JPS58124704A - Granular chemical for agricultural and disinfection use - Google Patents

Abstract

PURPOSE:To provide the titled chemical stable for a long period, and compatible with any kinds of carrier particles, by coating a granular carrier with a liquid composition obtained by adding a surface active agent to a binder comprising liquid mineral oil, plasticizer or a specific animal or vegetable oil or fat, and smearing the surface the carrier with powdery chemical for agricultural or disinfection use. CONSTITUTION:A liquid composition obtained by adding a surface active agent (e.g. polyoxyethylene nonylphenyl ether, etc.) to a binder comprising a liquid mineral oil (e.g. kerosine, machine oil, etc.), a plasticizer (e.g. dimethyl phthalate, triphenyl phosphate, etc.) or a semidrying or non-drying liquid animal or vegetable oil or fat (e.g. whale oil, castor oil, etc.) to the surface of inorganic or organic granules having particle diameter of 0.1-2.0mm. (e.g. igneous rock, plutonic rock, granular urea, etc.), and its surface is dusted with powdery chemical for agricultural and disinfection use to obtain the objective granular chemical for agricultural and disinfection use.

Description

DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a granular drug for agricultural epidemic prevention that can maintain stability for a long period of time without undergoing physical or chemical changes even during storage.

Recently, from the viewpoint of saving labor and preventing environmental pollution when applying agricultural chemicals for pest control, weed control, and fertilization,
Spraying equipment has been improved and enlarged, and spraying methods have ranged from manual spreading to aerial spraying using sprayers and aircraft. In this case, it is necessary to prevent drifting of the fine powder due to the powdering of the herbal medicine by spraying, to preserve the environment other than the surface where the main medicine is applied, and to avoid chemical damage to the growing crops.

As a dosage form that meets these objectives, granular medicines formed into granules are often used for agricultural epidemic prevention medicines. Compared to other dosage forms such as powders, wettable powders, emulsions, etc., this granular agent is applied with a relatively high concentration of active ingredients after dispersion, and is particularly sensitive to weather conditions after application. Water moves vertically and horizontally, or moves to physiologically active points along with physiological and ecological functions during growth and nutrient absorption of the plant itself, and takes the process of exerting its effects, so its effects last for a relatively long period of time. It is a drug type with long-lasting residual effects.

In this way, granules are used to treat various diseases, weeds, crops, and where they are applied, especially the relationship with soil moisture, the mechanism of action of the active ingredient of the agricultural chemical, the physicochemical properties, and the concentration of the active ingredient in the preparation. There are various granulation methods, but the following methods are currently used. The first method is a transfer granulation method using a granulator manufactured by Ehrlich or a granulator manufactured by Lodge 1. This involves kneading a predetermined amount of the active ingredient with a powder extender, binder, and disintegration aid with water or a mixed solution of water and a binder, and then granulating and molding the mixture into desired particles using the above-mentioned granulator. The second method is to use an extrusion molding machine, where the active ingredient is mixed with the same fillers and adjuvants as in the first method, and generally 0 to 20% water. In addition, knead to make a diameter of 0.5-1.7n (32-9m).
In this method, the material is extruded by pressing it against a metal plate with small holes, dried, and then passed through a crusher, and the particles are sieved to size. The third method is the coating method. This is a method in which the active ingredient is directly pulverized into a fine powder and then coated on the surface of sized mineral or vegetable granules with a liquid binder to form granules. . With these granulation methods, the particle size distribution is generally 0.1 to 2fi (150 to 90 mesh) based on the required distribution density per unit area of the ground surface during granulation.
Many of these have been put into practical use.

Looking at the method for manufacturing the above granules, in the first granulation method, when the purpose is to obtain fine particles with a particle size of about 2 or less, the particle size of the granules is uneven. In the second extrusion molding method, the particle size is uniform (manufacturing yield is 85 to 95%, resulting in poor yield).Furthermore, in these methods, water is relatively removed after granulation. This granulation method is not suitable if the active ingredient is easily chemically changed by water or tends to evaporate during drying.

In addition, in the third coating method, granular materials such as bentonite and diatomaceous earth that have porous absorption properties or disintegrate and swell in water, or materials that have relatively low water and oil absorption properties such as silica stone, volcanic lapilli, and marble; Alternatively, the active ingredient can be coated in the next step by using natural or synthetic oils or oily liquids such as water, kerosene, machine oil, animal and vegetable oils, etc., as a binder, as well as water suitable for the purpose. Manufactured in a variety of ways. Moreover, if we analyze the granules produced by this coating method from the viewpoint of economic evaluation, (111i material can be obtained in large quantities at low cost and with uniform quality. (2) It can be obtained with low energy during granulation. In other words, the time required for granulation is short, and the desired particle size can be obtained at a high yield without the need for a drying process. (3) During storage, the active ingredient of the granular drug begins to decompose and the coated powder is dissolved. No deterioration of physicochemical properties such as powdering or caking due to peeling.

(4) It requires less labor to disperse particles, does not produce physiologically active effects, and has the greatest economic effect.

As described above, granulation using the coating method has many advantages over the former two methods as a granular drug for agricultural epidemic prevention.
Since the liquid binder determines the quality of the drug, there are also drawbacks such as the need to select a binder depending on the type and nature of the base particles.

Therefore, as a result of intensive research with the aim of obtaining a coating liquid binder that can be universally used for any base grain, the present inventors have found that as a binder, liquid mineral oil, a plasticizer, semi-drying to non-drying When producing granular agricultural epidemic prevention chemicals using a coating method using a non-drying to semi-drying liquid made by adding surfactants to animal and vegetable oils and fats, it was discovered that granular chemicals compatible with any base grains could be produced. The invention has been completed.

The present invention uses inorganic or organic granules with a particle size of 0.1 to 2.0, a liquid mineral oil, a plasticizer, and one or more liquid semi-drying to non-drying animal and vegetable oils and fats, and a surfactant. This is a granular agent for agricultural epidemic prevention, in which the active ingredient of the powdered agricultural epidemic prevention agent is coated on the surface of a liquid substance containing .

The inorganic and organic granular substances used as the granular base used in the present invention include crushed stones such as igneous rock, high volcanic rock, aqueous rock, and marble rock, crushed granules of ceramic products such as ceramics and refractories, granular urea, inorganic salt granules, bagasse grains, Rice grains, tobacco waste grains, corn grains, soybean oil cake, etc. are crushed to a particle size of 0.1 to 2.0 using an appropriate crusher or granulator.
It is made to match the grain size of Tsuru.

