TRANSLATOR CERTIFICATION
`
`Date: June 2, 2020
`
`To whom it may concern:
`
`I, Frank McGee, a translator fluent in the Japanese and English languages, on behalf of
`Morningside Translations, do solemnly and sincerely declare that the following is, to the best of
`my knowledge and belief, a true and correct translation of the documents listed below in a
`form that reflects the intention and meaning of the original text.
`
`I hereby declare that all statements made herein of my own knowledge are true and that all
`statements made on information and belief are believed to be true; and further that these
`statements were made with the knowledge that willful false statements and the like so made
`are punishable by fine or imprisonment, or both, under Section 1001 of Title 18 of the United
`States Code.
`
`The document is designated as:
`
`Japanese Patent Application Publication JP 9-315902 A
`
`Frank McGee
`
`CERT-11, 2019-APR-12, V1
`
`1
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`TIDE 1009
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`(19) [Issuing Country] Japan Patent Office (JP)
`(12) [Publication Name] Gazette of Unexamined Patent Applications (A)
`(11) [Publication Number] H09-315902
`(43) [Publication Date] December 9, 1997
`
`JP H09-315902 A
`
`(51) [Int.Cl.6]
`[ID Codes] [JPO Ref. Nos.]
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`A01N 25/12
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`43/16
`101
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`43/40
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`47/12
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`57/28
`[Examination Request] Not Yet Received
`[Number of Claims] 8
`[Application Format] Online (OL)
`[Total Number of Pages] 6
`
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`[FI]
`A01N 25/12
`A
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`43/16
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`43/40 101 A
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`47/12
`A
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`57/28
`F
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` [Tech. Indicators]
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`(21) [Application Number] H08-130418
`(22) [Filing Date] May 24, 1996
`(71) [Applicant]
`[Identification Number] 000002934
`[Name] Takeda Chemical Industries, Ltd.
`[Address] 4-1-1, Doshomachi, Chuo-ku, Osaka
`(72) [Inventor]
`[Name] Junichi MURAI
`[Address] 202 Moarissheru Tsukuba Inarimae, 8-6 Inarimae, Tsukuba-shi, Ibaraki-ken
`(72) [Inventor]
`[Name] Masatoshi SAWAMURA
`[Address] 1144-401 Yatabe, Tsukuba-shi, Ibaraki-ken
`(74) [Agent]
`[Attorney]
`[Name] Tadao ASAHINA (and 1 other)
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`JP H09-315902 A
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`(54) [Title of the Invention]
`
`Pesticide Granules
`
`(57) [Abstract]
`
`[Problem]
`
`To obtain easy-to-handle pesticide granules that prevent caking and experience very little
`dusting.
`
`[Solution]
`
`Provided are pesticide granules comprising a pesticide active ingredient and anhydrous silica
`having an average particle size of about 5 to 20 nm.
`
`[Effect]
`
`Because the pesticide granules of the present invention prevent caking during long-term
`storage and cause very little dusting during use, they are useful as easy-to-handle pesticide
`granules.
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`JP H09-315902 A
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`[Claims]
`
`[Claim 1]
`
`Pesticide granules comprising a pesticide active ingredient and anhydrous silica having an
`average particle size of about 5 to 20 nm.
`
`[Claim 2]
`
`Pesticide granules according to claim 1, wherein the pesticide granules are a granular
`water-soluble powder.
`
`[Claim 3]
`
`Pesticide granules according to claim 1, wherein the pesticide active ingredient is a water-
`soluble pesticide active ingredient having solubility in water at 20°C of about 0.1 g/ml or
`more.
`
`[Claim 4]
`
`Pesticide granules according to claim 1, wherein the pesticide active ingredient is acephate,
`nitenpyram, cartap hydrochloride, or validamycin A.
`
`[Claim 5]
`
`Pesticide granules according to claim 1, wherein the pesticide active ingredient is acephate.
`
`[Claim 6]
`
`Pesticide granules according to claim 1, wherein the amount of pesticide active ingredient is
`about from 10 to 95% by weight relative to the entire formulation.
`
`[Claim 7]
`
`Pesticide granules according to claim 1, wherein the amount of anhydrous silica is about
`from 0.1 to 3% by weight relative to the entire formulation.
