin (herbicidal active ingredient), 30.0 parts of Shirasu balloon (average particle diameter 90-120 μm) (floating carrier), 1.5 parts of dialkyl succinate sulfonic acid Na, 3.0 parts of naphthalene sulfonic acid formaldehyde condensate Na , Acrylic acid-methacrylic acid copolymer Na 2.0 parts, carboxymethylcellulose Na 2.0 parts, bentonite 10.0 parts, pearlite 20.0 parts, white carbon 15.0 parts, clay 4.5 parts, granulation diameter 3.0 mm, according to Example 52 A floating pesticide formulation was prepared. The particle size of the obtained formulation was 83% in the range of 2.80 to 1.70 mm, the long/short diameter ratio at the bottom was 1.4, and the number of particles per 1 g was 101.

[Example 67]

The formulation composition was 12.0 parts of cymethrin (herbicidal active ingredient), 30.0 parts of Shirasu balloon (average particle diameter 90-120 μm) (floating carrier), 3.0 parts of alkylnaphthalenesulfonic acid Na, 3.0 parts of partially desulfonated ligninsulfonic acid Na, acrylic- Maleic acid copolymer Na 3.0 parts, carboxymethylcellulose Na 3.0 parts, pearlite 39.0 parts, clay 7.0 parts, granulation diameter 3.0 mm, according to Example 52, the water-floating pesticide preparation was prepared. The particle size of the obtained formulation was 93% in the range of 2.80 to 1.70 mm, the long diameter/short diameter ratio at the bottom was 1.1, and the number of particles per 1 g was 94.

[Example 68]

The formulation composition was 12.0 parts of cymethrin (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, alkylnaphthalene sulfonic acid formaldehyde condensate Na 3.0 Part, 2.0 parts of polyacrylate Na, 3.0 parts of carboxymethylcellulose Na, 48.5 parts of diatomaceous earth, 5.0 parts of clay, and a granulation diameter of 2.8 mm were used to prepare a water-floating pesticide formulation based on Example 52. The particle size of the obtained formulation was 97% in the range of 2.80 to 1.70 mm, the long/short diameter ratio at the bottom was 1.2, and the number of particles per 1 g was 98.

[Example 69]

Benfurusate 18.0 parts (herbicidal active ingredient), Shirasu balloon (average particle diameter 70 to 90 μm) (floating carrier) 30.0 parts, alkyl naphthalene sulfonic acid Na 3.0 parts, dextrin 3.0 parts, polyvinyl alcohol 1.0 part, bentonite 5.0 parts , 30.0 parts of pearlite and 10.0 parts of clay were pulverized and mixed with a hammer mill (sample mill KIIW-1, Dalton Corporation) to obtain a powder mixture. The obtained powder mixture was put in a double arm kneader (KDHJ, Dalton Corporation), and kneaded for 15 minutes after adding water. Next, the kneaded water was assembled with an extrusion granulator equipped with a basket-type screen having a pore diameter of 3.0 mm. After pre-drying the obtained granulated product, it was sized with a drum-type sizer and dried with a fluidized bed dryer. This was sieved to a size of 3.35 mm to 2.00 mm to obtain a surface-floating pesticide formulation. The particle size of the obtained formulation was 83% in the range of 2.80 to 1.70 mm, the long/short diameter ratio at the bottom was 1.2, and the number of particles per 1 g was 93.

[Example 70]

The formulation composition was 18.0 parts of benfurusate (herbicidal active ingredient), fly ash balloon (average particle diameter 80 to 120 μm) (floating carrier) 28.0 parts, dialkyl succinate sulfonic acid Na 1.5 parts, carboxymethylcellulose Na 2.0 parts, pearlite With 45.5 parts, clay 5.0 parts, and a granulation diameter of 2.8 mm, in accordance with Example 50, a water-floating pesticide formulation was prepared. The particle size of the obtained formulation was 87% in the range of 2.80 to 1.70 mm, the long/short diameter ratio at the bottom was 1.4, and the number of particles per 1 g was 83.

[Example 71]

The formulation composition was 18.0 parts of benfurusate (herbicidal active ingredient), acrylonitrile resin balloon (average particle diameter 20 to 40 μm) (floating carrier) 2.0 parts, alkylnaphthalenesulfonic acid Na 3.0 parts, polyacrylate Na 2.0 parts, carboxymethyl With 2.0 parts of cellulose Na, 63.0 parts of pearlite, 10.0 parts of clay, and 3.0 mm of granulated diameter, a water-floating pesticide formulation was prepared in accordance with Example 69. The particle size of the obtained formulation was 84% in the range of 2.80 to 1.70 mm, the long/short diameter ratio at the bottom was 1.3, and the number of particles per 1 g was 86.

[Example 72]

The formulation composition was 18.0 parts of benfurusate (herbicidal active ingredient), ceramic balloon (average particle diameter of 20 to 150 μm) (floating carrier) 30.0 parts, alkylnaphthalenesulfonic acid Na 3.0 parts, carboxymethylcellulose Na 3.0 parts, diatomaceous earth 39.0 parts, With 7.0 parts of clay and 3.0 mm of granulated diameter, a water-floating pesticide formulation was prepared in accordance with Example 69. The particle size of the obtained formulation was 94% in the range of 2.80 to 1.70 mm, the long-diameter/short-diameter ratio at the bottom was 1.4, and the number of particles per 1 g was 97.

[Example 73]

The formulation composition was 18.0 parts of benfurusate (herbicidal active ingredient), Shirasu balloon (average particle diameter 70-90 μm) (floating carrier) 28.0 parts, dialkyl succinate sulfonic acid Na 1.5 parts, acrylic acid-maleic acid copolymer Na 2.0 parts, Carboxymethylcellulose Na 3.0 parts, bentonite 10.0 parts, pearlite 25.0 parts, white carbon 7.5 parts, clay 5.0 parts, granulation diameter 2.8 mm, according to Example 69, a water-floating pesticide formulation was prepared. The particle size of the obtained formulation was 93% in the range of 2.80 to 1.70 mm, the long/short diameter ratio at the bottom was 1.2, and the number of particles per 1 g was 82.

[Example 74]

The formulation composition was 18.0 parts of benfurusate (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 Na 2.0 parts, Carboxymethylcellulose Na 2.0 parts, diatomaceous earth 40.0 parts, clay 5.0 parts, granulation diameter 2.8 mm, according to Example 69, to prepare a water-floating pesticide formulation. The particle size of the obtained formulation was 86% in the range of 2.80 to 1.70 mm, the long diameter/short diameter ratio at the bottom was 1.4, and the number of particles per 1 g was 85.

[Example 75]

The formulation composition was 18.0 parts of benfursate (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, polyacrylic acid Na 3.0 parts, carboxymethylcellulose With 2.0 parts of Na, 40.0 parts of diatomaceous earth, 5.5 parts of clay, and 3.0 mm of granulated diameter, a water-floating pesticide formulation was prepared in accordance with Example 69. The particle size of the obtained formulation was 85% in the range of 2.80 to 1.70 mm, the long/short diameter ratio at the bottom was 1.3, and the number of particles per 1 g was 80.

[Example 76]

The formulation composition was 18.0 parts of benfurusate (herbicidal active ingredient), Shirasu balloon (average particle diameter 90 to 120 μm) (floating carrier) 28.0 parts, alkylnaphthalenesulfonic acid Na 3.0 parts, acrylic-maleic acid copolymer Na 3.0 parts, carboxymethyl With 2.0 parts of cellulose Na, 38.0 parts of pearlite, 8.0 parts of clay, and 3.0 mm of granulated diameter, a water-floating pesticide formulation was prepared in accordance with Example 69. The particle size of the obtained formulation was 93% in the range of 2.80 to 1.70 mm, the long/short diameter ratio at the bottom was 1.2, and the number of particles per 1 g was 91.

[Example 77]

The formulation composition was 18.0 parts of benfurusate (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 copolymer Na 2.0 parts , Carboxymethylcellulose Na 2.0 parts, pearlite 46.5 parts, clay 5.0 parts, granulation diameter 2.8 mm, according to Example 69, to prepare a water-floating pesticide formulation. The particle size of the obtained formulation was 97% in the range of 2.80 to 1.70 mm, the long diameter/short diameter ratio at the bottom was 1.1, and the number of particles per 1 g was 79.

[Example 78]

The formulation composition was 18.0 parts of benfurusate (herbicidal active ingredient), Shirasu balloon (average particle diameter 70 to 90 μm) (floating carrier) 28.0 parts, alkylnaphthalenesulfonic acid Na 3.0 parts, alkylnaphthalenesulfonic acid formaldehyde condensate Na 3.0 parts, Acrylic-methacrylic acid copolymer Na 2.0 parts, carboxymethylcellulose Na 2.0 parts, pearlite 39.0 parts, clay 5.0 parts, granulation diameter 2.8 mm, according to Example 69, a water-floating pesticide formulation was prepared. The particle size of the obtained formulation was 84% in the range of 2.80 to 1.70 mm, the long/short diameter ratio at the bottom was 1.2, and the number of particles per 1 g was 75.

[Example 79]

The formulation composition was 18.0 parts of benfurusate (herbicidal active ingredient), fly ash balloon (average particle diameter 80 to 120 μm) (floating carrier) 30.0 parts, dialkyl succinate sulfonic acid Na 1.5 parts, partially desulfonated lignin sulfonic acid Na 3.0 parts , Polyacrylic acid Na 2.0 parts, carboxymethylcellulose Na 2.0 parts, bentonite 10.0 parts, pearlite 18.5 parts, white carbon 10.0 parts, clay 5.0 parts, granulation diameter 3.0 mm, according to Example 69, a water-floating pesticide formulation Prepared. The particle size of the obtained formulation was 83% in the range of 2.80 to 1.70 mm, the long/short diameter ratio at the bottom was 1.4, and the number of particles per 1 g was 98.

[Example 80]

The formulation composition was 18.0 parts of benfurusate (herbicidal active ingredient), ceramic balloon (average particle diameter 20 to 150 μm) (floating carrier) 30.0 parts, alkyl naphthalene sulfonic acid Na 3.0 parts, naphthalene sulfonic acid formaldehyde condensate Na 3.0 parts, acrylic -Vinyl sulfonic acid copolymer Na 3.0 parts, carboxymethylcellulose Na 2.0 parts, bentonite 10.0 parts, diatomaceous earth 28.0 parts, clay 4.0 parts, granulation diameter 2.8 mm, according to Example 69, a water-floating pesticide formulation was prepared. The particle size of the obtained formulation was 97% in the range of 2.80 to 1.70 mm, the long/short diameter ratio at the bottom was 1.4, and the number of particles per 1 g was 89.

[Example 81]

The formulation composition was 18.0 parts of benfurusate (herbicidal active ingredient), acrylonitrile resin balloon (average particle diameter 20 to 40 μm) (floating carrier) 2.0 parts, dialkyl succinate sulfonic acid Na 1.5 parts, partially desulfonated lignin sulfonic acid Na 3.0 parts, acrylic acid-maleic acid copolymer Na 2.0 parts, carboxymethylcellulose Na 3.0 parts, diatomaceous earth 60.5 parts, clay 10.0 parts, granulation diameter 3.0 mm, according to Example 69, a water-floating pesticide formulation was prepared. The particle size of the obtained formulation was 95% in the range of 2.80 to 1.70 mm, the long diameter/short diameter ratio at the bottom was 1.3, and the number of particles per 1 g was 86.

[Example 82]

The formulation composition was 18.0 parts of benfurusate (herbicidal active ingredient), Shirasu balloon (average particle diameter 90 to 120 μm) (floating carrier) 28.0 parts, alkylnaphthalenesulfonic acid Na 3.0 parts, alkylnaphthalenesulfonic acid formaldehyde condensate Na 3.0 parts, Acrylic-vinyl sulfonic acid copolymer Na 3.0 parts, carboxymethylcellulose Na 3.0 parts, bentonite 10.0 parts, pearlite 28.0 parts, clay 4.0 parts, granulation diameter 2.8 mm, according to Example 69, a water-floating pesticide formulation was prepared. . The particle size of the obtained formulation was 83% in the range of 2.80 to 1.70 mm, the long/short diameter ratio at the bottom was 1.4, and the number of particles per 1 g was 98.

[Example 83]

The formulation composition was 18.0 parts of benfurusate (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, carboxymethylcellulose Na 3.0 parts, bentonite 10.0 parts, pearlite 15.0 parts, white carbon 12.0 parts, clay 4.5 parts, granulation diameter 3.0 mm, according to Example 69 water surface A floating pesticide formulation was prepared. The particle size of the obtained formulation was 84% in the range of 2.80 to 1.70 mm, the long/short diameter ratio at the bottom was 1.1, and the number of particles per 1 g was 101.

[Example 84]

The formulation composition was 18.0 parts of benfurusate (herbicidal active ingredient), Shirasu balloon (average particle diameter 90 to 120 μm) (floating carrier) 28.0 parts, alkylnaphthalenesulfonic acid Na 3.0 parts, partially desulfonated lignin sulfonic acid Na 3.0 parts, acrylic- Maleic acid copolymer Na 3.0 parts, carboxymethylcellulose Na 3.0 parts, pearlite 37.0 parts, clay 5.0 parts, granulation diameter was made into 3.0 mm, and the water-floating agrochemical formulation was prepared according to Example 69. The particle size of the obtained formulation was 95% in the range of 2.80 to 1.70 mm, the long/short diameter ratio at the bottom was 1.4, and the number of particles per 1 g was 96.

[Example 85]

The formulation composition was 18.0 parts of benfurusate (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, alkylnaphthalene sulfonic acid formaldehyde condensate Na 3.0 Part, 3.0 parts of polyacrylate Na, 3.0 parts of carboxymethylcellulose Na, 36.5 parts of diatomaceous earth, 5.0 parts of clay, and a granulation diameter of 2.8 mm were used to prepare a water-floating pesticide formulation based on Example 69. The particle size of the obtained formulation was 93% in the range of 2.80 to 1.70 mm, the long/short diameter ratio at the bottom was 1.3, and the number of particles per 1 g was 93.

[Comparative Example 1]

The formulation composition was gasgamycin 24.0 parts (sterilizing active ingredient), Shirasu balloon (average particle diameter 90-120 μm) (floating carrier) 25.0 parts, alkylnaphthalenesulfonic acid Na 3.0 parts, carboxymethylcellulose Na 2.0 parts, pearlite 40.0 parts, Clay 6.0 parts, granulation diameter 3.0 mm, sieves at the time of sifting were 3.35 mm and 0.85 mm sieves, according to Example 1, a water-floating pesticide formulation was prepared. The particle size of the obtained formulation is 72% in the range of 2.80 to 1.70 mm (the rest are 28% below the particle size 1.70 mm), the long/short diameter ratio at the bottom is 1.2, the number of particles per 1 g is 179, and the particle size is 1.70. A formulation having many particles smaller than mm was prepared.

[Comparative Example 2]

Formulation composition is gasgamycin 24.0 parts (sterilizing active ingredient), Shirasu balloon (average particle diameter 90 to 120 μm) (floating carrier) 25.0 parts, alkyl naphthalene sulfonic acid Na 3.0 parts, partially desulfonated lignin sulfonic acid Na 3.0 parts, carboxymethyl Cellulose Na 2.0 parts, pearlite 36.0 parts, clay 7.0 parts, granulation diameter 1.7 mm, sieve at the time of sieving was 2.00 mm and 0.85 mm sieve, according to Example 1, a water-floating pesticide formulation was prepared. The particle size of the obtained formulation is 5% in the range of 2.80 to 1.70 mm (the rest are 95% below the particle size 1.70 mm), the long/short diameter ratio at the bottom is 1.0, the number of particles per 1 g is 259, and 1.70 mm The following formulations having many small particles were prepared.

[Comparative Example 3]

The formulation composition was gasgamycin 24.0 parts (sterilizing active ingredient), Shirasu balloon (average particle diameter 90 to 120 μm) (floating carrier) 25.0 parts, alkylnaphthalenesulfonic acid Na 3.0 parts, alkylnaphthalenesulfonic acid formaldehyde condensate Na 3.0 parts, Carboxymethylcellulose Na 2.0 parts, pearlite 35.0 parts, clay 8.0 parts, granulation diameter 4.0 mm, sieves of 4.76 mm and 2.36 mm at the time of sieving were sieves, and in accordance with Example 1, a water-floating pesticide formulation was prepared. The particle size of the obtained formulation is 23% in the range of 2.80 to 1.70 mm (the remaining is 77% above 2.80 mm), the long/short diameter ratio at the bottom is 1.3, the number of particles per 1 g is 36, and is greater than 2.80 mm. A formulation with many particles was prepared.

[Comparative Example 4]

Formulation composition is gasgamycin 24.0 parts (sterilizing active ingredient), Shirasu balloon (average particle diameter 90 to 120 μm) (floating carrier) 25.0 parts, alkyl naphthalene sulfonic acid Na 3.0 parts, partially desulfonated lignin sulfonic acid Na 3.0 parts, carboxymethyl Cellulose Na 2.0 parts, pearlite 37.0 parts, clay 6.0 parts, granulation diameter 3.0 mm, without going through sizing in a drum sizing machine, drying in a state in a true circle in cross section to prepare a surface-floating pesticide formulation I did. The particle size of the obtained formulation was 83% in the range of 2.80 to 1.70 mm, the long diameter/short diameter ratio at the bottom was 1.0, and the number of particles per 1 g was 112.

[Comparative Example 5]

The formulation composition was gasgamycin 24.0 parts (sterilizing active ingredient), Shirasu balloon (average particle diameter 90 to 120 μm) (floating carrier) 25.0 parts, alkylnaphthalenesulfonic acid Na 3.0 parts, carboxymethylcellulose Na 2.0 parts, pearlite 38.0 parts, The clay was set to 8.0 parts and the granulation diameter was 3.0 mm, and in addition to the sizing in a drum sizing machine, the sizing was additionally dried in a plastic bag by tapping up and down to prepare a water-floating pesticide formulation. The particle size of the obtained formulation was 85% in the range of 2.80 to 1.70 mm, the long/short diameter ratio at the bottom was 1.6, and the number of particles per 1 g was 108.

[Comparative Example 6]

Formulation composition is gasgamycin 24.0 parts (sterilizing active ingredient), Shirasu balloon (average particle diameter 90 to 120 μm) (floating carrier) 25.0 parts, alkyl naphthalene sulfonic acid Na 3.0 parts, partially desulfonated lignin sulfonic acid Na 3.0 parts, carboxymethyl Cellulose Na 2.0 parts, pearlite 33.0 parts, clay 10.0 parts, granulation diameter 3.0 mm, in addition to sizing in a drum sizing machine, in addition to sizing in a drum sizing machine, additionally dry the sizing in a plastic bag by tapping it up and down, and floating on the water surface. A pesticide formulation was prepared. The particle size of the obtained formulation was 85% in the range of 2.80 to 1.70 mm, the long/short diameter ratio at the bottom was 1.8, and the number of particles per 1 g was 119.

[Comparative Example 7]

The formulation composition was gasgamycin 24.0 parts (sterilizing active ingredient), alkylnaphthalene sulfonic acid Na 3.0 parts, partially desulfonated lignin sulfonic acid Na 3.0 parts, carboxymethylcellulose Na 3.0 parts, pearlite 60.0 parts, clay 7.0 parts, granulation diameter 3.0 mm. , In accordance with Example 1, a surface-floating pesticide formulation was prepared. The particle size of the obtained formulation was 82% in the range of 2.80 to 1.70 mm, the long diameter/short diameter ratio at the bottom was 1.2, and the number of particles per 1 g was 103.