The coating binder used in the present invention includes mineral oils such as kerosene, machine oil, spindle oil, cold oil, power generation oil, insulating oil, marine machine oil, and liquid paraffin, and plasticizers such as phthalates such as dibutyl phthalate, Examples of semi-drying to non-drying liquid animal and vegetable oils, such as phosphates such as triphenyl phosphate, include whale oil, castor oil, olive oil, peanut oil, tea oil, and rapeseed oil.

The surfactants added to the above binder include polyoxyethylene alkylaryl ether such as polyoxyethylene nonyl phenyl ether, sorbitan fatty acid ester,
Nonionic surfactants such as polyoxyethylene sorbicun fatty acid esters, anionic surfactants such as calcium dodecylbenzenesulfonate, cationic surfactants such as lymethylbenzylammonium chloride, cetyl amino acid acid These amphoteric surfactants can be used alone or in an appropriate mixture of two or more. The amount added is approximately 0.1% to 40% of the binder.
It is preferably 0.5 to 10%.

In order to produce the granular drug of the present invention, the above particle size is from 0.1 to
2.0 amount of inorganic or organic granules, liquid mineral oil, plasticizer, or liquid drying or non-drying animal or vegetable oil and fat with a surfactant added to the granules in an amount of about 0.5 to 40% , preferably 1 to 15%, so as to sufficiently coat the surface of the granules. Separately, a predetermined amount of an agricultural drug or an epidemic prevention drug is mixed with approximately the same amount of a carrier such as powder of clay, white carbon, diatomaceous earth, bentonite, kaolin, talc, etc., or mixed and pulverized, and the surface of the granules is Manufactured by coating. Furthermore, when the drug is a powder, the drug and carrier may be coated on the surface of the granules separately without being mixed in advance. It is also effective for oily substances containing surfactants, and can also be produced by making the ingredients into a liquid form at room temperature or heating them, absorbing the oil into base granules, and then coating with talc or the like.

As the agricultural and epidemic prevention chemicals used in the present invention, any known liquid or powdered chemicals can be used.

The agricultural epidemic prevention granular drug of the present invention obtained as described above already has a stable adhesive strength of the coating layer immediately after production,
Even during storage, its physicochemical properties do not undergo any chemical changes such as oxidation, and it can maintain stability for a long period of time.

Next, examples of the present invention will be shown.

Example 1 2.91 parts of machine oil, 0.045 parts of polyoxyethylene nonylphenyl ether, and 0.03 parts of polyoxyethylene dodecylbenzene ether were added to the surface of crushed stone with a particle size of 0.5 to 1.7 m (32 to 10 m). While stirring 0.015 parts of calcium dodecylbenzenesulfonate, oryzemate (3-allyloxy-
1,2-benziisothiazole-1,1-dioxide)
8B and 16 parts of a powder obtained by mixing and pulverizing 8 parts of clay were added to obtain 8% oryzemate granules.

Example 2 Crushed stone 8 with a particle size of 0.5 to 1.7 m (32 to 10 meso5)
To 9 parts, add 2.9111 parts of machine oil, 0.045 parts of polyoxyethylene nonylphenyl ether, 0.03 parts of polyoxyethylene dodecylbenzene ether, and 0 and 0 parts of calcium dodecylbenzenesulfonate with stirring. 8 parts of powder obtained by mixing and pulverizing 4 parts of clay and 4 parts of clay were added to the crushed stone grains subjected to the above treatment and coated to obtain 4% oryzemate granules.

Example 3 90 parts of sea sand with a particle size of 0.5 to 1.7 cm (32 to 10 m/L), 0.3 part of polyethyleneoxy (E, 0=5) dodecyl ether, and 1.7 parts of spindle oil was added with stirring, and then Marchette (2-chloro-2',
Add 5 parts of 6'-diethyl-N-butoxymethylacetanilide and then coat with 3 parts of white carbon to obtain Marge Eso 15% granules.

Example 4 89 parts of sea sand with a particle size of 0.5 to 1.7 fi (32 to 10 mesh), 2.5 parts of rapeseed oil, polyoxyethylene (E,
0.5 part of octylphenyl ether (04 mol) was added with stirring to wet the sea sand surface,
Mix and crush 4 parts of Improbylphenyl-N-methylcarbamate) and 4 parts of clay, coat the powder, and mix.
Obtain PC4% granules.

Example 5 10 parts of pyridafention (diethyloxophenylpyridazine ilkis horothioate), 7 parts of peanut oil, and 08 mol of polyoxyethylene (E) were added to 5 parts of natural silica with a particle size of 0.5 to 0.8. ) A heated melt of 0.5 parts of octylphenyl ether at about 50°C was added to absorb the oil, and after 0.046 days or less white carbon 2
The mixture was coated with powder to obtain 10% pyridafention granules for epidemic prevention.

Next, experiments and evaluations showing the superiority of the granules of the present invention over conventional granules will be described.

In the method of manufacturing granular drugs by coating method, granules produced using the coating binder of the present invention (product of the present invention), water-soluble coating binders such as polyvinyl alcohol, carboxymethyl cellulose, etc., which are conventionally used coating binders. Granules using an aqueous solution of a polymer compound as a coating binder (Control Example 1); Granules using a water-soluble aliphatic polyhydric alcohol such as ethylene glycol or polypropylene glycol as a coating binder (
Comparative Example 2), Granules using kerosene, machine oil (kerosene, lubricating oil) as a coating binder (Comparative Example 3), Granules using natural animal and vegetable oils, especially drying oils, as a coating binder (Comparative Example 4) ,
Granules using synthetic drying oil as coating binder (Control Example 5)
, raw material unit price, manufacturing energy, for granules using synthetic resin adhesive solution as coating binder (Control Example 6),
Looking at the evaluation of storage stability and biological effects, the following
As shown in the table.

Table 1 Economic overall ranking of each agglomerate (Note) Number of rankings when the best one from each evaluation aspect is taken as 1. Here, the term "powdery" in the storage stability section means that it is not observed immediately after manufacture. However, after a certain period of time, the binder undergoes changes such as hardening, resulting in partial hardening and shrinkage, exposing areas where the adhesive strength between the granule coating layer and the base grains is weakened. As a result, a phenomenon called powdering occurs. In contrast, the product of the present invention uses a non-drying coating bonding agent made of a saturated compound that can be expected to be stable for a long period of time, so the adhesive strength of the coating layer is already stable immediately after manufacturing, and even during storage. Its physicochemical properties are completely unaffected by chemical changes such as oxidation and can maintain stability for a long period of time. Furthermore, in the method using alkylene glycols in Comparative Example (2), the above-mentioned pressure is higher than that of the coated binder of the present invention, and there is a risk that the binder will disappear and turn into powder when the container is opened.