`
`[Claim 8]
`
`Use of anhydrous silica to prevent caking of pesticide granules.
`
`[Detailed Description of the Invention]
`
`[0001]
`
`[Technical Field of the Invention]
`
`The present invention relates to pesticide granules that prevent caking and experience very
`little dusting. The pesticide granules of the present invention prevent caking during long-
`term storage and cause very little dusting during use, and can be used as excellent
`pesticide granules for insecticidal, fungicidal, and herbicidal purposes.
`
`[0002]
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`JP H09-315902 A
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`
`[Prior Art]
`
`Calcium carbonate and high boiling-point solvents such as lactone and phenylxylylethane
`are used as anti-caking agents in the field of pesticides (JP S53-015425 A, JP S59-216801
`A, JP S63-107903 A, etc.). A granular wettable powder comprising a pesticide active
`ingredient and diatomaceous earth is described in JP H06-128102 A. A solid pesticide
`formulation comprising a fired product of acephate and synthetic silicic acid is described in
`JP H07-002612 A. However, pesticide granules comprising anhydrous silica having an
`average particle size of about 5 to 20 nm and the use of anhydrous silica to prevent caking
`of pesticide granules is not described in the literature.
`
`[0003]
`
`[Problem to be Solved by the Invention]
`
`Water-soluble powders of the prior art experience dusting when chemical agents are
`measured and liquid chemical agents are prepared. They are also difficult to measure due to
`poor fluidity. Granules experience caking during long-term storage. Liquids cannot be used
`with pesticide active ingredients that break down when dissolved in water. Liquids also have
`to be stored in solid containers such as glass bottles and plastic bottles. These containers
`are fragile and require a large amount of storage space. Disposal of used containers is also
`a problem from an environmental standpoint. It has been difficult to solve these problems
`with water-soluble powders and provide formulations that are easy to measure and that
`protect workers by not experiencing dusting. The major problem of disposing packaging
`containers for liquids also remains. Therefore, development of pesticide granules that do not
`experience dusting, that are easy to measure and handle, and that are easy to store is
`desired. Pesticide granules containing a water-soluble pesticide active ingredient also
`experience caking during long-term storage to pressure and humidity, and so measures that
`prevent caking are required.
`
`[0004]
`
`[Means for Solving the Problem]
`
`After conducting extensive research in order to solve this problem, the present inventors
`unexpectedly discovered that pesticide granules that prevent caking and experience very
`little dusting could be obtained by combining a pesticide active ingredient with anhydrous
`silica having an average particle size of about 5 to 20 nm.
`
`[0005]
`
`Specifically, the present invention relates to (1) pesticide granules comprising a pesticide
`active ingredient and anhydrous silica having an average particle size of about 5 to 20 nm;
`(2) pesticide granules according to (1), wherein the pesticide granules are a granular water-
`soluble powder; (3) pesticide granules according to (1), wherein the pesticide active
`ingredient is a water-soluble pesticide active ingredient having solubility in water at 20°C of
`about 0.1 g/ml or more; (4) pesticide granules according to (1), wherein the pesticide
`active ingredient is acephate, nitenpyram, cartap hydrochloride, or validamycin A; (5)
`pesticide granules according to (1), wherein the pesticide active ingredient is acephate; (6)
`pesticide granules according to (1), wherein the amount of pesticide active ingredient is
`about from 10 to 95% by weight relative to the entire formulation; pesticide granules
`according to (1), wherein the amount of anhydrous silica is about from 0.1 to 3% by weight
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`JP H09-315902 A
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`relative to the entire formulation; and (8) use of anhydrous silica to prevent caking of
`pesticide granules. Note that TM used in the present specification means a registered
`trademark.
`
`[0006]
`
`The pesticide active ingredient in pesticide granules of the present invention can be any
`insecticide, fungicide, or herbicide that is solid at room temperature. These pesticide active
`ingredients can be used alone or in combinations of two or more. The following are
`examples of these pesticide active ingredients.