[Comparative Example 8]

The formulation composition was gasgamycin 24.0 parts (sterilizing active ingredient), alkylnaphthalene sulfonic acid Na 3.0 parts, partially desulfonated lignin sulfonic acid Na 3.0 parts, carboxymethylcellulose Na 3.0 parts, pearlite 18.0 parts, clay 49.0 parts, granulation diameter 3.0 mm. , In accordance with Example 1, a surface-floating pesticide formulation was prepared. The particle size of the obtained formulation was 86% in the range of 2.80 to 1.70 mm, the long/short diameter ratio at the bottom was 1.4, and the number of particles per 1 g was 43.

[Comparative Example 9]

Formulation composition is gasgamycin 24.0 parts (sterilizing active ingredient), Shirasu balloon (average particle diameter 90 to 120 μm) (floating carrier) 25.0 parts, partially desulfonated lignin sulfonic acid Na 3.0 parts, carboxymethylcellulose Na 3.0 parts, pearlite 39.0 Part, clay 6.0 parts, granulation diameter 3.0 mm, according to Example 1, to prepare a water-floating pesticide formulation. The particle size of the obtained formulation was 84% in the range of 2.80 to 1.70 mm, the long/short diameter ratio at the bottom was 1.2, and the number of particles per 1 g was 108.

[Comparative Example 10]

Formulation composition is gasgamycin 24.0 parts (sterilizing active ingredient), Shirasu balloon (average particle diameter 90 to 120 μm) (floating carrier) 25.0 parts, partially desulfonated lignin sulfonic acid Na 3.0 parts, alkyl sulfate Na 3.0 parts, carboxymethylcellulose With 3.0 parts of Na, 34.0 parts of pearlite, 8.0 parts of clay, and 3.0 mm of granulated diameter, a water-floating pesticide formulation was prepared in accordance with Example 1. The particle size of the obtained formulation was 83% in the range of 2.80 to 1.70 mm, the long/short diameter ratio at the bottom was 1.2, and the number of particles per 1 g was 98.

[Comparative Example 11]

Formulation composition is gasgamycin 24.0 parts (sterilizing active ingredient), Shirasu balloon (average particle diameter 90 to 120 μm) (floating carrier) 25.0 parts, partially desulfonated lignin sulfonic acid Na 3.0 parts, alkylbenzene sulfonic acid Na 3.0 parts, carboxymethyl With 2.0 parts of cellulose Na, 38.0 parts of pearlite, 5.0 parts of clay, and 3.0 mm of granulation diameter, a water-floating pesticide formulation was prepared in accordance with Example 1. The particle size of the obtained formulation was 85% in the range of 2.80 to 1.70 mm, the long/short diameter ratio at the bottom was 1.4, and the number of particles per 1 g was 100.

[Comparative Example 12]

Formulation composition is gasgamycin 24.0 parts (sterilizing 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 ether 3.0 parts , Carboxymethylcellulose Na 2.0 parts, pearlite 36.0 parts, clay 7.0 parts, granulation diameter 3.0 mm, according to Example 1, a water-floating pesticide formulation was prepared. The particle size of the obtained formulation was 86% in the range of 2.80 to 1.70 mm, the long diameter/short diameter ratio at the bottom was 1.3, and the number of particles per 1 g was 95.

[Comparative Example 13]

Formulation composition is gasgamycin 24.0 parts (sterilizing active ingredient), Shirasu balloon (average particle diameter 90 to 120 μm) (floating carrier) 25.0 parts, polyoxyethylene arylphenyl ether 3.0 parts, carboxymethylcellulose Na 3.0 parts, pearlite 39.0 Part, clay 6.0 parts, granulation diameter 3.0 mm, according to Example 1, to prepare a water-floating pesticide formulation. The particle size of the obtained formulation was 83% in the range of 2.80 to 1.70 mm, the long/short diameter ratio at the bottom was 1.2, and the number of particles per 1 g was 113.

[Comparative Example 14]

Formulation composition of pimetrozine 12.0 parts (insecticide active ingredient), Shirasu balloon (average particle diameter 90 to 120 μm) (floating carrier) 25.0 parts, alkyl naphthalene sulfonic acid Na 3.0 parts, carboxymethylcellulose Na 3.0 parts, pearlite 47.0 parts, 10.0 parts of clay, a granulation diameter of 3.0 mm, and sieves of 3.35 mm and 0.85 mm at the time of sieving were sieves, and a water-floating pesticide formulation was prepared in accordance with Example 18. The particle size of the obtained formulation is 65% in the range of 2.80 to 1.70 mm (the remainder is 35% below the particle size 1.70 mm), the long/short diameter ratio at the bottom is 1.2, the number of particles per 1 g is 195, and the particle size is 1.70. A formulation having many particles smaller than mm was prepared.

[Comparative Example 15]

Formulation composition of pimetrozine 12.0 parts (insecticide active ingredient), Shirasu balloon (average particle diameter 90 to 120 μm) (floating carrier) 25.0 parts, alkyl naphthalene sulfonic acid Na 3.0 parts, partially desulfonated lignin sulfonic acid Na 3.0 parts, carboxymethyl Cellulose Na 3.0 parts, pearlite 48.0 parts, clay 6.0 parts, granulation diameter 1.7 mm, sieve at the time of sieving were sieves of 2.00 mm and 0.85 mm, and according to Example 18, a water-floating pesticide formulation was prepared. The particle size of the obtained formulation is 1% in the range of 2.80 to 1.70 mm (the rest are 99% below the particle size 1.70 mm), the long/short diameter ratio at the bottom is 1.0, the number of particles per 1 g is 283, and 1.70 mm The following formulations having many small particles were prepared.

[Comparative Example 16]

The formulation composition was 12.0 parts of pymetrozine (insecticide active ingredient), Shirasu balloon (average particle diameter 90 to 120 μm) (floating carrier) 25.0 parts, alkylnaphthalenesulfonic acid Na 3.0 parts, alkylnaphthalenesulfonic acid formaldehyde condensate Na 3.0 parts, Carboxymethylcellulose Na 3.0 parts, pearlite 47.0 parts, clay 7.0 parts, granulation diameter 4.0 mm, sieves of 4.76 mm and 2.36 mm at the time of sieving were sieves, and in accordance with Example 18, a water-floating pesticide formulation was prepared. The particle size of the obtained formulation is 15% in the range of 2.80 to 1.70 mm (the remainder is 85% above 2.80 mm), the long/short diameter ratio at the bottom is 1.2, the number of particles per 1 g is 40, and is greater than 2.80 mm. A formulation with many particles was prepared.

[Comparative Example 17]

Formulation composition of pimetrozine 12.0 parts (insecticide active ingredient), Shirasu balloon (average particle diameter 90 to 120 μm) (floating carrier) 25.0 parts, alkyl naphthalene sulfonic acid Na 3.0 parts, partially desulfonated lignin sulfonic acid Na 3.0 parts, carboxymethyl With 3.0 parts of cellulose Na, 47.0 parts of pearlite, 7.0 parts of clay, and 3.0 mm of granulation diameter, drying was carried out in a state in which the cross section was in a true circle without going through the sizing in a drum sizing machine, and a surface floating pesticide formulation was prepared. The particle size of the obtained formulation was 86% in the range of 2.80 to 1.70 mm, the long/short diameter ratio at the bottom was 1.0, and the number of particles per 1 g was 105.

[Comparative Example 18]

Formulation composition of pimetrozine 12.0 parts (insecticide active ingredient), Shirasu balloon (average particle diameter 90 to 120 μm) (floating carrier) 25.0 parts, alkyl naphthalene sulfonic acid Na 3.0 parts, carboxymethylcellulose Na 3.0 parts, pearlite 51.0 parts, The clay was 6.0 parts and the granulation diameter was 3.0 mm, and in addition to the sizing in a drum sizing machine, the sizing was additionally dried in a plastic bag by tapping up and down to prepare a water-floating pesticide formulation. The particle size of the obtained formulation was 82% in the range of 2.80 to 1.70 mm, the long/short diameter ratio at the bottom was 1.6, and the number of particles per 1 g was 96.

[Comparative Example 19]

Formulation composition of pimetrozine 12.0 parts (insecticide active ingredient), Shirasu balloon (average particle diameter 90 to 120 μm) (floating carrier) 25.0 parts, alkyl naphthalene sulfonic acid Na 3.0 parts, partially desulfonated lignin sulfonic acid Na 3.0 parts, carboxymethyl Cellulose Na 3.0 parts, pearlite 47.0 parts, clay 7.0 parts, granulation diameter 3.0 mm, in addition to sizing in a drum sizing machine, in addition to sizing in a drum sizing machine, additionally drying the sizing in a plastic bag by tapping it up and down, and floating on water A pesticide formulation was prepared. The particle size of the obtained formulation was 84% in the range of 2.80 to 1.70 mm, the long/short diameter ratio at the bottom was 1.8, and the number of particles per 1 g was 108.

[Comparative Example 20]

The formulation composition was 12.0 parts of pymetrozine (insecticide active ingredient), 3.0 parts of alkylnaphthalenesulfonic acid Na, 3.0 parts of partially desulfonated ligninsulfonic acid Na, 3.0 parts of carboxymethylcellulose Na, 69.0 parts of pearlite, 10.0 parts of clay, and 3.0 mm in granulation diameter. , In accordance with Example 18, a surface-floating pesticide formulation was prepared. The particle size of the obtained formulation was 85% in the range of 2.80 to 1.70 mm, the long/short diameter ratio at the bottom was 1.2, and the number of particles per 1 g was 93.

[Comparative Example 21]

The formulation composition was 12.0 parts of pymetrozine (insecticide active ingredient), 3.0 parts of alkylnaphthalenesulfonic acid Na, 3.0 parts of partially desulfonated ligninsulfonic acid Na, 3.0 parts of carboxymethylcellulose Na, 21.0 parts of pearlite, 58.0 parts of clay, and 3.0 mm in granulation diameter. , In accordance with Example 18, a surface-floating pesticide formulation was prepared. The particle size of the obtained formulation was 85% in the range of 2.80 to 1.70 mm, the long/short diameter ratio at the bottom was 1.4, and the number of particles per 1 g was 38.

[Comparative Example 22]

Formulation composition of pimetrozine 12.0 parts (insecticide active ingredient), Shirasu balloon (average particle diameter 90 to 120 μm) (floating carrier) 25.0 parts, partially desulfonated lignin sulfonic acid Na 3.0 parts, carboxymethylcellulose Na 2.0 parts, pearlite 51.0 A part, 7.0 parts of clay, and a granulation diameter of 3.0 mm were used to prepare a water-floating pesticide formulation in accordance with Example 18. The particle size of the obtained formulation was 83% in the range of 2.80 to 1.70 mm, the long/short diameter ratio at the bottom was 1.2, and the number of particles per 1 g was 106.

[Comparative Example 23]

Formulation composition of pimetrozine 12.0 parts (insecticide active ingredient), Shirasu balloon (average particle diameter 90 to 120 μm) (floating carrier) 25.0 parts, partially desulfonated lignin sulfonic acid Na 3.0 parts, alkyl sulfate Na 3.0 parts, carboxymethylcellulose With 2.0 parts of Na, 48.0 parts of pearlite, 7.0 parts of clay, and 3.0 mm of granulated diameter, a water-floating pesticide formulation was prepared in accordance with Example 18. The particle size of the obtained formulation was 85% in the range of 2.80 to 1.70 mm, the long/short diameter ratio at the bottom was 1.4, and the number of particles per 1 g was 93.

[Comparative Example 24]

Formulation composition of pimetrozine 12.0 parts (insecticide active ingredient), Shirasu balloon (average particle diameter 90 to 120 μm) (floating carrier) 25.0 parts, partially desulfonated lignin sulfonic acid Na 3.0 parts, alkylbenzene sulfonic acid Na 3.0 parts, carboxymethyl With 2.0 parts of cellulose Na, 46.0 parts of pearlite, 9.0 parts of clay, and 3.0 mm of granulation diameter, a water-floating pesticide formulation was prepared in accordance with Example 18. The particle size of the obtained formulation was 84% in the range of 2.80 to 1.70 mm, the long/short diameter ratio at the bottom was 1.2, and the number of particles per 1 g was 95.

[Comparative Example 25]

Formulation composition of pimetrozine 12.0 parts (insecticide 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 ether 3.0 parts , Carboxymethylcellulose Na 3.0 parts, pearlite 50.0 parts, clay 4.0 parts, granulation diameter 3.0 mm, according to Example 18, to prepare a water-floating pesticide formulation. The particle size of the obtained formulation was 85% in the range of 2.80 to 1.70 mm, the long/short diameter ratio at the bottom was 1.4, and the number of particles per 1 g was 83.

[Comparative Example 26]

Formulation composition of pimetrozine 12.0 parts (insecticide active ingredient), Shirasu balloon (average particle diameter 90 to 120 μm) (floating carrier) 25.0 parts, polyoxyethylene arylphenyl ether 3.0 parts, carboxymethylcellulose Na 3.0 parts, pearlite 49.0 Part, clay 8.0 parts, granulation diameter 3.0 mm, according to Example 18, to prepare a water-floating pesticide formulation. The particle size of the obtained formulation was 86% in the range of 2.80 to 1.70 mm, the long diameter/short diameter ratio at the bottom was 1.1, and the number of particles per 1 g was 99.

[Comparative Example 27]

Formulation composition is 10.0 parts of iffencarbazone (herbicidal active ingredient), Shirasu balloon (average particle diameter 90-120 μm) (floating carrier) 25.0 parts, alkylnaphthalenesulfonic acid Na 3.0 parts, carboxymethylcellulose Na 2.0 parts, pearlite 52.0 parts , 8.0 parts of clay (the composition used in the slurry is 10.0 parts of iffencarbazone, 1.0 parts of alkylnaphthalenesulfonic acid Na, 14.0 parts of water), a granulation diameter of 3.0 mm, sieves of 3.35 mm and 0.85 mm for sifting, According to Example 35, a surface-floating pesticide formulation was prepared. The particle size of the obtained formulation is 68% in the range of 2.80 to 1.70 mm (the rest are 32% below the particle size 1.70 mm), the long/short diameter ratio at the bottom is 1.2, the number of particles per 1 g is 175, and the particle size is 1.70. A formulation having many particles smaller than mm was prepared.

[Comparative Example 28]

The formulation composition was 10.0 parts of iffencarbazone (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 lignin sulfonic acid Na 3.0 parts, carboxy Methylcellulose Na 2.0 parts, pearlite 48.0 parts, clay 9.0 parts (the composition used in the slurry is iffencarbazone 10.0 parts, alkylnaphthalene sulfonic acid Na 1.0 parts, water 14.0 parts), granulation diameter 1.7 mm, sieve when sifting Sieves of 2.00 mm and 0.85 mm were used, and a surface floating pesticide formulation was prepared in accordance with Example 35. The particle size of the obtained formulation is 10% in the range of 2.80 to 1.70 mm (the remainder is 90% below the particle size 1.70 mm), the long/short diameter ratio at the bottom is 1.0, the number of particles per 1 g is 354, and 1.70 mm. The following formulations having many small particles were prepared.

[Comparative Example 29]

Formulation composition is 10.0 parts of iffencarbazone (herbicidal active ingredient), Shirasu balloon (average particle diameter 90-120 μm) (floating carrier) 25.0 parts, alkylnaphthalenesulfonic acid Na 3.0 parts, alkylnaphthalenesulfonic acid formaldehyde condensate Na 3.0 parts , Carboxymethylcellulose Na 2.0 parts, pearlite 51.0 parts, clay 6.0 parts (the composition used in the slurry is 10.0 parts of iffencarbazone, alkylnaphthalene sulfonic acid Na 1.0 parts, water 14.0 parts), granulation diameter 4.0 mm, sieve The sieves were sieves of 4.76 mm and 2.36 mm, and a surface-floating pesticide formulation was prepared in accordance with Example 35. The particle size of the obtained formulation is 38% in the range of 2.80 to 1.70 mm (the rest are 62% above 2.80 mm), the long/short diameter ratio at the bottom is 1.2, the number of particles per 1 g is 41, and is larger than 2.80 mm. A formulation with many particles was prepared.

[Comparative Example 30]

The formulation composition was 10.0 parts of iffencarbazone (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 lignin sulfonic acid Na 3.0 parts, carboxy Methylcellulose Na 3.0 parts, pearlite 49.0 parts, clay 7.0 parts (the composition used in the slurry is 10.0 parts iffencarbazone, alkylnaphthalene sulfonic acid Na 1.0 parts, water 14.0 parts), a granulation diameter of 3.0 mm, and a drum sizing machine Drying was carried out in a state in which the cross section was in the shape of a true circle without going through the sizing in, and a surface-floating pesticide formulation was prepared. The particle size of the obtained formulation was 86% in the range of 2.80 to 1.70 mm, the long/short diameter ratio at the bottom was 1.0, and the number of particles per 1 g was 98.

[Comparative Example 31]

Formulation composition is 10.0 parts of iffencarbazone (herbicidal active ingredient), Shirasu balloon (average particle diameter 90 to 120 μm) (floating carrier) 25.0 parts, alkylnaphthalenesulfonic acid Na 3.0 parts, carboxymethylcellulose Na 3.0 parts, pearlite 52.0 parts , Clay 7.0 parts (the composition used in the slurry is 10.0 parts of iffencarbazone, 1.0 parts of alkylnaphthalenesulfonic acid Na, 14.0 parts of water), a granulation diameter of 3.0 mm, in addition to the sizing in a drum sizing machine, additionally After drying the sizing in a plastic bag as if tapping it up and down, a water-floating pesticide formulation was prepared. The particle size of the obtained formulation was 83% in the range of 2.80 to 1.70 mm, the long/short diameter ratio at the bottom was 1.6, and the number of particles per 1 g was 89.

[Comparative Example 32]

The formulation composition was 10.0 parts of iffencarbazone (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 lignin sulfonic acid Na 3.0 parts, carboxy Methylcellulose Na 3.0 parts, pearlite 49.0 parts, clay 7.0 parts (the composition used in the slurry is 10.0 parts iffencarbazone, alkylnaphthalene sulfonic acid Na 1.0 parts, water 14.0 parts), a granulation diameter of 3.0 mm, and a drum sizing machine In addition to the sizing in, the sizing was additionally dried in a plastic bag by tapping it up and down, and a surface-floating pesticide formulation was prepared. The particle size of the obtained formulation was 84% in the range of 2.80 to 1.70 mm, the long/short diameter ratio at the bottom was 1.8, and the number of particles per 1 g was 83.

[Comparative Example 33]

The formulation composition was 10.0 parts of iffencarbazone (herbicidal active ingredient), 3.0 parts of alkylnaphthalenesulfonic acid Na, 3.0 parts of partially desulfonated ligninsulfonic acid Na, 2.0 parts of carboxymethylcellulose Na, 65.0 parts of pearlite, 17.0 parts of clay (which was used in the slurry. The composition was 10.0 parts of iffencarbazone, 1.0 part of alkylnaphthalenesulfonic acid Na, 14.0 parts of water), and a granulation diameter of 3.0 mm, to prepare a water-floating pesticide formulation in accordance with Example 35. The particle size of the obtained formulation was 86% in the range of 2.80 to 1.70 mm, the long/short diameter ratio at the bottom was 1.3, and the number of particles per 1 g was 96.