Control example (3) uses the same material as the product of the present invention, but it does not contain a surfactant, so it takes a long time to produce, especially the granulation time, and the particles in the target particle size range. The dosage of the product is also poor, and the time to develop biocuring after application is slow, resulting in poor overall effectiveness. In addition, control examples (41, (51) basically use a drying oil containing an unsaturated compound having an unsaturated bond in the binder raw material or a synthetic drying oil as a binder, so the coating layer deteriorates due to oxidation during storage. effect occurs and hence powdering occurs.

In addition, during the manufacturing process, an air drying or heat drying process is required, and the resulting granular drugs are not dissolved or dispersed in water or soil moisture, and their water insolubility prevents uniform dispersion of the drug after application. It also takes a long time for the effect to appear. Comparative example (6) is generally more expensive and more toxic than the others, and its adhesive strength requires a special process because it uses a hardening agent or is hardened by baking at high temperatures. Unless the weather resistance of the resin is carefully selected, there is a risk of producing incompetent granules that do not exhibit the effects of the active ingredients of agricultural epidemic prevention agents. Now, among these coating binders according to the above-mentioned groups, the following ones were selected to make eight granular pesticide Oryzemate granules.

Coating binder Inventive product Machine oil, viscosity, 5 cm Bose 97 parts polyoxyethylene (E, 04 mole addition) nonylphenyl ether
1.5 parts polyoxyethylene (E, On
=6) Dodecyl ether
1.0 parts Calcium dotesylbenzenesulfonate
0.5 part or more of the mixed liquid was used as the coating binder of the present invention.

The following was used as a coating binder for a control product of the present invention.

Control example 1 Polyvinyl alcohol (saponification degree 88 mol) 5
% aqueous solution control example 2 Polypyrene glycol control example 3fi machine oil (viscosity path, 5 centipause 50°
) Control example 4 Linseed oil control example 5 Varnish control example 6 Urea resin (65% solids) [Manufacturing method] Particle size 0.5-1.7 (32-IO mesh)
Add 3 parts of the above-mentioned coating binder to 85 parts of crushed mineral stone using a flat stirrer while stirring, and after soaking the whole with the coating binder, 16 parts of milled flour, which was prepared by mixing and pulverizing % oryzemate % and clay %, were mixed into powder. Manufactured by coating.

However, magnetic 1°N1 other than magnetic 2 and -3 of the present invention product and control product
4. m5 and chen 6 were made by air drying for more than one night.

The thus produced Orizume 18% granules for rice fever control 0.
The yield of a product having a particle size of 5 to 1.7 m (32 to IO m), the degree of desorption in water of the product, the decomposition rate and powdering rate of the active ingredient after storage under heating and abuse were measured by the following methods.

B. Accurately weigh 20g of the underwater desorption sample and add it to a 250m graduated cylinder with a stopper containing 200mJ of standard hard water.

Immediately after 5 rotations of 1 rotation up and down at a speed of 10 seconds,
．． Using a 15n+ (100 mesh) sieve, the liquid that passes through is sieved at 300 mJ! Using a porcelain stirrer, stir the liquid into a beaker of 5 m7 to exactly 300 m1! Transfer to a separatory funnel and extract with 1(X) m# of ether. The aqueous layer is further divided into the second layer. Transfer to a third separatory funnel and extract with ether. Discard water layer number 1. These ether solutions are combined, dehydrated using anhydrous sodium sulfate, and then filtered. The residue on the container and filter paper is washed with a small amount of ether, the washing liquid is combined with the filtrate, and the ether is distilled off. Add 1Qmjt of acetone to the residue and dissolve it to 1mj! Spot on the thin layer chromatogram grate. Develop with a 7:3 mixture of benzene:acetone. Protection iIN ratio (Rf
) Scrape off the oryzemate layer of about 0.64 and add acetone 25
mj! Extract with Add 5 ml of the internal standard substance solution (diisobutylketone 0.3 g/10 ml! acetone) to 5 mA of this solution, apply it to a gas chromatograph under the following conditions, calculate the amount of Oryzeme F (Amg), and calculate the degree of desorption in water using the following formula. .

Oryzemate Rt 5.2 minutes Internal standard Ht 2.2 minutes x 200 Degree of desorption in water % - OV -17 Power ram temperature: 21O.

Vaporization chamber; 235° carrier gas i N2, 50 mJ/min Detector; hydrogen ion detection IF, 1. Port D, residual ratio of active ingredient The residual ratio of the ingredient after storage (%) to the oryzemate content (g) at the time of manufacture. However, the active ingredient content is determined by taking 5 g of a sample and
1 ml of the supernatant liquid was subjected to the thin layer chromatograph described above, and the amount was calculated in the same manner.

A calibration curve is prepared in advance using pure Oryzemate.

C. Take 100g of powdering rate sample, inner diameter 100mm, inner fi 100w.
Place it in a ball mill porcelain pot of size 10m and place it on top of it for a total of 105cm.
Put 3 porcelain balls with a diameter of about 30 g and rotate at 75 revolutions per minute for 15 minutes, then 0.3 m (48 mesh: L)
The ratio of the amount passing through the sieve is the powdering rate.

The characteristics of the prototype were examined with respect to these characteristic values, and the results shown in Table 2 were obtained.

Table 2 Characteristic values of granules due to differences in binders As shown above, the granular drug of the present invention has much superior characteristic values compared to others.

Next, an experimental example will be given showing that the granules of the present invention exhibit superior curing of the active ingredient compared to granules produced using conventional coating binders.

Experimental example 1 Test granules Present invention product Oryzemate 8% granules of Example 1 Control example 1
0.06 parts of carboxymethyl cellulose and 2.94 parts of water (viscosity Granule control example 2, manufactured in exactly the same manner as in Example 1, except that 700 centipose and saponification value of 0.69) were used.3 parts of polyglobylene glycol was used in place of the coating binder of Example 1. Granule control example 3 manufactured in the same manner as in Example 1 Granule control example manufactured in the same manner as in Example I except that 3 parts of machine oil was used in place of the coating binder in Example 1 4 Granule control example 5 manufactured in exactly the same manner as in Example 1 except that 3 parts of linseed oil was used instead of the coating binder of Example 1. Granule control example 6 produced in exactly the same manner as in Example 1 except that 4 parts of urea resin (solid bone 60%) was used instead of the coating binder of Example 1. Granular paddy rice variety produced in exactly the same manner as Example 1: Nishihomare Cutting date = June Habi Harvesting date: October 31 Cultivation details: Planting density, 15 x 3001 m (22,2 plants/if) Fertilization amount: Base oil Phosphorus No. 280 (12-18-14
) per 10a, 40 kg, additional fertilizer August 14th, August 2nd
The same fertilizer was applied twice on the 7th at a dose of 20 kg per 10 a.

Plot area: 1 plot area 10rrl, each plot surrounded by corrugated ridge boards.

Date of Spraying and Amount of Spraying: On August 13th, an amount of 3 kg/10a was sprinkled.

Survey date and method: Rice blast disease onset survey was conducted on September 5th day of the imperial edict in each ward.
Plants were investigated by dividing the incidence of panicles into those with branch rot disease severity of 1/3 or more and 1/3 or less.The investigation of the onset of white leaf blight was conducted on September 3rd, with the incidence of disease occurring on 30 upper leaves of 25 plants in each district. Leaf dungeons and their lesion area rates were investigated.

The yield survey will be conducted on October 31st, the harvest day, at 3.3rr in the center of each district.
The spermatozoa type (g) of r (73 strains) was investigated.

The survey results are shown in Table 3.

Experimental example 2 Test granules Present invention product Oryzeme 14% granules of Example 2 Control example 1
0.06 parts of carboxymethyl cellulose and 2.94 parts of water (viscosity Granule control example 2, manufactured in exactly the same manner as in Example 2, except that 700 centiBose and saponification value of 0.69) were used.Execution example except that 3 parts of polypropylene glycol was used in place of the coating binder of Example 2. Granule control example 3 produced in exactly the same manner as in example 2 Granule control example 4 produced in exactly the same manner as in example 2 except that 3 parts of machine oil was used instead of the coating binder in example 2 Granule control example 5 produced in exactly the same manner as in Example 2 except that 3 parts of linseed oil was used in place of the coating binder in Example 2. Varnish (solid content 75%) 4 in place of the coating binder in Example 2 Example 6 Granules prepared in exactly the same manner as in Example 2 except that part of the urea resin was used instead of the coating binder of Example 2
The granules manufactured in exactly the same manner as in Example 2 except that 5 parts (solids content %) were used were mixed with the same paddy rice variety, inserting date, and the same as in Experimental Example 1.
Table 4 shows the results of investigating the disease onset status of panicle neck blast and branch blast blast based on harvest date, cultivation details, zoning area, application date, application amount, survey date, and method.

As is clear from Experimental Example 1.2 in Table 4 and above, the granules of the present invention have superior effects on pesticides containing 8% oryzemate and 4% compared to granules using conventional coated binders. There is.

Experimental Example 3 Test granules Present invention product Merge 5% granules control product of Example 3
Add 20 parts of water to a mixed powder of 79.5 parts of kaolin, part of bentonite, and 0.511 parts of dodecylbenzenesulfonic acid sorter, make the mixture, apply it to an extrusion granulator, and after drying, the powder will be 0.5 to 1.
On the 7th day (32 to 10 meshes), it is sieved to form base grains. From this, 95 parts were taken and, without stirring, 5 parts of marchet was absorbed to obtain a 5% granule.

Paddy rice variety: Healthy seedling transplant cultivation Nishihomare Sowing date: May 28th, Cutting date: 'June 20th Cultivation details: Planting density 15 x 30cm (22.2 plants/r)
rf) Fertilization amount Base oil ammonium sulfate No. 280 (12-18-4) 1
Fertilize 40kg per 0a Field area: 1 plot, 10 plots Each plot is surrounded by corrugated ridge boards.

Application date, amount, and method: Soil was treated at a rate of 3 kg/10 a at three times: 3 days before cutting, immediately after cutting, and 3 days after cutting.

Survey period and method Weeds were cut out on the 20th of each month, and 30 days later, weeds were pulled out for each weed type, washed with water, and the biomass (g) after being air-dried was weighed.

The survey results are shown in Table 5.

Table 5 As shown above, the product of the present invention is more effective than the control product in controlling annual weeds, perennial weeds, and other major weeds in paddy fields, and it is more effective to control annual weeds, perennial weeds, and other major weeds in paddy fields than the control product. It was more effective after a day.

Experimental Example 4 Test granules Invention product, MIPC 4% granule control product of Example 4 Dirty sand 8
Add 5 parts of carbolic acid resin adhesive (solid content 60%) to 7 parts with stirring, add powder prepared by mixing and pulverizing 4 parts of MIPC and 4 parts of clay in advance, coat with powder, and heat at 65°±3°C for about 2 hours. Granules obtained by air drying for hours Paddy rice variety: Asominori Date of insertion: June 20th Cultivation details: Planting density: 15 x 30 cm Base fertilizer amount: Base oil No. 280 (12-18-14) 40 per 10 a
k+r fertilization, August 6th Shioka Rin-an No. 280 No. 108 2
0 kg fertilization zone area = 1 zone 20 onf each zone with corrugated ridge board.

Application date, amount, method: August 1st, 3 kg per 108
Survey timing and method2 July 31st (just before spraying) August 2nd (1 day after spraying) August 15th (15 days after spraying) and August 3rd
On day 0 (□□□ days after spraying), the insect repellent effect was investigated using the following scooping method and brushing off method.

Scooping method: Two plots were set in each plot, and using an insect net with a diameter of 361 mm, scoops were scooped out from each plot 10 times and 20 times in each plot, and the pests were counted according to the pest type in each plot.

Wipe-off method: Arbitrarily extract 20 plants and a total of 60 plants from each plot as 3 plots in each area, and apply adhesive to them in a 18x2
The pests were brushed off onto a 5 cm (85 size) black celluloid board and counted by type.

The results of the scooping survey are shown in Table 6 below, and the results of the scraping survey are shown in Table 7.

Table 6, Table 7 and above, Section 6. As is clear from Table 7, the product of the present invention was effective in controlling leafhoppers and planthoppers over a long period of time.

Experimental Example 5 Test Granules 10% Pyridacoenethione Granules Control Example of Example 5 Polyoxyethylene (E, 0
8 mol) Peanut oil in place of 0.5 part of octyl phenyl ether (Total usage: 7.5 parts) Each granule larger than the granules produced in the same manner was added to 20 last instar fly larvae and 10 ml of water.
1 g each in a waist-high petri dish with a diameter of 9 cm and a height of 5 cm.
Table 8 shows the killing power after a certain period of time.

From the results shown in Table 8 and above, the granules of the present invention exhibit more rapid killing power than the control granules.