[Comparative Example 34]

The formulation composition was 10.0 parts of iffencarbazone (herbicidal active ingredient), 3.0 parts of alkylnaphthalenesulfonic acid Na, 3.0 parts of partially desulfonated ligninsulfonic acid Na, 3.0 parts of carboxymethylcellulose Na, 30.0 parts of pearlite, 51.0 parts of clay (which was used in the slurry. The composition was 10.0 parts of iffencarbazone, 1.0 part of alkylnaphthalenesulfonic acid Na, 14.0 parts of water), and a granulation diameter of 3.0 mm, to prepare a water-floating pesticide formulation in accordance with Example 35. The particle size of the obtained formulation was 83% in the range of 2.80 to 1.70 mm, the long/short diameter ratio at the bottom was 1.4, and the number of particles per 1 g was 33.

[Comparative Example 35]

The formulation composition was 10.0 parts of iffencarbazone (herbicidal active ingredient), Shirasu balloon (average particle diameter 90 to 120 μm) (floating carrier) 25.0 parts, partially desulfonated lignin sulfonic acid Na 3.0 parts, carboxymethylcellulose Na 3.0 parts, pearlite 50.0 parts, clay 9.0 parts (the composition used in the slurry is 10.0 parts of iffencarbazone, 1.0 parts of partially desulfonated lignin sulfonic acid Na, 14.0 parts of water), a granulation diameter of 3.0 mm, and the water surface part according to Example 35 An oily pesticide formulation was prepared. The particle size of the obtained formulation was 83% in the range of 2.80 to 1.70 mm, the long diameter/short diameter ratio at the bottom was 1.2, and the number of particles per 1 g was 105.

[Comparative Example 36]

The formulation composition was 10.0 parts of iffencarbazone (herbicidal active ingredient), Shirasu balloon (average particle diameter 90 to 120 μm) (floating carrier) 25.0 parts, partially desulfonated lignin sulfonic acid Na 3.0 parts, alkyl sulfate Na 3.0 parts, carboxymethyl Cellulose Na 2.0 parts, pearlite 48.0 parts, clay 9.0 parts (the composition used in the slurry is 10.0 parts of iffencarbazone, 1.0 parts of partially desulfonated lignin sulfonic acid Na, 14.0 parts of water), a granulation diameter of 3.0 mm, Examples In accordance with 35, a surface-floating pesticide formulation was prepared. The particle size of the obtained formulation was 85% in the range of 2.80 to 1.70 mm, the long diameter/short diameter ratio at the bottom was 1.1, and the number of particles per 1 g was 90.

[Comparative Example 37]

Formulation composition is 10.0 parts of iffencarbazone (herbicidal active ingredient), Shirasu balloon (average particle diameter 90-120 μm) (floating carrier) 25.0 parts, partially desulfonated lignin sulfonic acid Na 3.0 parts, alkylbenzene sulfonic acid Na 3.0 parts, carboxy Methylcellulose Na 3.0 parts, pearlite 51.0 parts, clay 5.0 parts (the composition used in the slurry is 10.0 parts of iffencarbazone, 1.0 parts of partially desulfonated lignin sulfonic acid Na, 14.0 parts of water), and a granulation diameter of 3.0 mm. According to Example 35, a surface-floating pesticide formulation was prepared. The particle size of the obtained formulation was 82% in the range of 2.80 to 1.70 mm, the long/short diameter ratio at the bottom was 1.2, and the number of particles per 1 g was 110.

[Comparative Example 38]

Formulation composition is 10.0 parts of iffencarbazone (herbicidal active ingredient), Shirasu balloon (average particle diameter 90-120 μm) (floating carrier) 25.0 parts, alkylnaphthalenesulfonic acid formaldehyde condensate Na 3.0 parts, polyoxyethylene alkyl ether 3.0 Parts, carboxymethylcellulose Na 3.0 parts, pearlite 49.0 parts, clay 7.0 parts (the composition used in the slurry is 10.0 parts iffencarbazone, 1.0 parts polyoxyethylene alkyl ether, 14.0 parts water), and a granulation diameter of 3.0 mm , In accordance with Example 35, a surface-floating pesticide formulation was prepared. The particle size of the obtained formulation was 87% in the range of 2.80 to 1.70 mm, the long/short diameter ratio at the bottom was 1.2, and the number of particles per 1 g was 99.

[Comparative Example 39]

Formulation composition is 10.0 parts of iffencarbazone (herbicidal active ingredient), Shirasu balloon (average particle diameter 90 to 120 μm) (floating carrier) 25.0 parts, polyoxyethylene arylphenyl ether 3.0 parts, carboxymethylcellulose Na 2.0 parts, pearlite 54.0 parts, clay 6.0 parts (the composition used in the slurry is 10.0 parts of iffencarbazone, 1.0 parts of polyoxyethylene arylphenyl ether, 14.0 parts of water), and the granulation diameter is 3.0 mm, and according to Example 35, the water surface part An oily pesticide formulation was prepared. The particle size of the obtained formulation was 83% in the range of 2.80 to 1.70 mm, the long diameter/short diameter ratio at the bottom was 1.2, and the number of particles per 1 g was 86.

[Comparative Example 40]

The formulation composition was 12.0 parts of cymethrin (herbicidal active ingredient), Shirasu balloon (average particle diameter 90 to 120 μm) (floating carrier) 25.0 parts, alkylnaphthalenesulfonic acid Na 3.0 parts, carboxymethylcellulose Na 3.0 parts, pearlite 51.0 parts, Clay 6.0 parts, granulation diameter 3.0 mm, sieve at the time of sifting were 3.35 mm and 0.85 mm sieves, and the water-floating pesticide formulation was prepared in accordance with Example 52. The particle size of the obtained formulation is 55% in the range of 2.80 to 1.70 mm (the remainder is 45% below the particle size 1.70 mm), the long/short diameter ratio at the bottom is 1.4, the number of particles per 1 g is 203, and the particle size is 1.70. A formulation having many particles smaller than mm was prepared.

[Comparative Example 41]

The formulation composition was 12.0 parts of cymethrin (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 lignin sulfonic acid Na 3.0 parts, carboxymethyl Cellulose Na 2.0 parts, pearlite 47.0 parts, clay 8.0 parts, granulation diameter 1.7 mm, sieves at the time of sifting were sieves of 2.00 mm and 0.85 mm, and according to Example 52, a water-floating pesticide formulation was prepared. The particle size of the obtained formulation is 8% in the range of 2.80 to 1.70 mm (the rest are 92% below the particle size 1.70 mm), the long/short diameter ratio at the bottom is 1.0, the number of particles per 1 g is 236, and 1.70 mm. The following formulations having many small particles were prepared.

[Comparative Example 42]

The formulation composition was 12.0 parts of cymethrin (herbicidal active ingredient), Shirasu balloon (average particle diameter 90 to 120 μm) (floating carrier) 25.0 parts, alkylnaphthalenesulfonic acid Na 3.0 parts, alkylnaphthalenesulfonic acid formaldehyde condensate Na 3.0 parts, Carboxymethylcellulose Na 3.0 parts, pearlite 49.0 parts, clay 5.0 parts, granulation diameter 4.0 mm, sieves of 4.76 mm and 2.36 mm at the time of sieving were sieves, and in accordance with Example 52, a water-floating pesticide formulation was prepared. The particle size of the obtained formulation is 18% in the range of 2.80 to 1.70 mm (the remainder is 82% above 2.80 mm), the long/short diameter ratio at the bottom is 1.4, the number of particles per 1 g is 43, and is greater than 2.80 mm. A formulation with many particles was prepared.

[Comparative Example 43]

The formulation composition was 12.0 parts of cymethrin (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 lignin sulfonic acid Na 3.0 parts, carboxymethyl With 2.0 parts of cellulose Na, 49.0 parts of pearlite, 6.0 parts of clay, and 3.0 mm of granulation diameter, drying was performed in a state in which the cross section was in a true circle without going through the sizing in a drum sizing machine, and a surface floating pesticide formulation was prepared. The particle size of the obtained formulation was 85% in the range of 2.80 to 1.70 mm, the long/short diameter ratio at the bottom was 1.0, and the number of particles per 1 g was 90.

[Comparative Example 44]

The formulation composition was 12.0 parts of cymethrin (herbicidal active ingredient), Shirasu balloon (average particle diameter 90 to 120 μm) (floating carrier) 25.0 parts, alkylnaphthalenesulfonic acid Na 3.0 parts, carboxymethylcellulose Na 3.0 parts, pearlite 51.0 parts, The clay was 6.0 parts and the granulation diameter was 3.0 mm, and in addition to the sizing in a drum sizing machine, the sizing was additionally dried in a plastic bag by tapping up and down to prepare a water-floating pesticide formulation. The particle size of the obtained formulation was 83% in the range of 2.80 to 1.70 mm, the long diameter/short diameter ratio at the bottom was 1.6, and the number of particles per 1 g was 84.

[Comparative Example 45]

The formulation composition was 12.0 parts of cymethrin (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 lignin sulfonic acid Na 3.0 parts, carboxymethyl Cellulose Na 3.0 parts, pearlite 47.0 parts, clay 7.0 parts, granulation diameter 3.0 mm, in addition to sizing in a drum sizing machine, in addition to sizing in a drum sizing machine, additionally drying the sizing in a plastic bag by tapping it up and down, and floating on water A pesticide formulation was prepared. The particle size of the obtained formulation was 86% in the range of 2.80 to 1.70 mm, the long/short diameter ratio at the bottom was 1.8, and the number of particles per 1 g was 95.

[Comparative Example 46]

The formulation composition was made into 12.0 parts of cymethrin (herbicidal active ingredient), 3.0 parts of alkylnaphthalenesulfonic acid Na, 3.0 parts of partially desulfonated ligninsulfonic acid Na, 2.0 parts of carboxymethylcellulose Na, 68.0 parts of pearlite, 12.0 parts of clay, and 3.0 mm of granulation diameter. , In accordance with Example 52, a surface-floating pesticide formulation was prepared. The particle size of the obtained formulation was 83% in the range of 2.80 to 1.70 mm, the long diameter/short diameter ratio at the bottom was 1.1, and the number of particles per 1 g was 99.

[Comparative Example 47]

The formulation composition was made into 12.0 parts of cymethrin (herbicidal active ingredient), 3.0 parts of alkylnaphthalenesulfonic acid Na, 3.0 parts of partially desulfonated ligninsulfonic acid Na, 2.0 parts of carboxymethylcellulose Na, 25.0 parts of pearlite, 55.0 parts of clay, and 3.0 mm of granulation diameter. , In accordance with Example 52, a surface-floating pesticide formulation was prepared. The particle size of the obtained formulation was 82% in the range of 2.80 to 1.70 mm, the long/short diameter ratio at the bottom was 1.2, and the number of particles per 1 g was 31.

[Comparative Example 48]

Formulation composition was 12.0 parts of cymethrin (herbicidal active ingredient), Shirasu balloon (average particle diameter 90 to 120 μm) (floating carrier) 25.0 parts, partially desulfonated lignin sulfonic acid Na 3.0 parts, carboxymethylcellulose Na 3.0 parts, pearlite 49.0 A part, 8.0 parts of clay, and a granulation diameter of 3.0 mm were used to prepare a water-floating pesticide formulation in accordance with Example 52. The particle size of the obtained formulation was 86% in the range of 2.80 to 1.70 mm, the long/short diameter ratio at the bottom was 1.2, and the number of particles per 1 g was 98.

[Comparative Example 49]

Formulation composition was 12.0 parts of cymethrin (herbicidal active ingredient), Shirasu balloon (average particle diameter 90 to 120 μm) (floating carrier) 25.0 parts, partially desulfonated lignin sulfonic acid Na 3.0 parts, alkyl sulfate Na 3.0 parts, carboxymethylcellulose With 3.0 parts of Na, 48.0 parts of pearlite, 6.0 parts of clay, and 3.0 mm of granulated diameter, a water-floating pesticide formulation was prepared in accordance with Example 52. The particle size of the obtained formulation was 85% in the range of 2.80 to 1.70 mm, the long/short diameter ratio at the bottom was 1.4, and the number of particles per 1 g was 107.

[Comparative Example 50]

The formulation composition was 12.0 parts of cymethrin (herbicidal active ingredient), Shirasu balloon (average particle diameter 90 to 120 μm) (floating carrier) 25.0 parts, partially desulfonated lignin sulfonic acid Na 3.0 parts, alkylbenzene sulfonic acid Na 3.0 parts, carboxymethyl With 3.0 parts of cellulose Na, 48.0 parts of pearlite, 6.0 parts of clay, and 3.0 mm of granulation diameter, a water-floating pesticide formulation was prepared in accordance with Example 52. The particle size of the obtained formulation was 84% in the range of 2.80 to 1.70 mm, the long/short diameter ratio at the bottom was 1.2, and the number of particles per 1 g was 110.

[Comparative Example 51]

The formulation composition was 12.0 parts of cymethrin (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 ether 3.0 parts , Carboxymethylcellulose Na 2.0 parts, pearlite 47.0 parts, clay 8.0 parts, granulation diameter 3.0 mm, according to Example 52, to prepare a water-floating pesticide formulation. The particle size of the obtained formulation was 84% in the range of 2.80 to 1.70 mm, the long/short diameter ratio at the bottom was 1.3, and the number of particles per 1 g was 106.

[Comparative Example 52]

Formulation composition was 12.0 parts of cymethrin (herbicidal active ingredient), Shirasu balloon (average particle diameter 90 to 120 μm) (floating carrier) 25.0 parts, polyoxyethylene arylphenyl ether 3.0 parts, carboxymethylcellulose Na 2.0 parts, pearlite 50.0 A part, 8.0 parts of clay, and a granulation diameter of 3.0 mm were used to prepare a water-floating pesticide formulation in accordance with Example 52. The particle size of the obtained formulation was 85% in the range of 2.80 to 1.70 mm, the long diameter/short diameter ratio at the bottom was 1.2, and the number of particles per 1 g was 114.

[Comparative Example 53]

The formulation composition was 18.0 parts of benfurusate (herbicidal active ingredient), Shirasu balloon (average particle diameter 90-120 μm) (floating carrier) 25.0 parts, alkylnaphthalenesulfonic acid Na 3.0 parts, carboxymethylcellulose Na 2.0 parts, pearlite 46.0 parts, Clay 6.0 parts, granulation diameter 3.0 mm, sieves at the time of sifting were 3.35 mm and 0.85 mm sieves, according to Example 69, a water-floating pesticide formulation was prepared. The particle size of the obtained formulation is 63% in the range of 2.80 to 1.70 mm (the rest are 37% below the particle size 1.70 mm), the long/short diameter ratio at the bottom is 1.4, the number of particles per 1 g is 188, and the particle size is 1.70. A formulation having many particles smaller than mm was prepared.

[Comparative Example 54]

The formulation composition was 18.0 parts of benfurusate (herbicidal active ingredient), Shirasu balloon (average particle diameter 90 to 120 μm) (floating carrier) 25.0 parts, alkyl naphthalene sulfonic acid Na 3.0 parts, partially desulfonated lignin sulfonic acid Na 3.0 parts, carboxymethyl Cellulose Na 3.0 parts, pearlite 40.0 parts, clay 8.0 parts, granulation diameter 1.7 mm, sieve at the time of sieving was 2.00 mm and 0.85 mm sieve, according to Example 69, a water-floating pesticide formulation was prepared. The particle size of the obtained formulation is 5% in the range of 2.80 to 1.70 mm (the rest are 95% below the particle size 1.70 mm), the long/short diameter ratio at the bottom is 1.0, the number of particles per 1 g is 313, and 1.70 mm The following formulations having many small particles were prepared.

[Comparative Example 55]

The formulation composition was 18.0 parts of benfurusate (herbicidal active ingredient), Shirasu balloon (average particle diameter 90 to 120 μm) (floating carrier) 25.0 parts, alkylnaphthalenesulfonic acid Na 3.0 parts, alkylnaphthalenesulfonic acid formaldehyde condensate Na 3.0 parts, Carboxymethylcellulose Na 3.0 parts, pearlite 40.0 parts, clay 8.0 parts, granulation diameter 4.0 mm, sieves of 4.76 mm and 2.36 mm at the time of sieving were sieves, and in accordance with Example 69, a water-floating pesticide formulation was prepared. The particle size of the obtained formulation is 13% in the range of 2.80 to 1.70 mm (the rest are 87% above 2.80 mm), the long/short diameter ratio at the bottom is 1.2, the number of particles per 1 g is 39, and is larger than 2.80 mm. A formulation with many particles was prepared.

[Comparative Example 56]

The formulation composition was 18.0 parts of benfurusate (herbicidal active ingredient), Shirasu balloon (average particle diameter 90 to 120 μm) (floating carrier) 25.0 parts, alkyl naphthalene sulfonic acid Na 3.0 parts, partially desulfonated lignin sulfonic acid Na 3.0 parts, carboxymethyl With 3.0 parts of cellulose Na, 38.0 parts of pearlite, 10.0 parts of clay, and 3.0 mm of granulation diameter, drying was performed in a state in which the cross section was in a true circle without going through the sizing in a drum sizing machine, and a surface floating pesticide formulation was prepared. The particle size of the obtained formulation was 82% in the range of 2.80 to 1.70 mm, the long diameter/short diameter ratio at the bottom was 1.0, and the number of particles per 1 g was 108.

[Comparative Example 57]

The formulation composition was 18.0 parts of benfursate (herbicidal active ingredient), Shirasu balloon (average particle diameter 90 to 120 μm) (floating carrier) 25.0 parts, alkylnaphthalenesulfonic acid Na 3.0 parts, carboxymethylcellulose Na 2.0 parts, pearlite 45.0 parts, The clay was 7.0 parts and the granulation diameter was 3.0 mm, and in addition to the sizing in a drum sizing machine, the sizing was additionally dried in a plastic bag by tapping up and down to prepare a water-floating pesticide formulation. The particle size of the obtained formulation was 82% in the range of 2.80 to 1.70 mm, the long/short diameter ratio at the bottom was 1.6, and the number of particles per 1 g was 98.

[Comparative Example 58]

The formulation composition was 18.0 parts of benfurusate (herbicidal active ingredient), Shirasu balloon (average particle diameter 90 to 120 μm) (floating carrier) 25.0 parts, alkyl naphthalene sulfonic acid Na 3.0 parts, partially desulfonated lignin sulfonic acid Na 3.0 parts, carboxymethyl Cellulose Na 2.0 parts, pearlite 39.0 parts, clay 10.0 parts, granulation diameter 3.0 mm, in addition to sizing in a drum sizing machine, in addition to sizing in a plastic bag, dry the sizing up and down in a plastic bag, floating on the water surface A pesticide formulation was prepared. The particle size of the obtained formulation was 85% in the range of 2.80 to 1.70 mm, the long/short diameter ratio at the bottom was 1.8, and the number of particles per 1 g was 93.

[Comparative Example 59]

The formulation composition was made into 18.0 parts of benfursate (herbicidal active ingredient), 3.0 parts of alkylnaphthalenesulfonic acid Na, 3.0 parts of partially desulfonated ligninsulfonic acid Na, 2.0 parts of carboxymethylcellulose Na, 67.0 parts of pearlite, 7.0 parts of clay, and 3.0 mm of granulation diameter. , According to Example 69, a surface-floating pesticide formulation was prepared. The particle size of the obtained formulation was 84% in the range of 2.80 to 1.70 mm, the long/short diameter ratio at the bottom was 1.3, and the number of particles per 1 g was 102.

[Comparative Example 60]

The formulation composition was 18.0 parts of benfursate (herbicidal active ingredient), 3.0 parts of alkylnaphthalenesulfonic acid Na, 3.0 parts of partially desulfonated ligninsulfonic acid Na, 2.0 parts of carboxymethylcellulose Na, 19.0 parts of pearlite, 55.0 parts of clay, and 3.0 mm of granulated diameter. , According to Example 69, a surface-floating pesticide formulation was prepared. The particle size of the obtained formulation was 86% in the range of 2.80 to 1.70 mm, the long/short diameter ratio at the bottom was 1.1, and the number of particles per 1 g was 35.