Patent Applicant Mikasa Chemical Industry Co., Ltd. Agent Sunshi Ito (and 2 others) Procedural Amendment 1, 11 Cow Jushi R Patent Application No. 5296 of Mongolia 1957 2, Title of Invention Granular Agent for Agricultural Epidemic Prevention 3, i Relationship with the person making the case: Address of the patent applicant: 4, Attorney's statement: 1, Title of the invention: Granular agent for agricultural epidemic prevention 2, Claims: ■4: Inorganic particles with a particle size of 0.1 to 2.0; The organic granules are coated with liquid mineral oil, plasticizer, or liquid semi-drying to non-drying animal and vegetable oil with a surfactant added, and the surface is coated with powdered agricultural epidemic prevention medicine 1. Detailed Description of the Invention The present invention provides a granular agent for agricultural epidemic prevention which is characterized by being coated with a powder and which maintains stability for a long period of time without undergoing sudden physical or chemical changes even during storage. The invention relates to granular drugs for use.

Recently, from the viewpoint of labor saving and prevention of environmental contamination when pest control agents for agricultural chemicals are used for pest control, weed control, and fertilization, spraying equipment has been improved and increased in size. Applications range from hand-spreading to aerial spraying using spray machines and aircraft. In this case, it is necessary to prevent drifting of fine powder due to the powdering of the main drug by spraying, preserve the environment other than the area where the herbal medicine is applied, and avoid chemical damage to growing crops. .

As a dosage form that meets these objectives, granular medicines formed into granules are often used as agricultural chemicals for epidemic prevention. Compared to other dosage forms such as powders, wettable powders, emulsions, etc., this granular agent is applied with a relatively high concentration of active ingredients after dispersion, and is particularly sensitive to weather conditions after application. Water moves vertically and horizontally, or moves to physiologically active points along with physiological and ecological functions during growth and nutrient absorption of the plant itself, and takes the process of exerting its effects, so its effects last for a relatively long period of time. It is a drug type with long-lasting residual effects.

In this way, granules differ in their relationship with target diseases, weeds, crops, and where they are used, especially soil moisture, the mechanism of action of the active ingredients of agricultural chemicals, their physicochemical properties, and the concentration of active ingredients in the formulation. There are various methods of granulation, but the following methods are currently in use.The first is a transfer-type granulation method using a granulator manufactured by Eri/Hi or a granulator manufactured by Ronosier. This involves kneading a predetermined amount of the active ingredient with a powder extender, binder, and disintegration aid with water or a mixture of water and a binder, and then forming the desired particles into the above-mentioned granulator. The second method is to use an extrusion molding machine, and the active ingredient is mixed with the same fillers and adjuvants as in the first method, generally in a concentration of 0 to 20%.
% of water and knead to form a diameter of 0.5~1.7m (32~
9 meshes) and extruded by pressing on a metal plate having small holes.
After drying, it is passed through a crusher and sieved to size the particles. The third method is the coating method. This is a method in which the active ingredient is coated directly or in a pre-pulverized powder state onto the surface of sized mineral or vegetable granules using a liquid binder to form granules. These granulation methods have generally put into practical use a particle size distribution of 0.1 to 2 fi (150 to 90 mesos) based on the required distribution density per unit area of the earth's surface during granulation.

Looking at the method for producing the above granules, in the first granulation method, when the purpose is to obtain fine particles with a particle size of about 2 dragons or less, the particle size of the granules becomes irregular. In the second extrusion molding method, the particle size is uniform, but the manufacturing yield is 85 to 95%, which has the disadvantage of poor yield. Furthermore, in these methods, it is relatively difficult to remove water after granulation, so strong ventilation or heat drying is required, and if the active ingredient is easily chemically changed by water, it may have a tendency to evaporate during drying. Such a granulation method is not suitable for grains.

In addition, in the third coating method, granular materials such as bentonite and diatomaceous earth that have porous absorption properties or disintegrate and swell in water, or materials that have relatively low water and oil absorption properties such as silica stone, volcanic lapilli, and marble; Alternatively, the natural main stone grains are coated with the active ingredient in the next step by using water, natural or synthetic oils such as kerosene, machine oil, animal and vegetable oils, or oily liquids as a binder, depending on the purpose. are manufactured in a variety of ways. Furthermore, if we analyze the granules produced by this coating method from the viewpoint of economic evaluation, (11) the raw materials can be obtained in large quantities at low cost and with uniform quality; (2) the granules can be obtained with low energy during granulation; In other words, the time required for granulation is short, and the desired particle size can be obtained at a high yield without the need for a drying process. (3) During storage, the active ingredient of the granular drug begins to decompose and the coated powder is dissolved. No deterioration of physicochemical properties such as powdering or caking due to peeling.

(4) Few grains require less labor, and their physiologically active effects have the greatest economic effect.

As described above, granulation using the coating method has many advantages over the former two methods as a granular drug for agricultural epidemic prevention.
Since the liquid binder determines the quality of the drug, there are also drawbacks such as the need to select a binder depending on the type and nature of the base particles.

Therefore, as a result of intensive research with the aim of obtaining a liquid binder for coating that can be universally used in base grains of When a granular agricultural epidemic prevention agent was manufactured by a coating method using a non-drying to semi-drying liquid made by adding a surfactant to dry animal and vegetable oil, it was found that a granular agent compatible with any base grain could be manufactured. Heading Completing the Invention.

In the present invention, one kind of liquid mineral oil, a plasticizer, and a liquid semi-drying to non-drying animal or vegetable oil or fat, or a surfactant is added to inorganic or organic granules having a particle size of 0.1 to 2.0 m. This is a granular agricultural epidemic prevention agent in which the added liquid is coated and the active ingredient of the powdered agricultural epidemic prevention agent is coated on the surface.

The inorganic and organic granular substances used as the granular base used in the present invention include crushed stones such as igneous rock, plutonic rock, aqueous rock, and marble rock, crushed granules of ceramic products such as ceramics and refractories, granular urea, inorganic salt granules, bagasse grains, and rice grains. , tobacco waste grains, corn grains, soybean oil cake, etc., are crushed to a particle size of 0.1 to 2.0 using an appropriate crusher or granulator.
The particle size is adjusted to the desired size.

The coating binder used in the present invention includes mineral oils such as kerosene, machine oil, spindle oil, refrigeration oil, turbine oil, insulating oil,
Marine machine oil, liquid paraffin, plasticizers such as phthalates such as dibutyl phthalate, phosphates such as triphenylphosphny, semi-drying to non-drying liquid animal and vegetable oils such as whale oil, castor oil, olive oil. , peanut oil, tea oil, rapeseed oil, etc.

The surfactants added to the above binder include polyoxyethylene alkylaryl ether such as polyoxyethylene nonylphenyl ether, sorbitan fatty acid ester,
Nonionic surfactants such as polyoxyethylene sorbitan fatty acid ester, anionic surfactants such as calcium dodecylbenzenesulfonate, cationic surfactants such as trimethylbenzifurammonium chloride,
Amphoteric surfactants such as cetyl aminoacetic acid can be used alone or in combination of two or more. The amount added is approximately 0.1% to the bond side number.
It is about 40%, preferably 0.5 to 10%.