[Comparative Example 61]

The formulation composition was 18.0 parts of benfursate (herbicidal active ingredient), Shirasu balloon (average particle diameter 90 to 120 μm) (floating carrier) 25.0 parts, partially desulfonated lignin sulfonic acid Na 3.0 parts, carboxymethylcellulose Na 3.0 parts, pearlite 42.0 A part, 9.0 parts of clay, and 3.0 mm of granulated diameter were used to prepare a water-floating pesticide formulation in accordance with Example 35. The particle size of the obtained formulation was 83% in the range of 2.80 to 1.70 mm, the long/short diameter ratio at the bottom was 1.2, and the number of particles per 1 g was 96.

[Comparative Example 62]

The formulation composition was 18.0 parts of benfurusate (herbicidal active ingredient), Shirasu balloon (average particle diameter 90 to 120 μm) (floating carrier) 25.0 parts, partially desulfonated lignin sulfonic acid Na 3.0 parts, alkyl sulfate Na 3.0 parts, carboxymethylcellulose With 3.0 parts of Na, 41.0 parts of pearlite, 7.0 parts of clay, and 3.0 mm of granulated diameter, a water-floating pesticide formulation was prepared in accordance with Example 69. The particle size of the obtained formulation was 85% in the range of 2.80 to 1.70 mm, the long/short diameter ratio at the bottom was 1.2, and the number of particles per 1 g was 93.

[Comparative Example 63]

The formulation composition was 18.0 parts of benfurusate (herbicidal active ingredient), Shirasu balloon (average particle diameter 90 to 120 μm) (floating carrier) 25.0 parts, partially desulfonated lignin sulfonic acid Na 3.0 parts, alkylbenzene sulfonic acid Na 3.0 parts, carboxymethyl With 2.0 parts of cellulose Na, 43.0 parts of pearlite, 6.0 parts of clay, and 3.0 mm of granulated diameter, a water-floating pesticide formulation was prepared in accordance with Example 69. The particle size of the obtained formulation was 84% in the range of 2.80 to 1.70 mm, the long diameter/short diameter ratio at the bottom was 1.1, and the number of particles per 1 g was 83.

[Comparative Example 64]

The formulation composition was 18.0 parts of benfurusate (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 ether 3.0 parts , Carboxymethylcellulose Na 2.0 parts, pearlite 42.0 parts, clay 7.0 parts, granulation diameter 3.0 mm, according to Example 69, to prepare a water-floating pesticide formulation. The particle size of the obtained formulation was 82% in the range of 2.80 to 1.70 mm, the long/short diameter ratio at the bottom was 1.3, and the number of particles per 1 g was 78.

[Comparative Example 65]

The formulation composition was 18.0 parts of benfurusate (herbicidal active ingredient), Shirasu balloon (average particle diameter 90 to 120 μm) (floating carrier) 25.0 parts, polyoxyethylene arylphenyl ether 3.0 parts, carboxymethylcellulose Na 3.0 parts, pearlite 43.0 Part, 8.0 parts of clay, and a granulation diameter of 3.0 mm were used to prepare a water-floating pesticide formulation in accordance with Example 69. The particle size of the obtained formulation was 83% in the range of 2.80 to 1.70 mm, the long/short diameter ratio at the bottom was 1.3, and the number of particles per 1 g was 88.

[Example 86]

Gasgamycin 24.0 parts (sterilization 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, propylene glycol 2.0 Parts, alkylnaphthalenesulfonic acid Na 2.5 parts, methylcellulose 3.0 parts, pearlite 25.0 parts, clay 8.5 parts were pulverized and mixed with a hammer mill (sample mill KIIW-1, Dalton company), and a powder mixture was obtained. The obtained powder mixture and 25.0 parts of a Shirasu balloon (average particle diameter of 70 to 90 μm) (floating carrier) were mixed for 10 minutes with a double arm kneader (KDHJ, Dalton, Inc.), followed by adding water and kneading for 15 minutes. Next, the kneaded water was assembled with an extrusion granulator equipped with a basket-type screen having a pore diameter of 3.0 mm. After pre-drying the obtained granulated product, it was sized with a drum type sizing machine, and dried with a fluid bed dryer. This was sieved to a size of 3.35 mm to 2.00 mm to obtain a surface-floating pesticide formulation. The particle size of the obtained formulation was 83% in the range of 2.80 to 1.70 mm, the long/short diameter ratio at the bottom was 1.2, and the number of particles per 1 g was 113.

[Example 87]

Formulation composition is gasgamycin 24.0 parts (sterilizing active ingredient), fly ash balloon (average particle diameter 80 to 120 μm) (floating carrier) 28.0 parts, polyoxyalkylene alkyl ether phosphate ester salt (alkylene group: carbon number 2, 3 , Alkyl group: n-octyl, ester bond number: 2, cation: Na ⁺ ) 4.0 parts, propylene glycol 2.0 parts, alkyl naphthalene sulfonic acid Na 2.5 parts, acrylic acid-vinylsulfonic acid copolymer Na 2.0 parts, dextrin 6.0 parts, white carbon 20.0 Parts, bentonite 11.5 parts, granulation diameter 2.8 mm, according to Example 86, to prepare a water-floating pesticide formulation. The particle size of the obtained formulation was 86% in the range of 2.80 to 1.70 mm, the long diameter/short diameter ratio at the bottom was 1.4, and the number of particles per 1 g was 103.

[Example 88]

The formulation composition is gasgamycin 24.0 parts (sterilizing active ingredient), ceramic balloon (average particle diameter 20 to 150 μm) (floating carrier) 25.0 parts, polyoxyalkylene alkyl ether phosphate ester salt (alkylene group: carbon number 2, 3, Alkyl group: 2-ethylhexyl, ester bond number: 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, methylcellulose 3.0 parts, pearlite 25.0 parts, With 11.0 parts of bentonite and 3.0 mm in granulated diameter, a water-floating pesticide formulation was prepared in accordance with Example 86. The particle size of the obtained formulation was 85% in the range of 2.80 to 1.70 mm, the long diameter/short diameter ratio at the bottom was 1.6, and the number of particles per 1 g was 175.

[Example 89]

Formulation composition is gasgamycin 24.0 parts (sterilizing active ingredient), acrylonitrile resin balloon (average particle diameter 20 to 40 μm) (floating carrier) 2.5 parts, polyoxyalkylene alkyl ether phosphate ester salt (alkylene group: carbon number 2 , 3, alkyl group: 2-ethylhexyl, ester bond number: 2, cation: Na ⁺ ) 12.0 parts, propylene glycol 3.0 parts, alkylnaphthalenesulfonic acid Na 2.5 parts, methylcellulose 3.0 parts, white carbon 30.0 parts, bentonite 23.0 parts, The granulation diameter was set to 3.0 mm, and a water-floating pesticide formulation was prepared in accordance with Example 86. The particle size of the obtained formulation was 83% in the range of 2.80 to 1.70 mm, the long diameter/short diameter ratio at the bottom was 1.5, and the number of particles per 1 g was 132.

[Example 90]

Formulation composition is gasgamycin 24.0 parts (sterilization active ingredient), ceramic balloon (average particle diameter 20 to 150 μm) (floating carrier) 25.0 parts, polyoxyalkylene alkyl ether phosphate ester salt (alkylene group: carbon number 2, 4, Alkyl group: n-decyl, ester bond number: 1, cation: H ⁺ ) 10.0 parts, propylene glycol 2.0 parts, dialkyl succinate sulfonic acid Na 2.5 parts, polyacrylic acid Na 2.0 parts, dextrin 6.0 parts, pearlite 20.0 parts, bentonite 8.5 Part and granulation diameter was made into 3.0 mm, and the water-floating pesticide formulation was prepared in conformity with Example 86. The particle size of the obtained formulation was 85% in the range of 2.80 to 1.70 mm, the long/short diameter ratio at the bottom was 1.3, and the number of particles per 1 g was 115.

[Example 91]

Formulation composition is gasgamycin 24.0 parts (sterilizing active ingredient), acrylonitrile resin balloon (average particle diameter 20 to 40 μm) (floating carrier) 2.5 parts, polyoxyalkylene alkyl ether phosphate ester salt (alkylene group: carbon number 2 , 3, alkyl group: n-decyl, ester bond number: 2, cation: H ⁺ ) 10.0 parts, propylene glycol 2.0 parts, alkyl naphthalene sulfonic acid Na 2.5 parts, acrylic acid-vinyl sulfonic acid copolymer Na 2.0 parts, dextrin 6.0 parts, white With 30.0 parts of carbon, 23.0 parts of bentonite, and 2.8 mm of granulated diameter, a water-floating pesticide formulation was prepared in accordance with Example 86. The particle size of the obtained formulation was 86% in the range of 2.80 to 1.70 mm, the long/short diameter ratio at the bottom was 1.4, and the number of particles per 1 g was 102.

[Example 92]

Formulation composition of gas gamycin 24.0 parts (sterilizing active ingredient), fly ash balloon (average particle diameter 80 to 120 μm) (floating carrier) 25.0 parts, polyoxyalkylene alkyl ether phosphate ester salt (alkylene group: carbon number 2, 3 , Alkyl group: isodecyl, ester bond number: 1, cation: K ⁺ ) 8.0 parts, butylene glycol 2.5 parts, dialkyl succinate sulfonic acid Na 2.5 parts, acrylic acid-vinylsulfonic acid copolymer Na 2.0 parts, dextrin 6.0 parts, pearlite It was 17.0 parts, clay 13.0 parts, and granulated diameter 3.0 mm, and according to Example 86, the water-floating pesticide formulation was prepared. The particle size of the obtained formulation was 82% in the range of 2.80 to 1.70 mm, the long/short diameter ratio at the bottom was 1.3, and the number of particles per 1 g was 59.

[Example 93]

Formulation composition is gasgamycin 24.0 parts (sterilizing active ingredient), Shirasu balloon (average particle diameter 70 to 90 μm) (floating carrier) 28.0 parts, polyoxyalkylene alkyl ether phosphate ester salt (alkylene group: carbon number 2, 3, 4, alkyl group: isodecyl, ester bond number: 2, cation: K ⁺ ) 10.0 parts, propylene glycol 2.0 parts, alkyl naphthalene sulfonic acid Na 2.5 parts, acrylic acid-vinyl sulfonic acid copolymer Na 2.0 parts, methylcellulose 3.0 parts, white carbon With 18.0 parts, bentonite 10.5 parts, and a granulation diameter of 2.8 mm, a water-floating pesticide formulation was prepared in accordance with Example 86. The particle size of the obtained formulation was 87% in the range of 2.80 to 1.70 mm, the long/short diameter ratio at the bottom was 1.1, and the number of particles per 1 g was 121.

[Example 94]

Formulation composition of gas gamycin 24.0 parts (sterilizing active ingredient), fly ash balloon (average particle diameter 80 to 120 μm) (floating carrier) 25.0 parts, polyoxyalkylene alkyl ether phosphate ester salt (alkylene group: carbon number 2, 3 , Alkyl group: 2-ethylhexyl, ester bond number: 1, cation: Na ⁺ ) 5.0 parts, polyoxyalkylene alkyl ether phosphate ester salt (alkylene group: carbon number 2, 3, alkyl group: 2-ethylhexyl, ester bond number : 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, methylcellulose 3.0 parts, diatomaceous earth 20.0 parts, clay 11.0 parts, granulation diameter 3.0 mm, according to Example 86, to prepare a water-floating pesticide formulation. The particle size of the obtained formulation was 82% in the range of 2.80 to 1.70 mm, the long/short diameter ratio at the bottom was 1.5, and the number of particles per 1 g was 135.

[Example 95]

Formulation composition of gasgamycin 24.0 parts (sterilizing active ingredient), Shirasu balloon (average particle diameter 70 to 90 μm) (floating carrier) 25.0 parts, polyoxyalkylene alkyl ether phosphate ester salt (alkylene group: carbon number 2, alkyl group: n-octyl, ester bond number: 1, cation: Na ⁺ ) 4.0 parts, polyoxyalkylene alkyl ether phosphate ester salt (alkylene group: carbon number 2 or 3, alkyl group: 2-ethylhexyl, ester bond number: 1, cation : Na ⁺ ) 4.0 parts, polyoxyalkylene alkyl ether phosphate ester salt (alkylene group: carbon number 2, 3, 4, alkyl group: isodecyl, ester bond number: 2, cation: K ⁺ ) 4.0 parts, propylene glycol 2.0 parts , Alkylnaphthalenesulfonic acid Na 2.5 parts, polyacrylic acid Na 3.0 parts, methylcellulose 3.0 parts, pearlite 20.0 parts, clay 8.5 parts, granulation diameter 3.0 mm, according to Example 86, to prepare a water-floating pesticide formulation. The particle size of the obtained formulation was 82% in the range of 2.80 to 1.70 mm, the long/short diameter ratio at the bottom was 1.3, and the number of particles per 1 g was 127.

[Example 96]

The formulation composition is gasgamycin 24.0 parts (sterilizing active ingredient), ceramic balloon (average particle diameter 20 to 150 μm) (floating carrier) 25.0 parts, polyoxyalkylene alkyl ether phosphate ester salt (alkylene group: carbon number 2, 3, 4, alkyl group: n-octyl, ester bond number: 2, cation: Na ⁺ ) 6.0 parts, polyoxyalkylene alkyl ether phosphate ester salt (alkylene group: carbon number 2, 3, alkyl group: 2-ethylhexyl, ester bond number : 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, dextrin 6.0 parts, pearlite 20.0 parts, bentonite 6.0 parts, granulation diameter 3.0 mm Then, in accordance with Example 86, a surface-floating pesticide formulation was prepared. The particle size of the obtained formulation was 94% in the range of 2.80 to 1.70 mm, the long diameter/short diameter ratio at the bottom was 1.2, and the number of particles per 1 g was 161.

[Example 97]

Formulation composition is gasgamycin 24.0 parts (sterilizing active ingredient), Shirasu balloon (average particle diameter 90 to 120 μm) (floating carrier) 28.0 parts, polyoxyalkylene alkyl ether phosphate ester salt (alkylene group: carbon number 2, 3, Alkyl group: n-decyl, ester bond number: 2, cation: H ⁺ ) 5.0 parts, polyoxyalkylene alkyl ether phosphate ester salt (alkylene group: carbon number 2 or 3, alkyl group: isodecyl, ester bond number: 1, cation : K ⁺ ) 5.0 parts, propylene glycol 1.5 parts, dialkyl succinate sulfonic acid Na 2.5 parts, polyacrylic acid Na 2.5 parts, methylcellulose 3.0 parts, diatomaceous earth 18.0 parts, bentonite 10.5 parts, granulation diameter 3.0 mm, Example 86 A water-floating pesticide formulation was prepared in accordance with the following. The particle size of the obtained formulation was 82% in the range of 2.80 to 1.70 mm, the long diameter/short diameter ratio at the bottom was 1.3, and the number of particles per 1 g was 115.

[Example 98]

Formulation composition of gas gamycin 24.0 parts (sterilizing active ingredient), Shirasu balloon (average particle diameter 90 to 120 μm) (floating carrier) 25.0 parts, polyoxyalkylene alkyl ether phosphate ester salt (alkylene group: carbon number 2, 4, Alkyl group: n-decyl, ester bond number: 1, cation: H ⁺ ) 8.0 parts, propylene glycol 2.0 parts, dialkyl succinate sulfonic acid Na 2.5 parts, acrylic acid-vinylsulfonic acid copolymer Na 2.0 parts, methylcellulose 3.0 parts, pearlite With 25.0 parts, bentonite 8.5 parts, and a granulation diameter of 2.8 mm, according to Example 86, a water-floating pesticide formulation was prepared. The particle size of the obtained formulation was 92% in the range of 2.80 to 1.70 mm, the long/short diameter ratio at the bottom was 1.4, and the number of particles per 1 g was 105.

[Example 99]

The formulation composition is gasgamycin 24.0 parts (sterilizing active ingredient), ceramic balloon (average particle diameter 20 to 150 μm) (floating carrier) 25.0 parts, polyoxyalkylene alkyl ether phosphate ester salt (alkylene group: carbon number 2, 3, Alkyl group: isodecyl, ester bond number: 1, cation: K ⁺ ) 4.0 parts, polyoxyalkylene alkyl ether phosphate ester salt (alkylene group: carbon number 2, 3, 4, alkyl group: isodecyl, ester bond number: 2, Cation: K ⁺ ) 4.0 parts, propylene glycol 2.5 parts, alkyl naphthalene sulfonic acid Na 2.5 parts, naphthalene sulfonic acid formaldehyde condensate Na 5.0 parts, polyacrylic acid Na 3.0 parts, dextrin 6.0 parts, diatomaceous earth 20.0 parts, clay 4.0 parts, granulation diameter It was set to 3.0 mm, and a water-floating pesticide formulation was prepared in accordance with Example 86. The particle size of the obtained formulation was 86% in the range of 2.80 to 1.70 mm, the long/short diameter ratio at the bottom was 1.2, and the number of particles per 1 g was 183.

[Example 100]

Formulation composition is gasgamycin 24.0 parts (sterilizing active ingredient), Shirasu balloon (average particle diameter 90 to 120 μm) (floating carrier) 28.0 parts, polyoxyalkylene alkyl ether phosphate ester salt (alkylene group: carbon number 2, 3, Alkyl group: isodecyl, ester bond number: 1, cation: K ⁺ ) 10.0 parts, propylene glycol 2.0 parts, alkyl naphthalene sulfonic acid Na 2.5 parts, alkyl naphthalene sulfonic acid formaldehyde condensate Na 3.0 parts, acrylic acid-maleic acid copolymer Na 2.0 parts , 6.0 parts of dextrin, 17.0 parts of pearlite, 5.5 parts of clay, and 3.0 mm of granulated diameter, according to Example 86, a water-floating pesticide formulation was prepared. The particle size of the obtained formulation was 94% in the range of 2.80 to 1.70 mm, the long/short diameter ratio at the bottom was 1.2, and the number of particles per 1 g was 127.

[Example 101]

The formulation composition is gasgamycin 24.0 parts (sterilizing active ingredient), ceramic balloon (average particle diameter 20 to 150 μm) (floating carrier) 25.0 parts, polyoxyalkylene alkyl ether phosphate ester salt (alkylene group: carbon number 2, 3, Alkyl group: n-octyl, ester bond number: 2, cation: Na ⁺ ) 6.0 parts, polyoxyalkylene alkyl ether phosphate ester salt (alkylene group: carbon number 2 or 3, alkyl group: n-decyl, ester bond number: 2, Cation: H ⁺ ) 6.0 parts, propylene glycol 2.5 parts, dialkyl succinate sulfonic 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, granulation diameter It was set to 2.8 mm, and a water-floating pesticide formulation was prepared in accordance with Example 86. The particle size of the obtained formulation was 82% in the range of 2.80 to 1.70 mm, the long/short diameter ratio at the bottom was 1.3, and the number of particles per 1 g was 118.