In order to produce the granular drug of the present invention, the above particle size is from 0.1 to
2.0fi inorganic or organic granules, liquid mineral oil, plasticizer, or liquid drying or non-drying animal or vegetable oil and fat with a surfactant added to the granules in an amount of about 0.5 to 40%; The mixture is preferably 1 to 15% so that the surface of the granules is sufficiently coated. Separately, predetermined amounts of agricultural chemicals and epidemic prevention chemicals are mixed with approximately the same amount of carrier such as clay, white carbon, etc.
It is produced by mixing it with powders such as silica frozen earth, bentonite, kaolin, talc, etc., or by mixing and pulverizing the mixture and coating the surface of the granular material. Furthermore, when the drug is a powder, the drug and carrier may be coated on the surface of the granules separately without being mixed in advance. Alternatively, it can also be produced by adding active ingredients to an oily substance containing a surfactant at room temperature or heating to make a liquid substance, which is then coated with talc or the like after absorbing the oil into base granules.

As the agricultural and epidemic prevention chemicals used in the present invention, any known liquid or powdered chemicals can be used.

The agricultural epidemic prevention granular drug of the present invention obtained as described above already has a stable adhesive strength of the coating layer immediately after production,
Even during storage, its physicochemical properties do not undergo any chemical changes such as oxidation, and it can maintain stability for a long period of time.

Next, examples of the present invention will be shown.

Example 1 85 parts of crushed stone with particle size of 0.5 to 1.7 Tsuru (32 to 10 Me Noche), 2.91 parts of machine oil, polyoxyethylene (E,
While stirring a mixture of 0.045 m of nonylphenyl ether (02 mol), 0.03 part of polyoxyethylene (E, 05 mol) dodecylhenzen ether, and 0.015 part of calcium dodecylbenzenesulfonate, 16 parts of a powder obtained by mixing and pulverizing 8 parts of -1,2-hendiisothiazole-1,1-dioxide) and 8 parts of clay are added to obtain 8% orimate granules.

Example 2 Crushed stone 8 with a particle size of 0.5 to 1.7 m (32 to 10 m)
9 parts, 2.91 parts of machine oil, polyoxyethylene (E,
0.02 mol) nonylphenyl ether, 0.03 part of polyoxyethylene (E, 0.5 mol) dodecylbenzene ether, and 0.015 part of calcium dodecylbenzenesulfonate were added with stirring, and 4 parts of ori-supermate and clay were added in advance. 8 parts of powder obtained by mixing and pulverizing 4 parts of the above-mentioned powder are added to the crushed stone grains subjected to the above treatment, and coated to obtain 4% orimate granules.

Example 3 Sea sand 9 with a particle size of 0.5 to 1.7 m (32 to IO mesh)
To 0 parts, 0.3 parts of polyethyleneoxy (E, 0=5) dodecyl ether and 1.7 parts of spindle oil were added with stirring, and then merged end (2-chloro-2',6'-
diethyl-N-butoxymethylacetanilide) 5
1 part and then coated with 3 parts of white carbon to obtain a merged end 5% granule.

Example 4 2.5 parts of rapeseed oil, polyoxyethylene (E,
0.5 part of octylphenyl ether (04 mol) was added with stirring to moisten the surface of the polluted sand, and
14 parts of isopropylphenyl-N-methyl carhaf,
Mix and crush 4 parts of clay, add powder, coat with powder, and MIP.
C4% granules are obtained.

Example 5 5 parts of natural silica stone with a particle size of 0.5 to 0.8, 10 parts of pyridafention (diethyloxophenylpyridazine ilkisholothioate), 7 parts of peanut oil, polyoxyethylene ( A mixture of 0.5 parts of octylphenyl ether (E, 08 mol) was heated to ℃ to absorb the oil, and then coated with 2 parts of white carbon of 0.046 m or less to form 10% grains of pyridafention for epidemic prevention. get the agent.

Example 6 To 74.4 parts of granular urea having a particle size of 0.8 to 1.6 mm, 3.8 parts of sewing machine oil, 0.1 part of polyoxyethylene (E, 02 mol) nonylphenyl ether, and 0.5 parts of gum arabic were added. Moisten a mixture of 1 part and 0.6 parts of water.

To this, a mixed pulverized powder of 7.5 parts of sodium 2.4-dichlorophenoxyacetate, 412.5 parts of bentona, and 1 part of white carbon was added in advance and coated with powder to give 2.4-D゛7.
Obtain % granules.

Next, experiments and evaluations showing the superiority of the granules of the present invention over conventional granules will be described.

In the method of manufacturing granular drugs by coating method, granules produced using the coating binder of the present invention (product of the present invention), water-soluble coating binders such as polyvinyl alcohol, carboxymethyl cellulose, etc., which are conventionally used coating binders. Granules using an aqueous solution of a polymer compound as a coating binder (Control Example 1); Granules using a water-soluble aliphatic polyhydric alcohol such as ethylene glycol or polypropylene glycol as a coating binder (
Comparative Example 2), Granules using kerosene or machine oil as a coating binder (Comparative Example 3), Granules using natural animal and vegetable oil, especially drying oil, as a coating binder (Comparative Example 4), Coating with synthetic drying oil Regarding the raw material unit price, manufacturing energy, storage stability, and biological effects of granules used as a binder (Control Example 5) and granules using a synthetic resin adhesive solution as a coating binder (Control Example 6), The evaluation is as shown in Table 1 below.

Table 1 it) Each ranking number when the best one from each evaluation aspect is set as 1. Here, the term "powderization" in the storage stability section is not seen immediately after production, but after a certain period of time, the binder Due to changes such as hardening, partial hardening and shrinkage occur, exposing areas where the adhesive strength between the granule coating layer and the base grains is weakened, resulting in a phenomenon called powdering. It is. In contrast, the product of the present invention uses a non-drying coating bonding agent made of a saturated compound that can be expected to be stable for a long period of time, so the adhesive strength of the coating layer is already stable immediately after manufacturing, and even during storage. Its physicochemical properties are completely unaffected by chemical changes such as oxidation and can maintain stability for a long period of time.

Furthermore, the method using alkylene glycols in Comparative Example (2) has a higher vapor pressure than the coated binder of the present invention, and there is a risk that it will disappear and turn into powder when the container is opened. Control example (3) uses the same material as the product of the present invention, but does not contain a surfactant, which requires energy during production, especially granulation time, and particles in the target particle size range. The yield of the product is also low, and the time required for biological effects to appear after application is slow, resulting in poor overall effectiveness.