[Example 102]

Formulation composition is gasgamycin 24.0 parts (sterilizing active ingredient), Shirasu balloon (average particle diameter 90 to 120 μm) (floating carrier) 25.0 parts, polyoxyalkylene alkyl ether phosphate ester salt (alkylene group: carbon number 2, 3, Alkyl group: 2-ethylhexyl, ester bond number: 2, cation: Na ⁺ ) 4.0 parts, polyoxyalkylene alkyl ether phosphate ester salt (alkylene group: carbon number 2 or 4, alkyl group: n-decyl, ester bond number: 1 , Cations: H ⁺ ) 4.0 parts, propylene glycol 3.0 parts, lignin sulfonic acid Na 3.0 parts, polyacrylate Na 2.0 parts, polyvinyl alcohol 3.0 parts, pearlite 20.0 parts, clay 9.5 parts, granulation diameter 3.0 mm, Example 86 A water-floating pesticide formulation was prepared in accordance with the following. The particle size of the obtained formulation was 96% in the range of 2.80 to 1.70 mm, the long/short diameter ratio at the bottom was 1.3, and the number of particles per 1 g was 116.

[Example 103]

Formulation composition is gasgamycin 24.0 parts (sterilizing active ingredient), Shirasu balloon (average particle diameter 90 to 120 μm) (floating carrier) 25.0 parts, polyoxyalkylene alkyl ether phosphate ester salt (alkylene group: carbon number 2, 3, Alkyl group: n-octyl, ester bond number: 2, cation: Na ⁺ ) 5.0 parts, polyoxyalkylene alkyl ether phosphate ester salt (alkylene group: carbon number 2 or 3, alkyl group: n-decyl, ester bond number: 2, Cations: H ⁺ ) 5.0 parts, alkylnaphthalenesulfonic acid Na 2.5 parts, alkylnaphthalenesulfonic acid formaldehyde condensate Na 3.0 parts, polyacrylic acid Na 2.0 parts, carboxymethylcellulose Na 3.0 parts, diatomaceous earth 12.5 parts, bentonite 18.0 parts, granulation diameter 3.0 mm, according to Example 86, to prepare a water-floating pesticide formulation. The particle size of the obtained formulation was 94% in the range of 2.80 to 1.70 mm, the long/short diameter ratio at the bottom was 1.3, and the number of particles per 1 g was 61.

[Example 104]

Formulation composition is gasgamycin 24.0 parts (sterilizing active ingredient), Shirasu balloon (average particle diameter 90 to 120 μm) (floating carrier) 25.0 parts, propylene glycol 3.0 parts, alkyl naphthalene sulfonic acid Na 2.5 parts, naphthalene sulfonic 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, granulation diameter 3.0 mm, according to Example 86, a water-floating pesticide formulation was prepared. . The particle size of the obtained formulation was 92% in the range of 2.80 to 1.70 mm, the long/short diameter ratio at the bottom was 1.4, and the number of particles per 1 g was 105.

[Example 105]

Pymetrozine 12.0 parts (insecticide 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, propylene glycol 2.5 Parts, alkylnaphthalenesulfonic acid Na 2.5 parts, dextrin 6.0 parts, pearlite 27.0 parts, bentonite 15.0 parts were pulverized and mixed with a hammer mill (sample mill KIIW-1, Dalton Corporation) to obtain a powder mixture. The obtained powder mixture and 25.0 parts of a Shirasu balloon (average particle diameter of 70 to 90 μm) (floating carrier) were mixed for 10 minutes with a double arm kneader (KDHJ, Dalton, Inc.), followed by adding water and kneading for 15 minutes. Next, the kneaded water was assembled with an extrusion granulator equipped with a basket-type screen having a pore diameter of 2.8 mm. After pre-drying the obtained granulated product, it was sized with a drum-type sizer, and dried with a fluidized bed dryer. This was sieved to a size of 3.35 mm to 2.00 mm to obtain a surface-floating pesticide formulation. The particle size of the obtained formulation was 84% in the range of 2.80 to 1.70 mm, the long/short diameter ratio at the bottom was 1.2, and the number of particles per 1 g was 138.

[Example 106]

Formulation composition of pimetrozine 12.0 parts (insecticide active ingredient), fly ash balloon (average particle diameter 80 to 120 μm) (floating carrier) 25.0 parts, polyoxyalkylene alkyl ether phosphate ester salt (alkylene group: carbon number 2, 4 , Alkyl group: n-octyl, ester bond number: 2, cation: Na ⁺ ) 4.0 parts, propylene glycol 2.0 parts, dialkyl succinate sulfonic acid Na 2.5 parts, acrylic acid-vinylsulfonic acid copolymer Na 1.5 parts, dextrin 6.0 parts, diatomaceous earth With 28.0 parts, clay 19.0 parts, and a granulation diameter of 3.0 mm, in accordance with Example 105, a water-floating pesticide formulation was prepared. The particle size of the obtained formulation was 87% in the range of 2.80 to 1.70 mm, the long/short diameter ratio at the bottom was 1.4, and the number of particles per 1 g was 105.

[Example 107]

Formulation composition of pimetrozine 12.0 parts (insecticide active ingredient), fly ash balloon (average particle diameter 80 to 120 μm) (floating carrier) 30.0 parts, polyoxyalkylene alkyl ether phosphate ester salt (alkylene group: carbon number 2, 3 , Alkyl group: 2-ethylhexyl, ester bond number: 1, cation: Na ⁺ ) 6.0 parts, propylene glycol 2.0 parts, dialkyl succinate sulfonic acid Na 2.5 parts, acrylic acid-vinylsulfonic acid copolymer Na 2.0 parts, methylcellulose 3.0 parts , Diatomaceous earth 25, 0 parts, bentonite 17.5 parts, granulation diameter 3.0 mm, according to Example 105, to prepare a water-floating pesticide formulation. The particle size of the obtained formulation was 85% in the range of 2.80 to 1.70 mm, the long/short diameter ratio at the bottom was 1.2, and the number of particles per 1 g was 182.

[Example 108]

Formulation composition of pimetrozine 12.0 parts (insecticide active ingredient), fly ash balloon (average particle diameter 80 to 120 μm) (floating carrier) 30.0 parts, polyoxyalkylene alkyl ether phosphate ester salt (alkylene group: carbon number 2, alkyl group : 2-ethylhexyl, ester bond number: 2, cation: Na ⁺ ) 12.0 parts, hexylene glycol 2.5 parts, alkylnaphthalene sulfonic acid Na 2.5 parts, dextrin 7.0 parts, white carbon 17.0 parts, bentonite 17.0 parts, granulation diameter 3.0 mm And, in accordance with Example 105, a water-floating pesticide formulation was prepared. The particle size of the obtained formulation was 83% in the range of 2.80 to 1.70 mm, the long/short diameter ratio at the bottom was 1.4, and the number of particles per 1 g was 159.

[Example 109]

Formulation composition of pimetrozine 12.0 parts (insecticide active ingredient), ceramic balloon (average particle diameter 20 to 150 μm) (floating carrier) 25.0 parts, polyoxyalkylene alkyl ether phosphate ester salt (alkylene group: carbon number 2, alkyl group: n-decyl, ester bond number: 1, cation: H ⁺ ) 10.0 parts, propylene glycol 2.0 parts, alkyl naphthalene sulfonic acid Na 2.5 parts, acrylic acid-methacrylic acid copolymer Na 2.0 parts, methylcellulose 3.0 parts, pearlite 25.0 parts, The clay was 18.5 parts and the granulated diameter was 3.0 mm, and a water-floating pesticide formulation was prepared in accordance with Example 105. The particle size of the obtained formulation was 86% in the range of 2.80 to 1.70 mm, the long/short diameter ratio at the bottom was 1.3, and the number of particles per 1 g was 108.

[Example 110]

Formulation composition of pimetrozine 12.0 parts (insecticide active ingredient), acrylonitrile resin balloon (average particle diameter 20 to 40 μm) (floating carrier) 2.5 parts, polyoxyalkylene alkyl ether phosphate ester salt (alkylene group: carbon number 2) , 3, 4, alkyl group: n-decyl, ester bond number: 2, cation: H ⁺ ) 10.0 parts, propylene glycol 2.5 parts, dialkyl succinate sulfonic acid Na 2.5 parts, dextrin 6.0 parts, diatomaceous earth 35.0 parts, bentonite 29.5 parts , The granulation diameter was set to 3.0 mm, and a water-floating pesticide formulation was prepared in accordance with Example 105. The particle size of the obtained formulation was 85% in the range of 2.80 to 1.70 mm, the long/short diameter ratio at the bottom was 1.4, and the number of particles per 1 g was 125.

[Example 111]

Formulation composition of pimetrozine 12.0 parts (insecticide active ingredient), ceramic balloon (average particle diameter 20 to 150 μm) (floating carrier) 30.0 parts, polyoxyalkylene alkyl ether phosphate ester salt (alkylene group: carbon number 2, alkyl group: Isodecyl, ester bond number: 1, cation: K ⁺ ) 10.0 parts, propylene glycol 2.5 parts, alkyl naphthalene sulfonic acid Na 2.5 parts, acrylic acid-methacrylic acid copolymer Na 2.0 parts, methylcellulose 3.0 parts, white carbon 23.0 parts, With 15.0 parts of clay and 2.8 mm in granulation diameter, a water-floating pesticide formulation was prepared in accordance with Example 105. The particle size of the obtained formulation was 86% in the range of 2.80 to 1.70 mm, the long/short diameter ratio at the bottom was 1.1, and the number of particles per 1 g was 113.

[Example 112]

Formulation composition of pimetrozine 12.0 parts (insecticide active ingredient), Shirasu balloon (average particle diameter 70 to 90 μm) (floating carrier) 25.0 parts, polyoxyalkylene alkyl ether phosphate ester salt (alkylene group: carbon number 2, alkyl group: Isodecyl, ester bond number: 2, cation: K ⁺ ) 10.0 parts, propylene glycol 2.0 parts, dialkyl succinate sulfonic acid Na 2.5 parts, polyacrylic acid Na 1.0 parts, methylcellulose 3.0 parts, diatomaceous earth 25.0 parts, clay 19.5 parts, The granulation diameter was set to 3.0 mm, and a surface-floating pesticide formulation was prepared in accordance with Example 105. The particle size of the obtained formulation was 87% in the range of 2.80 to 1.70 mm, the long/short diameter ratio at the bottom was 1.2, and the number of particles per 1 g was 113.

[Example 113]

Formulation composition of pimetrozine 12.0 parts (insecticide active ingredient), fly ash balloon (average particle diameter 80 to 120 μm) (floating carrier) 25.0 parts, polyoxyalkylene alkyl ether phosphate ester salt (alkylene group: carbon number 2, 3 , Alkyl group: 2-ethylhexyl, ester bond number: 1, cation: Na ⁺ ) 5.0 parts, polyoxyalkylene alkyl ether phosphate ester salt (alkylene group: carbon number 2, alkyl group: 2-ethylhexyl, ester bond number: 2 , Cations: 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 parts, diatomaceous earth 25.0 parts, clay 17.0 parts, granulation diameter 3.0 mm Then, in accordance with Example 105, a surface-floating pesticide formulation was prepared. The particle size of the obtained formulation was 85% in the range of 2.80 to 1.70 mm, the long/short diameter ratio at the bottom was 1.1, and the number of particles per 1 g was 124.

[Example 114]

Formulation composition of pimetrozine 12.0 parts (insecticide active ingredient), ceramic balloon (average particle diameter 20 to 150 μm) (floating carrier) 30.0 parts, polyoxyalkylene alkyl ether phosphate ester salt (alkylene group: carbon number 2, alkyl group: n-octyl, ester bond number: 1, cation: Na ⁺ ) 4.0 parts, polyoxyalkylene alkyl ether phosphate ester salt (alkylene group: carbon number 2 or 3, alkyl group: 2-ethylhexyl, ester bond number: 1, cation : Na ⁺ ) 4.0 parts, propylene glycol 2.0 parts, alkyl naphthalene sulfonic acid Na 2.5 parts, acrylic acid-maleic acid copolymer Na 3.0 parts, methylcellulose 3.0 parts, white carbon 23.0 parts, bentonite 17.5 parts, granulation diameter 3.0 mm According to Example 105, a surface-floating pesticide formulation was prepared. The particle size of the obtained formulation was 83% in the range of 2.80 to 1.70 mm, the long/short diameter ratio at the bottom was 1.6, and the number of particles per 1 g was 105.

[Example 115]

Formulation composition of pimetrozine 12.0 parts (insecticide active ingredient), acrylonitrile resin balloon (average particle diameter 20 to 40 μm) (floating carrier) 2.5 parts, polyoxyalkylene alkyl ether phosphate ester salt (alkylene group: carbon number 2) , 4, alkyl group: n-octyl, ester bond number: 2, cation: Na ⁺ ) 6.0 parts, polyoxyalkylene alkyl ether phosphate ester salt (alkylene group: carbon number 2, 3, alkyl group: 2-ethylhexyl, ester bond Number: 1, Cation: Na ⁺ ) 6.0 parts, propylene glycol 3.0 parts, dialkyl succinate sulfonic acid Na 2.5 parts, acrylic acid-vinylsulfonic acid copolymer Na 1.5 parts, dextrin 6.0 parts, pearlite 30.0 parts, bentonite 30.5 parts, granulation diameter It was set to 2.8 mm, and a water-floating pesticide formulation was prepared in accordance with Example 105. The particle size of the obtained formulation was 94% in the range of 2.80 to 1.70 mm, the long diameter/short diameter ratio at the bottom was 1.2, and the number of particles per 1 g was 95.

[Example 116]

Formulation composition of pimetrozine 12.0 parts (insecticide active ingredient), Shirasu balloon (average particle diameter 90 to 120 μm) (floating carrier) 28.0 parts, polyoxyalkylene alkyl ether phosphate ester salt (alkylene group: carbon number 2, 3, 4, alkyl group: n-decyl, ester bond number: 2, cation: H ⁺ ) 10.0 parts, propylene glycol 1.5 parts, alkyl naphthalene sulfonic acid Na 2.5 parts, polyacrylic acid Na 2.0 parts, methylcellulose 3.0 parts, diatomaceous earth 22.0 parts, bentonite It was 19.0 parts and the granulation diameter was 3.0 mm, and the water-floating pesticide formulation was prepared in conformity with Example 105. The particle size of the obtained formulation was 83% in the range of 2.80 to 1.70 mm, the long/short diameter ratio at the bottom was 1.3, and the number of particles per 1 g was 93.

[Example 117]

Formulation composition of pimetrozine 12.0 parts (insecticide active ingredient), Shirasu balloon (average particle diameter 90 to 120 μm) (floating carrier) 28.0 parts, polyoxyalkylene alkyl ether phosphate ester salt (alkylene group: carbon number 2, 4, Alkyl group: n-octyl, ester bond number: 2, cation: Na ⁺ ) 4.0 parts, polyoxyalkylene alkyl ether phosphate ester salt (alkylene group: carbon number 2, alkyl group: 2-ethylhexyl, ester bond number: 2, cation : Na ⁺ ) 4.0 parts, propylene glycol 1.5 parts, dialkyl succinate sulfonic acid Na 2.5 parts, acrylic acid-vinyl sulfonic acid copolymer Na 2.0 parts, methylcellulose 3.0 parts, diatomaceous earth 22.0 parts, clay 21.0 parts, granulation diameter 3.0 mm , In accordance with Example 105, a surface-floating pesticide formulation was prepared. The particle size of the obtained formulation was 97% in the range of 2.80 to 1.70 mm, the long/short diameter ratio at the bottom was 1.2, and the number of particles per 1 g was 109.

[Example 118]

Formulation composition of pimetrozine 12.0 parts (insecticide active ingredient), ceramic balloon (average particle diameter 20 to 150 μm) (floating carrier) 25.0 parts, polyoxyalkylene alkyl ether phosphate ester salt (alkylene group: carbon number 2, 3, 4, alkyl group: n-decyl, ester bond number: 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 , 6.0 parts of dextrin, 25.0 parts of pearlite, 8.5 parts of bentonite, and 2.8 mm in granulation diameter, according to Example 105, a water-floating pesticide formulation was prepared. The particle size of the obtained formulation was 82% in the range of 2.80 to 1.70 mm, the long/short diameter ratio at the bottom was 1.1, and the number of particles per 1 g was 111.

[Example 119]

Formulation composition of pimetrozine 12.0 parts (insecticide active ingredient), Shirasu balloon (average particle diameter 90 to 120 μm) (floating carrier) 25.0 parts, polyoxyalkylene alkyl ether phosphate ester salt (alkylene group: carbon number 2, 3, Alkyl group: 2-ethylhexyl, ester bond number: 1, cation: Na ⁺ ) 5.0 parts, polyoxyalkylene alkyl ether phosphate ester salt (alkylene group: carbon number 2, alkyl group: n-decyl, ester bond number: 1, cation : H ⁺ ) 5.0 parts, propylene glycol 1.5 parts, alkyl naphthalene sulfonic acid Na 2.5 parts, naphthalene sulfonic acid formaldehyde condensate Na 3.0 parts, acrylic acid-methacrylic acid copolymer Na 2.5 parts, methylcellulose 3.0 parts, pearlite 25.0 parts, clay With 15.5 parts and a granulation diameter of 3.0 mm, a surface-floating pesticide formulation was prepared in accordance with Example 105. The particle size of the obtained formulation was 96% in the range of 2.80 to 1.70 mm, the long/short diameter ratio at the bottom was 1.1, and the number of particles per 1 g was 128.

[Example 120]

Formulation composition of pimetrozine 12.0 parts (insecticide active ingredient), Shirasu balloon (average particle diameter 70 to 90 μm) (floating carrier) 25.0 parts, polyoxyalkylene alkyl ether phosphate ester salt (alkylene group: carbon number 2, alkyl group: n-octyl, ester bond number: 1, cation: Na ⁺ ) 10.0 parts, propylene glycol 2.0 parts, dialkyl succinate sulfonic acid Na 2.5 parts, acrylic acid-vinylsulfonic acid copolymer Na 2.0 parts, carboxymethylcellulose Na 2.0 parts, white With 25.0 parts of carbon, 19.5 parts of bentonite, and 3.0 mm of granulated diameter, a water-floating pesticide formulation was prepared in accordance with Example 105. The particle size of the obtained formulation was 85% in the range of 2.80 to 1.70 mm, the long diameter/short diameter ratio at the bottom was 1.2, and the number of particles per 1 g was 110.

[Example 121]

Formulation composition of pimetrozine 12.0 parts (insecticide active ingredient), Shirasu balloon (average particle diameter 90 to 120 μm) (floating carrier) 25.0 parts, polyoxyalkylene alkyl ether phosphate ester salt (alkylene group: carbon number 2, 4, Alkyl group: n-octyl, ester bond number: 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, polyacrylic acid Na 2.0 parts, polyvinyl alcohol 2.0 parts, With 26.0 parts of pearlite, 15.5 parts of bentonite, and 2.8 mm in granulation diameter, a water-floating pesticide formulation was prepared in accordance with Example 105. The particle size of the obtained formulation was 97% in the range of 2.80 to 1.70 mm, the long/short diameter ratio at the bottom was 1.4, and the number of particles per 1 g was 119.

[Example 122]

Formulation composition of pimetrozine 12.0 parts (insecticide active ingredient), Shirasu balloon (average particle diameter 90 to 120 μm) (floating carrier) 25.0 parts, polyoxyalkylene alkyl ether phosphate ester salt (alkylene group: carbon number 2, 3, Alkyl group: 2-ethylhexyl, ester bond number: 1, cation: Na ⁺ ) 10.0 parts, alkylnaphthalenesulfonic acid Na 2.5 parts, alkylnaphthalenesulfonic acid formaldehyde condensate Na 2.5 parts, polyacrylic acid Na 2.0 parts, carboxymethylcellulose Na 3.0 Part, pearlite 23.0 parts, bentonite 15.0 parts, clay 5.0 parts, granulation diameter 3.0 mm, according to Example 105, to prepare a water-floating pesticide formulation. The particle size of the obtained formulation was 93% in the range of 2.80 to 1.70 mm, the long diameter/short diameter ratio at the bottom was 1.2, and the number of particles per 1 g was 102.

[Example 123]

Formulation composition of pimetrozine 12.0 parts (insecticide active ingredient), Shirasu balloon (average particle diameter 90 to 120 μm) (floating carrier) 25.0 parts, propylene glycol 3.0 parts, alkyl naphthalene sulfonic acid Na 2.5 parts, naphthalene sulfonic acid formaldehyde condensate Na 2.5 parts, acrylic acid-vinylsulfonic acid copolymer Na 3.0 parts, carboxymethylcellulose Na 3.0 parts, pearlite 26.0 parts, bentonite 10.0 parts, clay 13.0 parts, granulation diameter 3.0 mm, according to Example 105, water surface floating pesticide The formulation was prepared. The particle size of the obtained formulation was 91% in the range of 2.80 to 1.70 mm, the long/short diameter ratio at the bottom was 1.2, and the number of particles per 1 g was 79.

[Example 124]

After mixing 10.0 parts of iffencarbazone (herbicidal active ingredient), 1.0 parts of alkylnaphthalenesulfonic acid Na, and 14.0 parts of water, wet grinding in a Dino Mill (Shinmaru Enterprises) until the average particle diameter becomes 1.0 μm, and slurry Got it. In addition, polyoxyalkylene alkyl ether phosphate ester salt (alkylene group: carbon number 2 or 3, alkyl group: n-octyl, ester bond number: 1, cation: H ⁺ ) 8.0 parts, propylene glycol 2.0 parts, alkyl naphthalene sulfonic acid Na 1.5 Parts, 3.0 parts of methylcellulose, 29.0 parts of pearlite, and 17.5 parts of bentonite were pulverized and mixed with a hammer mill (sample mill KIIW-1, Dalton Corporation) to obtain a powder mixture. 28.0 parts of the slurry, powder mixture, and Shirasu balloon (average particle diameter of 70 to 90 μm) (floating carrier) were mixed for 10 minutes with a double arm kneader (KDHJ, Dalton Corporation), followed by adding water and kneading for 15 minutes. Next, the kneaded water was assembled with an extrusion granulator equipped with a basket-type screen having a pore diameter of 3.0 mm. After pre-drying the obtained granulated product, it was sized with a drum-type sizer, and dried with a fluidized bed dryer. This was sieved to a size of 3.35 mm to 2.00 mm to obtain a surface-floating pesticide formulation. The particle size of the obtained formulation was 83% in the range of 2.80 to 1.70 mm, the long/short diameter ratio at the bottom was 1.2, and the number of particles per 1 g was 132.

[Example 125]

Formulation composition is 10.0 parts of iffencarbazone (herbicidal active ingredient), ceramic balloon (average particle diameter 20 to 150 μm) (floating carrier) 25.0 parts, polyoxyalkylene alkyl ether phosphate ester salt (alkylene group: carbon number 2, 4 , Alkyl group: n-octyl, ester bond number: 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, 30.0 parts of pearlite, 19.0 parts of clay (the composition used in the slurry is 10.0 parts of iffencarbazone, 1.0 parts of dialkyl succinate sulfonic acid, 14.0 parts of water), a granulation diameter of 3.0 mm, and water surface according to Example 124 A floating pesticide formulation was prepared. The particle size of the obtained formulation was 86% in the range of 2.80 to 1.70 mm, the long diameter/short diameter ratio at the bottom was 1.3, and the number of particles per 1 g was 102.

[Example 126]

Formulation composition is 10.0 parts of iffencarbazone (herbicidal active ingredient), fly ash balloon (average particle diameter of 20 to 150 μm) (floating carrier) 30.0 parts, polyoxyalkylene alkyl ether phosphate ester salt (alkylene group: carbon number 2, 4, alkyl group: 2-ethylhexyl, ester bond number: 1, cation: Na ⁺ ) 6.0 parts, propylene glycol 3.0 parts, dialkyl succinate sulfonic acid Na 2.5 parts, acrylic acid-vinylsulfonic acid copolymer Na 2.0 parts, methylcellulose 3.0 Parts, pearlite 27.0 parts, clay 16.5 parts (the composition used in the slurry is 10.0 parts of iffencarbazone, 1.0 parts of dialkyl succinate sulfonic acid Na, 14.0 parts of water), a granulation diameter of 3.0 mm, according to Example 124 Thus, a surface-floating pesticide formulation was prepared. The particle size of the obtained formulation was 87% in the range of 2.80 to 1.70 mm, the long/short diameter ratio at the bottom was 1.4, and the number of particles per 1 g was 105.

[Example 127]

Formulation composition is 10.0 parts of iffencarbazone (herbicidal active ingredient), acrylonitrile resin balloon (average particle diameter of 20 to 40 μm) (floating carrier) 2.5 parts, polyoxyalkylene alkyl ether phosphate ester salt (alkylene group: carbon number) 2, alkyl group: 2-ethylhexyl, ester bond number: 2, cation: Na ⁺ ) 10.0 parts, propylene glycol 2.0 parts, alkyl naphthalene sulfonic acid Na 2.5 parts, acrylic acid-vinyl sulfonic acid copolymer Na 2.0 parts, methylcellulose 3.0 parts, Pearlite 40.0 parts, bentonite 30.0 parts (the composition used in the slurry was 10.0 parts of iffencarbazone, 1.0 parts of alkylnaphthalenesulfonic acid Na, 14.0 parts of water), the granulation diameter was 3.0 mm, and water surface floatability according to Example 124 A pesticide formulation was prepared. The particle size of the obtained formulation was 86% in the range of 2.80 to 1.70 mm, the long/short diameter ratio at the bottom was 1.2, and the number of particles per 1 g was 118.

[Example 128]

Formulation composition is 10.0 parts of iffencarbazone (herbicidal active ingredient), ceramic balloon (average particle diameter 20 to 150 μm) (floating carrier) 25.0 parts, polyoxyalkylene alkyl ether phosphate ester salt (alkylene group: carbon number 2, 4 , Alkyl group: n-decyl, ester bond number: 1, cation: Na ⁺ ) 8.0 parts, butylene glycol 2.0 parts, alkyl naphthalene sulfonic acid Na 2.5 parts, acrylic acid-maleic acid copolymer Na 2.0 parts, dextrin 6.0 parts, diatomaceous earth 26.0 parts , 18.5 parts of bentonite (the composition used in the slurry is 10.0 parts of iffencarbazone, 1.0 parts of alkylnaphthalenesulfonic acid Na, 14.0 parts of water), and a granulation diameter of 3.0 mm, according to Example 124, a water-floating pesticide formulation Prepared. The particle size of the obtained formulation was 84% in the range of 2.80 to 1.70 mm, the long/short diameter ratio 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 iffencarbazone (herbicidal active ingredient), fly ash balloon (average particle diameter 80 to 120 μm) (floating carrier) 30.0 parts, polyoxyalkylene alkyl ether phosphate ester salt (alkylene group: carbon number 2, 4, alkyl group: n-decyl, ester bond number: 2, cation: Na ⁺ ) 12.0 parts, propylene glycol 3.0 parts, alkyl naphthalene sulfonic acid Na 2.5 parts, methylcellulose 3.0 parts, diatomaceous earth 26.0 parts, clay 13.5 parts (in slurry The composition used for was 10.0 parts of iffencarbazone, 1.0 part of alkylnaphthalenesulfonic acid Na, 14.0 parts of water), and a granulation diameter of 3.0 mm, to prepare a water-floating pesticide formulation in accordance with Example 124. The particle size of the obtained formulation was 87% in the range of 2.80 to 1.70 mm, the long/short diameter ratio at the bottom was 1.5, and the number of particles per 1 g was 143.

[Example 130]

Formulation composition is 10.0 parts of iffencarbazone (herbicidal active ingredient), Shirasu balloon (average particle diameter of 70 to 90 μm) (floating carrier) 25.0 parts, polyoxyalkylene alkyl ether phosphate ester salt (alkylene group: carbon number 2, 3 , 4, alkyl group: isodecyl, ester bond number: 1, cation: K ⁺ ) 12.0 parts, propylene glycol 2.5 parts, dialkyl succinate sulfonic acid Na 2.5 parts, polyacrylic acid Na 2.0 parts, dextrin 6.0 parts, white carbon 25.0 parts , 15.0 parts of bentonite (the composition used in the slurry is 10.0 parts of iffencarbazone, 1.0 parts of dialkyl succinate sulfonic acid, 14.0 parts of water), a granulation diameter of 2.8 mm, and a surface-floating pesticide according to Example 124 The formulation was prepared. The particle size of the obtained formulation was 85% in the range of 2.80 to 1.70 mm, the long/short diameter ratio at the bottom was 1.3, and the number of particles per 1 g was 85.

[Example 131]

Formulation composition is 10.0 parts of iffencarbazone (herbicidal active ingredient), fly ash balloon (average particle diameter 80 to 120 μm) (floating carrier) 25.0 parts, polyoxyalkylene alkyl ether phosphate ester salt (alkylene group: carbon number 2, 4, alkyl group: isodecyl, ester bond number: 2, cation: K ⁺ ) 10.0 parts, propylene glycol 3.0 parts, alkyl naphthalene sulfonic acid Na 2.5 parts, acrylic acid-methacrylic acid copolymer Na 2.0 parts, dextrin 6.0 parts, diatomaceous earth 25.0 Parts, bentonite 16.5 parts (the composition used in the slurry is 10.0 parts of iffencarbazone, 1.0 parts of alkylnaphthalenesulfonic acid Na, 14.0 parts of water), a granulation diameter of 2.8 mm, and a surface-floating pesticide formulation in accordance with Example 124 Was prepared. The particle size of the obtained formulation was 84% in the range of 2.80 to 1.70 mm, the long/short diameter ratio at the bottom was 1.6, and the number of particles per 1 g was 180.

[Example 132]

Formulation composition is 10.0 parts of iffencarbazone (herbicidal active ingredient), Shirasu balloon (average particle diameter of 70 to 90 μm) (floating carrier) 25.0 parts, polyoxyalkylene alkyl ether phosphate ester salt (alkylene group: carbon number 2, 4 , Alkyl group: 2-ethylhexyl, ester bond number: 1, cation: Na ⁺ ) 6.0 parts, polyoxyalkylene alkyl ether phosphate ester salt (alkylene group: carbon number 2, alkyl group: 2-ethylhexyl, ester bond number: 2 , Cations: Na ⁺ ) 6.0 parts, propylene glycol 2.5 parts, alkylnaphthalenesulfonic acid Na 2.5 parts, acrylic acid-vinylsulfonic acid copolymer Na 2.0 parts, methylcellulose 3.0 parts, pearlite 25.0 parts, clay 18.0 parts (the composition used in the slurry Silver iffencarbazone 10.0 parts, alkylnaphthalenesulfonic acid Na 1.0 parts, water 14.0 parts), granulation diameter 3.0 mm, according to Example 124, a water-floating pesticide formulation was prepared. The particle size of the obtained formulation was 82% in the range of 2.80 to 1.70 mm, the long diameter/short diameter ratio at the bottom was 1.1, and the number of particles per 1 g was 103.

[Example 133]

Formulation composition is 10.0 parts of iffencarbazone (herbicidal active ingredient), ceramic balloon (average particle diameter of 20 to 150 μm) (floating carrier) 25.0 parts, polyoxyalkylene alkyl ether phosphate ester salt (alkylene group: carbon number 2, 3 , Alkyl group: n-octyl, ester bond number: 1, cation: H ⁺ ) 3.0 parts, polyoxyalkylene alkyl ether phosphate ester salt (alkylene group: carbon number 2, 4, alkyl group: 2-ethylhexyl, ester bond number: 1, cation: Na ⁺ ) 3.0 parts, polyoxyalkylene alkyl ether phosphate ester salt (alkylene group: carbon number 2, 4, alkyl group: isodecyl, ester bond number: 2, cation: K ⁺ ) 3.0 parts, propylene glycol 3.0 Parts, alkylnaphthalenesulfonic acid Na 2.5 parts, acrylic acid-methacrylic acid copolymer Na 2.5 parts, methylcellulose 3.0 parts, white carbon 25.0 parts, bentonite 20.0 parts (the composition used in the slurry is iffencarbazone 10.0 parts, alkyl naphthalene Sulfonic acid Na 1.0 part, water 14.0 parts), granulation diameter 3.0 mm, according to Example 124, the water surface floating pesticide preparation was prepared. The particle size of the obtained formulation was 82% in the range of 2.80 to 1.70 mm, the long/short diameter ratio at the bottom was 1.2, and the number of particles per 1 g was 93.

[Example 134]

Formulation composition is 10.0 parts of iffencarbazone (herbicidal active ingredient), ceramic balloon (average particle diameter 20 to 150 μm) (floating carrier) 25.0 parts, polyoxyalkylene alkyl ether phosphate ester salt (alkylene group: carbon number 2, 4 , Alkyl group: n-decyl, ester bond number: 1, cation: Na ⁺ ) 8.0 parts, polyoxyalkylene alkyl ether phosphate ester salt (alkylene group: carbon number 2, 4, alkyl group: n-decyl, ester bond number: 2 , Cations: Na ⁺ ) 4.0 parts, propylene glycol 2.0 parts, dialkyl succinate sulfonic acid Na 2.5 parts, polyacrylic acid Na 2.0 parts, dextrin 6.0 parts, pearlite 25.0 parts, clay 15.5 parts (the composition used in the slurry is ifpene 10.0 parts of carbazone, 1.0 part of dialkyl succinate sulfonic acid, 14.0 parts of water), and a granulation diameter of 2.8 mm, according to Example 124, a water-floating pesticide formulation was prepared. The particle size of the obtained formulation was 95% in the range of 2.80 to 1.70 mm, the long/short diameter ratio at the bottom was 1.3, and the number of particles per 1 g was 108.

[Example 135]

Formulation composition is 10.0 parts of iffencarbazone (herbicidal active ingredient), Shirasu balloon (average particle diameter 90-120 μm) (floating carrier) 25.0 parts, polyoxyalkylene alkyl ether phosphate ester salt (alkylene group: carbon number 2, 3 , 4, alkyl group: isodecyl, ester bond number: 1, cation: K ⁺ ) 10.0 parts, propylene glycol 2.0 parts, alkyl naphthalene sulfonic acid Na 2.5 parts, acrylic acid-maleic acid copolymer Na 2.0 parts, dextrin 6.0 parts, diatomaceous earth 25.0 parts , 17.5 parts of bentonite (the composition used in the slurry is 10.0 parts of iffencarbazone, 1.0 parts of alkylnaphthalenesulfonic acid Na, 14.0 parts of water), and a granulation diameter of 2.8 mm, according to Example 124, a water-floating pesticide formulation Prepared. The particle size of the obtained formulation was 86% in the range of 2.80 to 1.70 mm, the long/short diameter ratio at the bottom was 1.4, and the number of particles per 1 g was 117.

[Example 136]

Formulation composition of iffencarbazone 10.0 parts (herbicidal active ingredient), Shirasu balloon (average particle diameter 90 to 120 μm) (floating carrier) 30.0 parts, polyoxyalkylene alkyl ether phosphate ester salt (alkylene group: carbon number 2, 4 , Alkyl group: isodecyl, ester bond number: 2, cation: K ⁺ ) 8.0 parts, propylene glycol 2.0 parts, dialkyl succinate sulfonic acid Na 2.5 parts, polyacrylic acid Na 2.0 parts, dextrin 6.0 parts, pearlite 23.0 parts, clay 16.5 Part (the composition used in the slurry is 10.0 parts of iffencarbazone, 1.0 part of dialkyl succinate sulfonic acid, 14.0 parts of water), and a granulation diameter of 3.0 mm, according to Example 124, to prepare a water-floating pesticide formulation I did. The particle size of the obtained formulation was 96% in the range of 2.80 to 1.70 mm, the long/short diameter ratio at the bottom was 1.2, and the number of particles per 1 g was 116.

[Example 137]

Formulation composition is 10.0 parts of iffencarbazone (herbicidal active ingredient), ceramic balloon (average particle diameter 20 to 150 μm) (floating carrier) 25.0 parts, polyoxyalkylene alkyl ether phosphate ester salt (alkylene group: carbon number 2, alkyl group : 2-ethylhexyl, ester bond number: 2, cation: Na ⁺ ) 10.0 parts, propylene glycol 2.0 parts, alkylnaphthalenesulfonic acid Na 2.5 parts, alkylnaphthalenesulfonic acid formaldehyde condensate Na 3.0 parts, acrylic acid-vinylsulfonic acid copolymer Na 2.0 parts, methylcellulose 3.0 parts, pearlite 25.0 parts, bentonite 17.5 parts (the composition used in the slurry is 10.0 parts of iffencarbazone, 1.0 parts of alkylnaphthalenesulfonic acid Na, 14.0 parts of water), and a granulation diameter of 3.0 mm. According to Example 124, a surface-floating pesticide formulation was prepared. The particle size of the obtained formulation was 84% in the range of 2.80 to 1.70 mm, the long/short diameter ratio at the bottom was 1.1, and the number of particles per 1 g was 108.

[Example 138]

Formulation composition is 10.0 parts of iffencarbazone (herbicidal active ingredient), Shirasu balloon (average particle diameter 90-120 μm) (floating carrier) 25.0 parts, polyoxyalkylene alkyl ether phosphate ester salt (alkylene group: carbon number 2, 3 , Alkyl group: n-octyl, ester bond number: 1, cation: H ⁺ ) 6.0 parts, polyoxyalkylene alkyl ether phosphate ester salt (alkylene group: carbon number 2, 4, alkyl group: 2-ethylhexyl, ester bond number: 1, Cation: Na ⁺ ) 6.0 parts, propylene glycol 2.5 parts, alkyl naphthalene sulfonic acid Na 2.5 parts, naphthalene sulfonic acid formaldehyde condensate Na 3.0 parts, acrylic acid-methacrylic acid copolymer Na 2.5 parts, dextrin 6.0 parts, diatomaceous earth 25.0 parts , 11.5 parts of clay (the composition used in the slurry is 10.0 parts of iffencarbazone, 1.0 parts of alkylnaphthalenesulfonic acid Na, 14.0 parts of water), and a granulation diameter of 3.0 mm, according to Example 124, a water-floating pesticide formulation Prepared. The particle size of the obtained formulation was 95% in the range of 2.80 to 1.70 mm, the long diameter/short diameter ratio at the bottom was 1.3, and the number of particles per 1 g was 156.

[Example 139]

Formulation composition is 10.0 parts of iffencarbazone (herbicidal active ingredient), Shirasu balloon (average particle diameter of 70 to 90 μm) (floating carrier) 25.0 parts, polyoxyalkylene alkyl ether phosphate ester salt (alkylene group: carbon number 2, 4 , Alkyl group: 2-ethylhexyl, ester bond number: 1, cation: Na ⁺ ) 5.0 parts, polyoxyalkylene alkyl ether phosphate ester salt (alkylene group: carbon number 2, alkyl group: 2-ethylhexyl, ester bond number: 2 , Cations: Na ⁺ ) 5.0 parts, propylene glycol 2.5 parts, alkyl naphthalene sulfonic acid Na 2.5 parts, acrylic acid-vinyl sulfonic acid copolymer Na 2.0 parts, polyvinyl alcohol 3.0 parts, white carbon 25.0 parts, bentonite 20.0 parts (in the slurry The composition used was 10.0 parts of iffencarbazone, 1.0 part of alkylnaphthalenesulfonic acid Na, 14.0 parts of water), and a granulation diameter of 2.8 mm, to prepare a water-floating pesticide formulation in accordance with Example 124. The particle size of the obtained formulation was 83% in the range of 2.80 to 1.70 mm, the long/short diameter ratio at the bottom was 1.5, and the number of particles per 1 g was 178.