Another control example! 41. +5) basically uses a drying oil containing an unsaturated compound having an unsaturated bond in the binder raw material or a synthetic drying oil as a binder, so the coating layer becomes hard and brittle due to oxidation during storage. This causes powdering.

In addition, during the manufacturing process, an air drying or heat drying process is required, and the resulting granular drug cannot be dissolved or dispersed in water or soil moisture (because it is water-insoluble, the drug cannot be uniformly dispersed after application). Comparative example (6) is generally more expensive and more toxic than others, and its adhesive strength is also limited by the use of hardening agents or baking at high temperatures. It requires a special process to harden, and if the weather resistance of the resin is not carefully selected, there is a risk of producing incompetent granules that do not exhibit the effects of the active ingredients of agricultural and epidemic prevention drugs. Now, among these coating binders according to the above-mentioned groups, the following were selected to make 8 granular agricultural chemical oryzemate granules.

Coating binder Inventive product Machine oil, viscosity, 5 cm Bose 97 parts Polyoxyethylene (E, 04 mol) Nonylphenyl ether
1.5 parts polyoxyethylene (E, 06
mole) dodecyl ether
1.0 parts Calcium dotesylhenzensulfonate 0.
A mixture of 5 parts or more was used as the coating binder of the present invention.

The following was used as a coating binder for a control product of the present invention.

Control example 1 Polyvinyl alcohol (saponification degree 88 mol) 5
% aqueous solution control example 2 Polypropylene glycol control example 3 Machine oil (viscosity 28.5 centipose) control example 4 Linseed oil control example 5 Varnish control example 6 Urea resin (65% solids) [Manufacturing method] Particle size 0 .5 to 1.7 cranes (32 to 1 o mesosyu)
Add 3 parts of the above-mentioned coating binder to 85 parts of crushed mineral stone using a flat stirrer while stirring, and after soaking the whole with the coating binder, 16 parts of milled flour is prepared by mixing and pulverizing % Oryzemate (equipment) and 50% clay in advance. Manufactured by coating with powder.

However, the products of the present invention and the control product had inhibitions other than No. 2 and N13.

lk4. N15 and Yo6 were made by air drying for over one night.

Orijomate 8% granules for controlling rice fever disease thus prepared 0.
The yield of a product having a particle size of 5 to 1.70 (32 to 10 mesos), the degree of desorption in water of the product, the decomposition rate and powdering rate of the active ingredient after storage under heating and abuse were measured by the following methods.

B. Accurately weigh 20g of the water desorption sample and add it to a 250ml graduated cylinder with a stopper containing 20Oml of standard hard water.

Immediately after 5 rotations of 1 rotation up and down at a speed of 10 seconds,
．． Using a 15m (100 mesh) sieve, 300mt of the liquid passed through the sieve! Transfer to a beaker. While stirring the liquid using a porcelain stirrer, 50 ml of it is accurately transferred to a 300 ml separatory funnel and extracted with 100 ml of ether. The aqueous layer is further divided into the second layer. Transfer to a third separatory funnel and extract with ether. Discard the water layer. These ether solutions are combined, hydrophilized using anhydrous sodium sulfate, and then filtered. The residue on the container and filter paper is washed with a small amount of ether, the washing liquid is combined with the filtrate, and the ether is distilled off. Add 10ml of acetone to the residue and dissolve it to make 1mj! Spot on a thin layer chromatogram plate. Develop with a 7:3 mixture of benzene:acetone. Retention layer ratio (Rf) approximately 0.6
Extract the oryzemate layer from Step 4 with oysters and 25ml of liacetone. Add 5 mj of internal standard substance solution (diisobutyl ketone 0.3 g/10 mJ! Acetone) to 5 ml of this solution.
! and subjected to gas chromatography under the following conditions to calculate the amount of oryzemate (Amg) and calculate the degree of desorption in water using the following formula.

Oryzemate R15, 2 minutes Internal standard Rt 2.2 minutes Amount of oryzemate in 20 g of sample (mg) Gas chromatograph operating conditions Column carrier: Chromosolve W-AW DMC3 liquid phase: 5% silicon OV -17 Power ram temperature: 21O.

Vaporization chamber; 235° carrier gas iNz, 50 m#/min detector; hydrogen flame ion detector F, 1. Port D: Remaining rate of active ingredient Ratio of remaining component after storage (%) to oryzemate content (g) at the time of manufacture.
1, and apply 1 ml of the supernatant liquid to the thin layer chromatograph described above.

A calibration curve was created in advance using pure Oryzemate.

C. Take 100g of powdering rate sample, inner diameter 100vm, internal 100m.
m ball mill porcelain bot, and the total weight is 105.
Put 3 porcelain balls with a diameter of about 30 g and rotate at 75 revolutions per minute for 15 minutes, then 0.3 crane (48 me nosh)
The ratio of the amount passing through the sieve is the powdering rate.

The characteristics of the prototype were examined with respect to these characteristic values, and the results shown in Table 2 were obtained.

As shown in Table 2 and above, the granular drug of the present invention has significantly superior characteristic values compared to others.

Next, we will give an experimental example showing that the granules of the present invention exhibit superior effects of the active ingredient compared to granules produced using conventional coated binders.

Experimental example 1 Test granules Present invention product Comparative example 1 of Example 1 8% granules
0.06 parts of carboxymethyl cellulose and 2.94 parts of water (viscosity Granule control example 2, manufactured in exactly the same manner as in Example 1, except that 700 centiBose and saponification value of 0.69) were used. Granule control example 2, except that 3 parts of polypropylene glycol was used in place of the coating binder of Example 1. Granule Control Example 3 manufactured in exactly the same manner as in Example 1 Granule Control Example 4 manufactured in exactly the same manner as in Example 1 except that 3 parts of machine oil was used in place of the coating binder in Example 1 Granule control example 5 produced in exactly the same manner as in Example 1 except that 3 parts of linseed oil was used in place of the coating binder in Example 1. Varnish (75% solid bone) 4 in place of the coating binder in Example 1 Granule control example 6, manufactured in exactly the same manner as in Example 1, except that 5 parts of urea resin (solid bone ω%) was used instead of the coating binder of Example 1. Granular paddy rice variety produced in exactly the same way: Nishihomare Cutting date: June 2nd, Harvest date: October 31st Cultivation details: Planting density, 15 x 30 cm (22,2
Book/n? ) Fertilization amount: Base oil Rin'an No. 280 (12-18-1
4) 40kg per 10a, additional fertilizer August 14th, August 27th
The above fertilizer was applied twice a day at 20 doses per 10a.