[Example 140]

Formulation composition is 10.0 parts of iffencarbazone (herbicidal active ingredient), Shirasu balloon (average particle diameter 90 to 120 μm) (floating carrier) 25.0 parts, polyoxyalkylene alkyl ether phosphate ester salt (alkylene group: carbon number 2, 4 , Alkyl group: n-decyl, ester bond number: 1, cation: Na ⁺ ) 7.0 parts, polyoxyalkylene alkyl ether phosphate ester salt (alkylene group: carbon number 2, 4, alkyl group: n-decyl, ester bond number: 2 , Cations: 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-maleic acid copolymer Na 1.5 parts, carboxymethylcellulose Na 2.0 parts, diatomaceous earth 25.0 parts, bentonite 18.5 parts (the composition used in the slurry is 10.0 parts of iffencarbazone, 1.0 part of dialkyl succinate sulfonic acid, 14.0 parts of water), a granulation diameter of 3.0 mm, and a water-floating pesticide formulation was prepared in accordance with Example 124. Prepared. The particle size of the obtained formulation was 95% in the range of 2.80 to 1.70 mm, the long/short diameter ratio at the bottom was 1.2, and the number of particles per 1 g was 125.

[Example 141]

Formulation composition is 10.0 parts of iffencarbazone (herbicidal active ingredient), Shirasu balloon (average particle diameter 90 to 120 μm) (floating carrier) 25.0 parts, polyoxyalkylene alkyl ether phosphate ester salt (alkylene group: carbon number 2, 4 , Alkyl group: 2-ethylhexyl, ester bond number: 1, cation: Na ⁺ ) 10.0 parts, dialkyl succinate sulfonic acid Na 2.5 parts, alkylnaphthalene sulfonic acid formaldehyde condensate Na 3.0 parts, acrylic acid-maleic acid copolymer Na 1.5 parts , Carboxymethylcellulose Na 3.0 parts, diatomaceous earth 22.0 parts, bentonite 23.0 parts (the composition used in the slurry is 10.0 parts iffencarbazone, dialkyl succinate sulfonic acid Na 1.0 parts, water 14.0 parts), and a granulation diameter of 3.0 mm , In accordance with Example 124, a surface-floating pesticide formulation was prepared. The particle size of the obtained formulation was 95% in the range of 2.80 to 1.70 mm, the long/short diameter ratio at the bottom was 1.3, and the number of particles per 1 g was 58.

[Example 142]

Formulation composition is 10.0 parts of iffencarbazone (herbicidal active ingredient), Shirasu balloon (average particle diameter 90 to 120 μm) (floating carrier) 25.0 parts, propylene glycol 2.5 parts, dialkyl succinate sulfonic acid Na 2.5 parts, alkyl naphthalene sulfonic acid Formaldehyde condensate Na 3.0 parts, acrylic acid-vinylsulfonic acid copolymer Na 2.0 parts, carboxymethylcellulose Na 3.0 parts, diatomaceous earth 35.0 parts, bentonite 17.0 parts (the composition used in the slurry is iffencarbazone 10.0 parts, dialkyl succinate) Nate sulfonic acid Na 1.0 part, water 14.0 parts), granulation diameter 3.0 mm, according to Example 124, the water surface floating pesticide preparation was prepared. The particle size of the obtained formulation was 91% in the range of 2.80 to 1.70 mm, the long/short diameter ratio at the bottom was 1.2, and the number of particles per 1 g was 112.

[Example 143]

After mixing 10.0 parts of iffencarbazone (herbicidal active ingredient), 1.0 parts of dialkyl succinate sulfonic acid, and 14.0 parts of water, wet grinding with a Dino Mill (Shinmaru Enterprises) until the average particle diameter is 1.0 μm. , To obtain a slurry. Further, 18.0 parts of benfurusate (herbicidal active ingredient), polyoxyalkylene alkyl ether phosphate ester salt (alkylene group: carbon number 2 or 3, alkyl group: n-octyl, ester bond number: 1, cation: Na ⁺ ) 12.0 parts , 2.5 parts of propylene glycol, 1.5 parts of dialkyl succinate sulfonic acid Na, 3.0 parts of methylcellulose, 18.0 parts of white carbon, and 9.0 parts of bentonite were pulverized and mixed with a hammer mill (Sample Mill KIIW-1, Dalton Corporation) to obtain a powder mixture. 25.0 parts of a slurry, a powder mixture, and a fly ash balloon (average particle diameter of 80 to 120 μm) (floating carrier) were mixed for 10 minutes with a double arm kneader (KDHJ, Dalton), followed by adding water and kneading for 15 minutes. Next, the kneaded water was assembled with an extrusion granulator equipped with a basket-type screen having a pore diameter of 3.0 mm. After pre-drying the obtained granulated product, it was sized with a drum-type sizer, and dried with a fluidized bed dryer. This was sieved to a size of 3.35 mm to 2.00 mm to obtain a surface-floating pesticide formulation. The particle size of the obtained formulation was 86% in the range of 2.80 to 1.70 mm, the long/short diameter ratio at the bottom was 1.1, and the number of particles per 1 g was 78.

[Example 144]

Formulation composition of iffencarbazone 10.0 parts (herbicidal active ingredient), benfurusate 18.0 parts (herbicidal active ingredient), Shirasu balloon (average particle diameter 70 to 90 μm) (floating carrier) 28.0 parts, polyoxyalkylene alkyl ether Phosphoric acid ester salt (alkylene group: carbon number 2, 3, 4, alkyl group: n-octyl, ester bond number: 2, cation: Na ⁺ ) 6.0 parts, hexylene glycol 2.0 parts, alkyl naphthalene sulfonic acid Na 2.5 parts, polyacrylic acid Na 2.0 parts, dextrin 6.0 parts, calcium silicate 15.0 parts, bentonite 10.5 parts (the composition used in the slurry is 10.0 parts of iffencarbazone, alkylnaphthalene sulfonic acid Na 1.0 parts, water 14.0 parts), and the granulation diameter is 2.8 mm. In accordance with Example 143, a surface-floating pesticide formulation was prepared. The particle size of the obtained formulation was 87% in the range of 2.80 to 1.70 mm, the long/short diameter ratio at the bottom was 1.3, and the number of particles per 1 g was 89.

[Example 145]

Formulation composition of iffencarbazone 10.0 parts (herbicidal active ingredient), benfurusate 18.0 parts (herbicidal active ingredient), ceramic balloon (average particle diameter 20 to 150 μm) (floating carrier) 28.0 parts, polyoxyalkylene alkyl ether Phosphoric acid ester salt (alkylene group: carbon number 2, 4, alkyl group: 2-ethylhexyl, ester bond number: 1, cation: K ⁺ ) 6.0 parts, propylene glycol 3.0 parts, alkyl naphthalene sulfonic acid Na 2.5 parts, acrylic acid-vinylsulfonic acid copolymer 1.5 parts of combined Na, 6.0 parts of dextrin, 18.0 parts of calcium silicate, 7.0 parts of clay (the composition used in the slurry is 10.0 parts of iffencarbazone, 1.0 parts of alkylnaphthalenesulfonic acid Na, 14.0 parts of water), and a granulation diameter of 2.8 mm , In accordance with Example 143, a water-floating pesticide formulation was prepared. The particle size of the obtained formulation was 83% in the range of 2.80 to 1.70 mm, the long/short diameter ratio at the bottom was 1.5, and the number of particles per 1 g was 96.

[Example 146]

Formulation composition of iffencarbazone 10.0 parts (herbicidal active ingredient), benfurusate 18.0 parts (herbicidal active ingredient), fly ash balloon (average particle diameter 80 to 120 μm) (floating carrier) 25.0 parts, polyoxyalkylene 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 sulfonic acid Na 2.5 parts, methylcellulose 3.0 parts , 18.0 parts of white carbon, 11.5 parts of bentonite (the composition used in the slurry is 10.0 parts of iffencarbazone, 1.0 parts of dialkyl succinate sulfonic acid Na, 14.0 parts of water), a granulation diameter of 3.0 mm, according to Example 143 Thus, a surface-floating pesticide formulation was prepared. The particle size of the obtained formulation was 85% in the range of 2.80 to 1.70 mm, the long diameter/short diameter ratio at the bottom was 1.3, and the number of particles per 1 g was 105.

[Example 147]

Formulation composition of iffencarbazone 10.0 parts (herbicidal active ingredient), benfurusate 18.0 parts (herbicidal active ingredient), ceramic balloon (average particle diameter 20 to 150 μm) (floating carrier) 28.0 parts, polyoxyalkylene alkyl ether Phosphoric acid ester salt (alkylene group: C2, 3, 4, alkyl group: n-decyl, ester bond number: 1, cation: Na ⁺ ) 10.0 parts, propylene glycol 2.0 parts, dialkyl succinate sulfonic acid Na 2.5 parts, acrylic acid- Vinylsulfonic acid copolymer Na 1.0 parts, methylcellulose 3.0 parts, white carbon 18.0 parts, bentonite 7.5 parts (the composition used in the slurry is iffencarbazone 10.0 parts, dialkyl succinate sulfonic acid Na 1.0 parts, water 14.0 parts), The granulation diameter was set to 3.0 mm, and a surface-floating pesticide formulation was prepared in accordance with Example 143. The particle size of the obtained formulation was 84% in the range of 2.80 to 1.70 mm, the long/short diameter ratio at the bottom was 1.4, and the number of particles per 1 g was 118.

[Example 148]

Formulation composition: 10.0 parts of iffencarbazone (herbicidal active ingredient), 18.0 parts of benfurusate (herbicidal active ingredient), Shirasu balloon (average particle diameter of 70 to 90 μm) (floating carrier) 25.0 parts, polyoxyalkylene alkyl ether Phosphoric acid ester salt (alkylene group: carbon number 2, 3, 4, alkyl group: n-decyl, ester bond number: 2, cation: Na ⁺ ) 12.0 parts, propylene glycol 2.5 parts, alkylnaphthalenesulfonic acid Na 2.5 parts, methylcellulose 3.0 parts , Calcium silicate 20.0 parts, clay 7.0 parts (the composition used in the slurry is 10.0 parts of iffencarbazone, 1.0 parts of alkylnaphthalenesulfonic acid Na, 14.0 parts of water), a granulation diameter of 3.0 mm, and water surface according to Example 143 A floating pesticide formulation was prepared. The particle size of the obtained formulation was 86% in the range of 2.80 to 1.70 mm, the long/short diameter ratio at the bottom was 1.2, and the number of particles per 1 g was 93.

[Example 149]

Formulation composition of iffencarbazone 10.0 parts (herbicidal active ingredient), benfurusate 18.0 parts (herbicidal active ingredient), fly ash balloon (average particle diameter 80 to 120 μm) (floating carrier) 25.0 parts, polyoxyalkylene alkyl Ether phosphate ester salt (alkylene group: carbon number 2, 3, 4, alkyl group: isodecyl, ester bond number: 1, cation: H ⁺ ) 12.0 parts, propylene glycol 3.0 parts, dialkyl succinate sulfonic acid Na 2.5 parts, acrylic acid- Maleic acid copolymer Na 2.0 parts, methylcellulose 3.0 parts, white carbon 18.0 parts, clay 6.5 parts (the composition used in the slurry is iffencarbazone 10.0 parts, dialkyl succinate sulfonic acid Na 1.0 parts, water 14.0 parts), granulated With a diameter of 3.0 mm, a water-floating pesticide formulation was prepared in accordance with Example 143. The particle size of the obtained formulation was 83% in the range of 2.80 to 1.70 mm, the long/short diameter ratio at the bottom was 1.3, and the number of particles per 1 g was 82.

[Example 150]

Formulation composition of iffencarbazone 10.0 parts (herbicidal active ingredient), benfurusate 18.0 parts (herbicidal active ingredient), acrylonitrile resin balloon (average particle diameter 20 to 40 μm) (floating carrier) 2.5 parts, polyoxyalkyl Rene alkyl ether phosphate ester salt (alkylene group: carbon number 2, 3, 4, alkyl group: isodecyl, ester bond number: 2, cation: H ⁺ ) 12.0 parts, propylene glycol 2.0 parts, alkyl naphthalene sulfonic 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 in the slurry is 10.0 parts iffencarbazone, alkyl naphthalene sulfonic acid Na 1.0 part, water 14.0 parts), granulation diameter It was set to 2.8 mm, and a water-floating pesticide formulation was prepared in accordance with Example 143. The particle size of the obtained formulation was 85% in the range of 2.80 to 1.70 mm, the long/short diameter ratio at the bottom was 1.4, and the number of particles per 1 g was 73.

[Example 151]

Formulation composition of iffencarbazone 10.0 parts (herbicidal active ingredient), benfurusate 18.0 parts (herbicidal active ingredient), ceramic balloon (average particle diameter 20 to 150 μm) (floating carrier) 25.0 parts, polyoxyalkylene alkyl ether Phosphoric acid ester salt (alkylene group: carbon number 2, 4, alkyl group: 2-ethylhexyl, ester bond number: 1, cation: K ⁺ ) 10.0 parts, polyoxyalkylene alkyl ether phosphate ester 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-vinylsulfonic acid copolymer Na 1.5 parts, methylcellulose 3.0 parts, white 18.0 parts of carbon, 8.0 parts of bentonite (the composition used in the slurry is 10.0 parts of iffencarbazone, 1.0 parts of dialkyl succinate sulfonic acid Na, 14.0 parts of water), a granulation diameter of 3.0 mm, and water surface according to Example 143 A floating pesticide formulation was prepared. The particle size of the obtained formulation was 84% in the range of 2.80 to 1.70 mm, the long/short diameter ratio at the bottom was 1.2, and the number of particles per 1 g was 75.

[Example 152]

Formulation composition of iffencarbazone 10.0 parts (herbicidal active ingredient), benfurusate 18.0 parts (herbicidal active ingredient), ceramic balloon (average particle diameter 20 to 150 μm) (floating carrier) 25.0 parts, polyoxyalkylene alkyl ether Phosphoric acid ester salt (alkylene group: carbon number 2, 3, alkyl group: n-octyl, ester bond number: 1, cation: Na ⁺ ) 3.0 parts, polyoxyalkylene alkyl ether phosphate ester salt (alkylene group: carbon number 2, 4, Alkyl group: 2-ethylhexyl, ester bond number: 1, cation: K ⁺ ) 3.0 parts, polyoxyalkylene alkyl ether phosphate ester salt (alkylene group: carbon number 2, 3, 4, alkyl group: isodecyl, ester bond number: 2, Cations: H ⁺ ) 3.0 parts, propylene glycol 3.0 parts, alkyl naphthalene sulfonic acid Na 2.5 parts, acrylic acid-maleic acid copolymer Na 1.0 parts, methylcellulose 3.0 parts, white carbon 18.0 parts, bentonite 10.5 parts (in which The composition was 10.0 parts of iffencarbazone, 1.0 part of alkylnaphthalenesulfonic acid Na, 14.0 parts of water), and a granulation diameter of 3.0 mm, to prepare a water-floating pesticide formulation in accordance with Example 143. The particle size of the obtained formulation was 82% in the range of 2.80 to 1.70 mm, the long/short diameter ratio at the bottom was 1.6, and the number of particles per 1 g was 78.

[Example 153]

Formulation composition of iffencarbazone 10.0 parts (herbicidal active ingredient), benfurusate 18.0 parts (herbicidal active ingredient), fly ash balloon (average particle diameter 80 to 120 μm) (floating carrier) 25.0 parts, polyoxyalkylene alkyl Ether phosphate ester salt (alkylene group: carbon number 2, 3, 4, alkyl group: n-octyl, ester bond number: 2, cation: Na ⁺ ) 10.0 parts, propylene glycol 1.5 parts, alkyl naphthalene sulfonic acid Na 2.5 parts, polyacrylic acid Na 2.0 parts, 6.0 parts of dextrin, 18.0 parts of white carbon, 7.0 parts of clay (the composition used in the slurry is 10.0 parts of iffencarbazone, 1.0 parts of alkylnaphthalenesulfonic acid Na, 14.0 parts of water), and a granulation diameter of 3.0 mm. In accordance with Example 143, a surface-floating pesticide formulation was prepared. The particle size of the obtained formulation was 93% in the range of 2.80 to 1.70 mm, the long/short diameter ratio at the bottom was 1.1, and the number of particles per 1 g was 83.

[Example 154]

Formulation composition of iffencarbazone 10.0 parts (herbicidal active ingredient), benfurusate 18.0 parts (herbicidal active ingredient), Shirasu balloon (average particle diameter 90 to 120 μm) (floating carrier) 28.0 parts, polyoxyalkylene alkyl ether Phosphoric acid ester salt (alkylene group: carbon number 2, 4, alkyl group: 2-ethylhexyl, ester bond number: 1, cation: K ⁺ ) 4.0 parts, polyoxyalkylene alkyl ether phosphate ester salt (alkylene group: carbon number 2, 3 , 4, alkyl group: n-decyl, ester bond number: 2, cation: Na ⁺ ) 6.0 parts, propylene glycol 1.5 parts, alkyl naphthalene sulfonic acid Na 2.5 parts, acrylic acid-vinyl sulfonic acid copolymer Na 2.0 parts, methylcellulose 3.0 parts, 18.0 parts of calcium silicate, 7.0 parts of bentonite (the composition used in the slurry is 10.0 parts of iffencarbazone, 1.0 parts of alkylnaphthalenesulfonic acid Na, 14.0 parts of water), a granulation diameter of 3.0 mm, and the water surface part according to Example 143 An oily pesticide formulation was prepared. The particle size of the obtained formulation was 83% in the range of 2.80 to 1.70 mm, the long diameter/short diameter ratio at the bottom was 1.2, and the number of particles per 1 g was 86.

[Example 155]

Formulation composition of iffencarbazone 10.0 parts (herbicidal active ingredient), benfurusate 18.0 parts (herbicidal active ingredient), Shirasu balloon (average particle diameter 90 to 120 μm) (floating carrier) 25.0 parts, polyoxyalkylene alkyl ether Phosphoric acid ester salt (alkylene group: carbon number 2, 3, alkyl group: n-octyl, ester bond number: 1, cation: Na ⁺ ) 5.0 parts, polyoxyalkylene alkyl ether phosphate ester salt (alkylene group: carbon number 2, 3, 4, alkyl group: n-decyl, ester bond number: 1, cation: Na ⁺ ) 2.5 parts, polyoxyalkylene alkyl ether phosphate ester salt (alkylene group: carbon number 2, 3, 4, alkyl group: isodecyl, ester bond number : 2, Cation: H ⁺ ) 2.5 parts, propylene glycol 2.0 parts, alkylnaphthalene sulfonic acid Na 2.5 parts, polyacrylic acid Na 2.5 parts, methylcellulose 3.0 parts, calcium silicate 18.0 parts, clay 9.0 parts (the composition used in the slurry is 10.0 parts of iffencarbazone, 1.0 part of alkylnaphthalenesulfonic acid, 14.0 parts of water), and a granulation diameter of 2.8 mm, according to Example 143, a water-floating pesticide formulation was prepared. The particle size of the obtained formulation was 95% in the range of 2.80 to 1.70 mm, the long/short diameter ratio at the bottom was 1.1, and the number of particles per 1 g was 85.

[Example 156]

Formulation composition: 10.0 parts of iffencarbazone (herbicidal active ingredient), 18.0 parts of benfurusate (herbicidal active ingredient), Shirasu balloon (average particle diameter of 70 to 90 μm) (floating carrier) 25.0 parts, polyoxyalkylene alkyl ether Phosphoric acid ester salt (alkylene group: C2, 4, alkyl group: 2-ethylhexyl, ester bond number: 1, cation: K ⁺ ) 10.0 parts, propylene glycol 2.5 parts, alkyl naphthalene sulfonic acid Na 2.5 parts, naphthalene sulfonic acid formaldehyde condensation Water Na 3.0 parts, acrylic acid-maleic acid copolymer Na 1.5 parts, methylcellulose 3.0 parts, white carbon 18.0 parts, bentonite 6.5 parts (the composition used in the slurry is iffencarbazone 10.0 parts, alkyl naphthalene sulfonic acid Na 1.0 part, water 14.0 parts) and a granulation diameter of 3.0 mm, according to Example 143, a water-floating pesticide formulation was prepared. The particle size of the obtained formulation was 86% in the range of 2.80 to 1.70 mm, the long/short diameter ratio at the bottom was 1.2, and the number of particles per 1 g was 93.

[Example 157]

Formulation composition of iffencarbazone 10.0 parts (herbicidal active ingredient), benfurusate 18.0 parts (herbicidal active ingredient), Shirasu balloon (average particle diameter 90 to 120 μm) (floating carrier) 25.0 parts, polyoxyalkylene alkyl ether Phosphoric acid ester salt (alkylene group: carbon number 2, 3, 4, alkyl group: n-octyl, ester bond number: 2, cation: Na ⁺ ) 8.0 parts, propylene glycol 3.0 parts, dialkyl succinate sulfonic acid Na 2.5 parts, alkyl naphthalene Sulfonic acid formaldehyde condensate Na 3.0 parts, acrylic acid-methacrylic acid copolymer Na 1.0 parts, methylcellulose 3.0 parts, white carbon 18.0 parts, bentonite 8.5 parts (the composition used in the slurry is iffencarbazone 10.0 parts, dialkyl Succinate sulfonic acid Na 1.0 part, water 14.0 parts), granulation diameter 3.0 mm, and according to Example 143, a water-floating pesticide formulation was prepared. The particle size of the obtained formulation was 94% in the range of 2.80 to 1.70 mm, the long diameter/short diameter ratio at the bottom was 1.3, and the number of particles per 1 g was 120.

[Example 158]

Formulation composition of iffencarbazone 10.0 parts (herbicidal active ingredient), benfurusate 18.0 parts (herbicidal active ingredient), fly ash balloon (average particle diameter 80 to 120 μm) (floating carrier) 25.0 parts, polyoxyalkylene alkyl Ether phosphate ester salt (alkylene group: C2, C3, 4, alkyl group: n-octyl, ester bond number: 2, cation: Na ⁺ ) 5.0 parts, polyoxyalkylene alkyl ether phosphate ester salt (alkylene group: C2) , 4, alkyl group: 2-ethylhexyl, ester bond number: 1, cation: K ⁺ ) 5.0 parts, propylene glycol 3.0 parts, alkyl naphthalene sulfonic acid Na 2.5 parts, acrylic acid-vinyl sulfonic acid copolymer Na 3.0 parts, polyvinyl alcohol 3.0 Parts, white carbon 18.0 parts, clay 7.5 parts (the composition used in the slurry was 10.0 parts of iffencarbazone, 1.0 parts of alkylnaphthalenesulfonic acid Na, 14.0 parts of water), and the granulation diameter was 3.0 mm, according to Example 143. A water-floating pesticide formulation was prepared. The particle size of the obtained formulation was 84% in the range of 2.80 to 1.70 mm, the long/short diameter ratio at the bottom was 1.2, and the number of particles per 1 g was 100.

[Example 159]

Formulation composition of iffencarbazone 10.0 parts (herbicidal active ingredient), benfurusate 18.0 parts (herbicidal active ingredient), Shirasu balloon (average particle diameter 90 to 120 μm) (floating carrier) 25.0 parts, polyoxyalkylene alkyl ether Phosphoric acid ester salt (alkylene group: carbon number 2, alkyl group: 2-ethylhexyl, ester bond number: 2, cation: K ⁺ ) 4.5 parts, polyoxyalkylene alkyl ether phosphate ester salt (alkylene group: carbon number 2, 3, 4 , Alkyl group: n-decyl, ester bond number: 1, cation Na ⁺ ) 4.5 parts, propylene glycol 2.0 parts, alkyl naphthalene sulfonic acid Na 2.5 parts, lignin sulfonic acid Na 3.0 parts, acrylic acid-methacrylic acid copolymer Na 2.0 parts, carboxy Methylcellulose Na 3.0 parts, white carbon 18.0 parts, bentonite 7.5 parts (the composition used in the slurry is iffencarbazone 10.0 parts, alkylnaphthalene sulfonic acid Na 1.0 parts, water 14.0 parts), granulation diameter 3.0 mm, Examples In accordance with 143, a surface-floating pesticide formulation was prepared. The particle size of the obtained formulation was 97% in the range of 2.80 to 1.70 mm, the long diameter/short diameter ratio at the bottom was 1.2, and the number of particles per 1 g was 90.

[Example 160]

Formulation composition of iffencarbazone 10.0 parts (herbicidal active ingredient), benfurusate 18.0 parts (herbicidal active ingredient), Shirasu balloon (average particle diameter 90 to 120 μm) (floating carrier) 25.0 parts, polyoxyalkylene alkyl ether Phosphoric acid ester salt (alkylene group: carbon number 2, 3, 4, alkyl group: n-decyl, ester bond number: 2, cation: Na ⁺ ) 10.0 parts, alkyl naphthalene sulfonic acid Na 2.5 parts, naphthalene sulfonic 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 (the composition used in the slurry is iffencarbazone 10.0 parts, alkylnaphthalenesulfonic acid Na 1.0 parts, water 14.0) Part), the granulation diameter was set to 3.0 mm, and a water-floating pesticide formulation was prepared in accordance with Example 143. The particle size of the obtained formulation was 93% in the range of 2.80 to 1.70 mm, the long/short diameter ratio at the bottom was 1.4, and the number of particles per 1 g was 102.

[Example 161]

Formulation composition of iffencarbazone 10.0 parts (herbicidal active ingredient), benfurusate 18.0 parts (herbicidal active ingredient), Shirasu balloon (average particle diameter 90 to 120 μm) (floating carrier) 25.0 parts, propylene glycol 3.0 parts, alkyl Naphthalenesulfonic acid Na 2.5 parts, naphthalenesulfonic acid formaldehyde condensate Na 3.0 parts, acrylic acid-methacrylic acid copolymer Na 2.0 parts, carboxymethylcellulose Na 3.0 parts, white carbon 21.5 parts, clay 12.0 parts (the composition used in the slurry is Iffencarbazone 10.0 parts, alkyl naphthalene sulfonic acid Na 1.0 part, water 14.0 parts), the granulation diameter was 3.0 mm, and the water-floating pesticide formulation was prepared in accordance with Example 143. The particle size of the obtained formulation was 95% in the range of 2.80 to 1.70 mm, the long diameter/short diameter ratio at the bottom was 1.3, and the number of particles per 1 g was 86.

Next, the usefulness of the sleep-floating pesticide formulation of the present invention is shown by test examples.

<Diffusivity test 1 (check diffusion in shallow water and gentle wind conditions)>

1 The faucet after rice transplantation is divided into wave plates so that the area of the division becomes 100 m2 (4 m × 25 m, fresh water depth 2 cm), and under conditions of 2 to 3 m/s in a fine wind, from one side of the 4 m side. 25 g of samples prepared according to Examples and Comparative Examples were treated, and the following three items were investigated.

(1) Distance to reach the longest formulation by naked eye 15 minutes after spraying

(2) Presence or absence of sediment at the spraying point 15 minutes after spraying

On the other hand, the sediment was evaluated according to the following standard table.

(3) Subsequently, after 48 hours of treatment, the spraying point of the test group was taken as the starting point, and 20 mL of water collected at 1 m intervals was collected, and the separately prepared 1 m 2 (1 m × 1 m, fresh water depth 2 cm) test group was described above. After 48 hours of uniformly spraying 0.25 g of a preparation sample, the concentration of the active ingredient in the collection solution was quantified by high performance liquid chromatography (HPLC) or gas chromatography (GC) (if a decomposition product was produced, the decomposition product was also quantified, and pesticides It is converted into active ingredient concentration and summed), and the diffusion rate (%) at each point was calculated by the following formula (2).

On the other hand, the maximum distance at the point where the diffusion rate was 90% or more was taken as the diffusion distance, and the diffusivity was evaluated. In addition, this test was conducted on the product immediately after preparation and the product stored at 40°C for 90 days (equivalent to storage at room temperature for 3 years).

<Diffusivity test 2 (confirmation of diffusion in shallow water and no wind conditions)>

1 partition by waveplate so that the area of the partition is 120 square meters (4 m × 30 m, fresh water depth 2 cm), under windless conditions, from one side of the 4 m side, 30 g of a sample prepared according to the example was treated, and the following 3 An investigation was conducted on the items.

(1) Distance to reach the longest formulation by naked eye 15 minutes after spraying

(2) Presence or absence of sediment at the spraying point 15 minutes after spraying

On the other hand, the sediment was evaluated according to the standard table.

(3) Subsequently, after 24 hours of treatment, the spraying point of the test group was taken as the starting point, and 20 mL of water collected at 1.5 m intervals was collected, and the separately prepared 1 m 2 (1 m × 1 m, fresh water depth 2 cm) test group was described above. After 24 hours of uniform spraying of 0.25 g of a preparation sample, the concentration of the active ingredient in the collection solution was quantified by high-performance liquid chromatography (HPLC) or gas chromatography (GC) (if a decomposition product is produced, the decomposition product is also quantified, and pesticides Converted to the active ingredient concentration and summed), and the diffusion rate (%) at each point was calculated by the above formula (2).

On the other hand, the maximum distance at the point where the diffusion rate was 90% or more was taken as the diffusion distance, and the diffusivity was evaluated. In addition, this test was conducted on the product immediately after preparation and the product stored at 40°C for 150 days (corresponding to storage at room temperature for 5 years).

As a result of the diffusivity test, it can be evaluated that a formulation having less sediment at the spraying point, a longer distance to reach the formulation, and extending a farther point at a diffusion rate of 90% or more can be evaluated as excellent in floatability and diffusivity.

The test results are shown in Tables 2-1 to 2-9 (Example) and Tables 3-1 to 3-5 (Comparative Example).

[Table 2-1]

[Table 2-2]

[Table 2-3]

[Table 2-4]

[Table 2-5]

[Table 2-6]

[Table 2-7]

[Table 2-8]

[Table 2-9]

[Table 3-1]

[Table 3-2]

[Table 3-3]

[Table 3-4]

[Table 3-5]

<Explanation of table>

(1) Diffusion test 1 (check diffusion in shallow water and gentle wind conditions)

The sediment was affected by the floating carrier, Na alkylnaphthalene sulfonic acid or Na dialkyl succinate sulfonic acid, particle size, the long/short diameter ratio of the bottom of the particles, and the number of particles per 1 g. In Tables 2-1 to 2-5, in Examples 1 to 85, which satisfy any of the requirements, the sediment, the arrival distance to the formulation, and the diffusion distance were in practically no problem ranges. On the other hand, in the comparative example in which any one component was excluded or replaced with a substitute product, the sediment at the time of preparation or after storage at 40°C for 90 days was a result of having a problem in practical terms.

On the other hand, for any of the examples, the formulation to which any one of the alkylnaphthalenesulfonic acid formaldehyde condensate Na, the naphthalenesulfonic acid formaldehyde condensate Na, or the partially desulfonated ligninsulfonic acid Na was added was obtained after 90 days at 40°C (sediment, The reduction in the distance to reach the formulation and the diffusion distance) was suppressed. In addition, the preparation containing carboxymethylcellulose Na as a binder has improved sediment and diffusion distance compared to the examples in which other binders are used. Comprehensive diffusivity is that the floating carrier is a Shirasu balloon having an average particle diameter of 90 to 120 μm, alkyl naphthalene sulfonic acid Na or dialkyl succinate sulfonic acid Na, and alkyl naphthalene sulfonic acid formaldehyde condensate Na, naphthalene sulfonic acid formaldehyde condensate Na, or Containing any one of partially desulfonated lignin sulfonic acid Na, containing carboxymethylcellulose Na 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 a long/short diameter ratio of 1.1 to the bottom of the particle 1.4, Examples 16, 17, 33, 34, 50, 51, 67, 68, 84, and 85 in which the number of particles per 1 g were 50 to 150 were the best including immediately after preparation and 90 days at 40°C.

From the above, in order to sufficiently exert the diffusibility of the sediment, the reach of the preparation, and the diffusion distance, not only immediately after preparation but also after long-term storage, the surface-floating pesticide preparation is a pesticide active ingredient, a floating carrier, Na alkylnaphthalenesulfonic acid or dialkyl succinate. Na ate sulfonic acid, a particle size of at least 80% by weight in the range of 2.80 mm to 1.70 mm, a long diameter/short diameter ratio of 1.1 to 1.4 at the bottom of the particle, and 50 to 150 particles per gram are effective means.In addition, a particle size In the range of 2.80 mm to 1.70 mm, at least 90% by weight, the floating carrier being a Shirasu balloon having an average particle diameter of 90 to 120 μm, alkylnaphthalene sulfonic acid formaldehyde condensate Na, naphthalene sulfonic acid formaldehyde condensate Na, or partial desulfurization It is a more effective means to contain any one of the fonned ligninsulfonic acid Na, and to contain carboxymethylcellulose Na as a binder.

(2) Diffusion test 2 (confirmation of diffusivity in shallow water and no wind conditions)

Examples 86 to 102, 105 to 121, 124 to 140, and 143 to 159 containing water-soluble alkylene glycols such as polyoxyalkylene alkyl ether phosphate salt and propylene glycol are examples 16 and 17 that do not contain the above components. , 33, 34, 50, 51, 67, 68, 84, 85, 103, 104, 122, 123, 141, 142, 160, 161 Sediment at the time of preparation and after 150 days at 40℃, distance to reach of the preparation, diffusion The result was that the distance was better and the diffusivity was further improved (Tables 2-1 to 2-9).

In addition, in the examples containing the polyoxyalkylene alkyl ether phosphate and propylene glycol, in particular, in the range of 2.80 mm to 1.70 mm, the particle size is 90% by weight or more, and the floating carrier has an average particle diameter of 90 to 120 μm. A formulation using a Shirasu balloon, a formulation in which any one of an alkyl naphthalene sulfonic acid formaldehyde condensate Na, a naphthalene sulfonic acid formaldehyde condensate Na, or a lignin sulfonic acid Na was added, and a formulation containing carboxymethylcellulose Na or polyvinyl alcohol as a binder The results were superior to the sediment at the time of preparation or storage at 40° C. for 150 days, the reach of the preparation, and the diffusion distance. Comprehensive diffusivity is that the floating carrier is a Shirasu balloon having an average particle diameter of 90 to 120 μm, alkyl naphthalene sulfonic acid Na or dialkyl succinate sulfonic acid Na, and alkyl naphthalene sulfonic acid formaldehyde condensate Na, naphthalene sulfonic acid formaldehyde condensate Na, or Containing any one of lignin sulfonic acid Na, containing carboxymethylcellulose Na or polyvinyl alcohol as a binder, a particle size of at least 90% by weight in the range of 2.80 mm to 1.70 mm, and the long/short diameter ratio of the bottom of the particle is 1.1 Examples 102, 121, 140, and 159 of ~1.6 were the best including immediately after preparation and 150 days at 40°C.

From the above, water-floating pesticide formulations are agrochemical active ingredients, floating carriers, polyoxyalkylene alkyl ether phosphoric acid in order to more effectively exert the diffusibility of sediment, formulation reach, and diffusion distance not only immediately after preparation, but also after long-term storage. Ester salt, and alkyl naphthalene sulfonic acid Na or dialkyl succinate sulfonic acid Na, particle size in the range of 2.80 mm to 1.70 mm, at least 80% by weight, the long/short diameter ratio of the bottom of the particle is 1.1 to 1.6, the number of particles per 1 g is 50 ~ 200 is an effective means, in addition, a particle size of at least 90% by weight in the range of 2.80 mm to 1.70 mm, a floating carrier being a Shirasu balloon having an average particle diameter of 90 to 120 μm, an alkylnaphthalenesulfonic acid formaldehyde condensate Na, naphthalene sulfonic acid formaldehyde condensate Na, or lignin sulfonic acid Na containing any one of, as a binder containing carboxymethyl cellulose Na or polyvinyl alcohol is a more effective means.

Claims (12)

a) a pesticide active ingredient, b) a hollow body as a floating carrier, and c) as an anionic surfactant, at least one selected from alkyl naphthalene sulfonic acid Na and dialkyl succinate sulfonic acid Na, Sleep floating pesticide formulations having the following characteristics:
d) The long/short diameter ratio of the bottom of the particle is 1.1 to 1.4,
e) a particle size of at least 80% by weight in the range of 2.80 mm to 1.70 mm, and
f) The number of particles per 1 g is 50 to 150. The method of claim 1,
e) The surface-floating pesticide formulation, characterized in that the particle size is at least 90% by weight in the range of 2.80 mm to 1.70 mm. The method according to claim 1 or 2,
A surface floating pesticide formulation, wherein the hollow body as the floating carrier is a Shirasu balloon having an average particle diameter of 90 to 120 μm. The method according to any one of claims 1 to 3,
In addition, as an anionic surfactant, a surface-suspending pesticide containing 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. Formulation. The method according to any one of claims 1 to 4,
Additionally, a water-floating agrochemical formulation, characterized in that it contains carboxymethylcellulose Na as a binder. a) a pesticide active ingredient, b) a hollow body as a floating carrier, c) a polyoxyalkylene alkyl ether phosphate salt represented by the following general formula (I) and a water-soluble alkylene glycol, and d) an anionic surfactant. A sleep-floating pesticide formulation comprising at least one selected from alkyl naphthalene sulfonic acid Na and dialkyl succinate sulfonic acid Na.
[Formula 1]

[Wherein, R represents a straight 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 p and q are p + q = 3 and p = 1 or 2 represents an integer, and M represents a hydrogen atom, an alkali metal atom, an ammonium group, or an organic ammonium group. On the other hand, when there are a plurality of R, A, and M, respectively, the types may be the same or different.] The method of claim 6,
Water-soluble alkylene glycol is propylene glycol, water-floating pesticide formulation. The sleep-floating pesticide formulation of claim 6 or 7 having the following characteristics.
e) The long/short diameter ratio of the bottom of the particle is 1.1 to 1.6,
f) a particle size of at least 80% by weight in the range of 2.80 mm to 1.70 mm, and
g) The number of particles per 1 g is 50 to 200. The method of claim 8,
f) The surface-floating pesticide formulation, characterized in that the particle size is at least 90% by weight in the range of 2.80 mm to 1.70 mm. The method according to any one of claims 6 to 9,
A surface floating pesticide formulation, wherein the hollow body as the floating carrier is a Shirasu balloon having an average particle diameter of 90 to 120 μm. The method according to any one of claims 6 to 10,
In addition, as an anionic surfactant, a surface-floating agrochemical formulation comprising at least one selected from alkyl naphthalene sulfonic acid formaldehyde condensate Na, naphthalene sulfonic acid formaldehyde condensate Na, and lignin sulfonic acid Na. The method according to any one of claims 6 to 11,
Additionally, a water-floating pesticide formulation comprising at least one selected from carboxymethylcellulose Na and polyvinyl alcohol as a binder.