Divided area: 1 concave area 10n? , each area was surrounded by corrugated ridge boards.

Spraying date and amount: 3 kg/1 on August 13'F3
An amount of 0 a was sprinkled.

Survey date and method: The rice blast disease onset survey was carried out on father plants in each district on September's imperial edict, and was divided into the incidence of affected panicles of 1/3 or higher and 173 or lower. To investigate the onset of bacterial leaf blight, on September 3, the percentage of affected leaves and the percentage area of lesions were investigated for 5 J30 leaves of 5 plants in each section.

The yield survey will be conducted on October 31st, the harvest day, at 3.3rr in the center of each district.
The spermatozoa type (g) of r (73 strains) was investigated.

The survey results are shown in Table 3.

Table 3 Experimental example 2 Test granules Present invention product Oryzemate 4% granules of Example 2 Control example 1
0.06 parts of carboxymethyl cellulose and 2.94 parts of water (viscosity 700 centipose, saponification value 0.69) was used (Granule control example 2 produced in the same manner as in Example 2) except that 3 parts of polypropylene glycol was used in place of the coating binder of Example 2. Granule control example 3 produced in exactly the same manner as in example 2 Granule control example 4 produced in exactly the same manner as in example 2 except that 3 parts of machine oil was used instead of the coating binder in example 2 Granule control example 5 produced in exactly the same manner as in Example 2, except that 3 parts of linseed oil was used instead of the coating binder of Example 2. Varnish (solid content 75%) was substituted for the coating binder of Example 2. Granule control example 6 produced in exactly the same manner as in Example 2 except that 4 parts were used. Example 2 except that 5 parts of urea resin (solid content 60%) was used instead of the coating binder of Example 2. Each of the granules manufactured in exactly the same manner as above was prepared using the same paddy rice variety, insertion date and date as in Experimental Example 1.
Table 4 shows the results of investigating the disease onset status of panicle neck blast and branch blast blast using harvest date, cultivation details, plot area, application date, application amount, survey date, and method.

As is clear from Experimental Example 1.2 in Table 4 and above, the granules of the present invention are less effective against pesticides containing 8% oryzemate and 4% compared to granules using conventional coated binders. ing.

Experimental Example 3 Test granule Inventive product Merged end 5% granule control product of Example 3
Add 20 parts of water to a mixed powder of 79.5 parts of kaolin, 20 parts of bentonite, and 0.5 parts of sodium dodecylbenzenesulfonate, make it, apply it to an extrusion granulator, and after drying, the powder will be 0.5-1.
Sieve into 7m (32 to 10 mesh) to form base grains.

From this, 95 parts were taken, and 5 parts of Marchet was absorbed while stirring to obtain a 5% Marchet granule.

Paddy rice variety 2M seedling transplant cultivation Nishihomare Sowing date: May 28th, Insertion date: June 20th Cultivation details: Planting density 15 x 30cm (22.2 plants/r)
rf) Fertilization amount Base oil ammonium sulfate No. 280 (12-18-4) 1
Fertilization: 40kg per 0a Zone area: 1 zone 1〇 - Each zone was fertilized by corrugated ridge boards.

Application date, amount, and method: Soil was treated at a rate of 3 kg/IOa at three times: 3 days before insertion, immediately after, and 3 days after insertion.

Survey period and method: After the first day of weeding, weeds were pulled out from each area, washed with water, and the amount of living organisms (g) weighed after being air-dried.

The survey results are shown in Table 5.

As shown in Table 5, the product of the present invention is more effective than the control product in controlling annual weeds, perennial weeds, and other major weeds in paddy fields. It was more effective after a day.

Experimental Example 4 Test granules Invention product, MIPC 4% granule control product of Example 4 Dirty sand 8
Add 5 parts of carbonic acid resin adhesive (solid official stamp %) to 7 parts with stirring, add powder prepared by mixing and pulverizing 4 parts of MIPC and 4 parts of clay in advance, coat with powder, and heat at 65°±3°C for about 2 hours. Granules obtained by ventilation drying Paddy rice variety: Asominori Date of planting = June 20th Cultivation details: Planting density 15 x 3 occm Base fertilizer amount Salt and Phosphorus 28
No. 0 (12-18-10> 40 kgm fertilizer per 10 a, August 6th Shioka Rin-an No. 280 20 kg per 10 a
fF! Area covered by zoning: 200rrf per ward.Each ward is surrounded by corrugated ridge boards.

Date and time of application, amount and method: On August 1st, the application was carried out by hand at a rate of 3 kg per 102 cm.

Survey timing and method Near August 31st (just before spraying) August 20th
(1st day of spraying f &) The insect repellent effect was investigated on August 15th (15 days after spraying) and August 30th (30 days after spraying) using the following scooping method and brushing off method.

Scooping method: Two plots were set in each plot, and insects were scooped 10 times and 20 times per plot using an insect trapping net with a diameter of 36c11, and each plot was counted according to pest type.

Brush-off method: 20 1θ0 plants were arbitrarily extracted from each plot as 3 plots in each plot, and adhesive was applied to them.
The pests were removed onto a black celluloid board of X2Scn (B5 size) and counted by type.

The results of the scooping survey are shown in Table 6 below, and the results of the scraping survey are shown in Table 7.

? ! MaSho 58-124704 (19) Table 6, Table 7 and above. As is clear from Table 7, the product of the present invention was effective in controlling leafhoppers and planthoppers over a long period of time.

Experimental Example 5 Test Granules lθ% Pyridafention Granules Control Example of Example 5 Polyoxyethylene (E, 0
8 mol) Peanut oil in place of 0.5 part of octyl phenyl ether (Total amount used: 7.5 parts) Each granule prepared in the same manner was treated with 20 last instar fly larvae and 10 mj of water.
Table 8 shows the results of adding 1 g of each to a waist-height petri dish with a diameter of 9 c and a height of 5 c Im containing No. 2 and observing the killing power after a certain period of time.

Table 8: Killing rate (%) From the above results, the granules of the present invention exhibit more rapid killing power than the control granules.

Patent applicant: Mikasa Chemical Industry Co., Ltd. Agent: Ito Sunshi (2 idiots)

Claims (1)

[Claims] 1. Inorganic or organic granules with a particle size of 0.1 to 2.0 fi are coated with liquid mineral oil, a plasticizer, or a liquid mixture of semi-drying to non-drying animal and vegetable oils and fats with a surfactant added. A granular agent for agricultural epidemic prevention, characterized in that the surface thereof is coated with a powdered agricultural epidemic prevention agent.