`
`(Insecticides)
`
`Pyridafenthion, dimethoate, PMP, CVMP, dimethylvinphos, acephate, salicion, DEP, NAC,
`MTMC, MIPC, PHC, MPMC, XMC, bendiocarb, pirimicarb, mesomil, oxamyl, thiodicarb,
`cypermethrin, cartap hydrochloride, thiocyclam, bensultap, diflubenzuron, teflubenzuron,
`chlorfluazuron, buprofezin, hexthiazox, fenbutatin oxide, pyridaben, clofentedine,
`nitenpyram
`
`(Fungicides)
`
`Ziram, thiuram, captan, TPN, fthalide, tolclofos methyl, fosetyl, thiophanate methyl,
`benomyl, carbendazole, thiabendazole, dietofencarb, iprozion, vinclozolin, procymidon,
`fluorimide, oxycarboxin, mepronil, flutolanil, penciclone, metalaxyl, oxadixyl, triadimehon,
`hexaconazole, triforine, blasticidin S, kasugamycin, polyoxin, validamycin A, mildiomycin,
`PCNB, hydroxyisoxazole, dazomet, dimethymol, diclomedine, triazine, ferrimson,
`probenazole, isoprothiolane, tricyclazole, pyroquilon, oxolinic acid
`
`[0007]
`
`(Herbicides)
`
`MCP, MCPB, triclopyr, naproanilide, CNP, clomethonil, bifenox, MCC, piributicarb, DCPA,
`bromobutide, mefenacet, naprobamide, diphenamide, propizzamide, asulam, DCMU,
`linuron, daimlon, methyl dymuron, thebchuuron, bensulfuron-methyl, simazine, atrazine,
`simethrin, ametrine, promethrin, dimethamethrin, metribuzin, bentazone, oxadiazon,
`pyrazolate, benzophenup, prodiamine, glyphosate, vialafos, aloxidim, imazosulfuron,
`azimsulfuron, pyrazosulfuron ethyl, synosulfuron
`
`Any pesticide active ingredient that is solid at room temperature may be used. Among these
`pesticide active ingredients, those that have solubility in water at 20°C of at least 0.1 g/ml
`are preferred. Acephate, nitenpyram, cartap hydrochloride, and validamycin A are
`preferred, and acephate is especially preferred.
`
`[0008]
`
`In pesticide granules of the present invention, SiO2 obtained by conducting hydrolysis on
`silicon tetrachloride at a high temperature (1,000°C or more) on an oxyhydrogen flame is
`used as the anhydrous silica. Specific examples include one or more selected from among
`Aerosil 130, Aerosil 200, Aerosil 200V, Aerosil 300CF, and Aerosil R972 (all from Nippon
`Aerosil). Among these anhydrous silicas, Aerosil 200 and Aerosil 200V are preferred, and
`Aerosil 200 is especially preferred. The average particle size of the anhydrous silica is
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`JP H09-315902 A
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`usually from about 5 to 20 nm, preferably from about 7 to 15 nm, and more preferably from
`10 to 12 nm.
`
`[0009]
`
`Pesticide granules of the present invention can contain additives commonly used in pesticide
`granules. Surfactants, binders, stabilizers, colorants, preservatives, and extenders can be
`freely used, and selection of particular additives depends on the type of pesticide granule.
`The surfactant can be a nonionic surfactant, cationic surfactant, and anionic surfactant. One
`or more type of surfactant may be used. Examples of nonionic surfactants include
`polyoxyethylene alkyl ethers, polyoxyethylene alkyl phenyl ethers, polyoxyethylene
`polyoxypropylene ether, polyoxyethylene alkyl esters, sorbitan fatty acid esters,
`polyoxyethylene sorbitan fatty acid esters, block copolymers of ethylene oxide and
`propylene oxide, and higher fatty acid alkanol amides. Examples of cationic surfactants
`include alkyl amine salts and quaternary ammonium salts.
`
`[0010]
`
`Examples of anionic surfactants include naphthalene sulfonic acid polycondensation metal
`salts, alkenyl sulfonates, formalin condensates of naphthalene sulfonate, alkyl naphthalene
`sulfonates, lignin sulfonates, alkylallyl sulfonates, alkylallyl sulfonate sulfates, and other
`polymer-based compounds, as well as polystyrene sulfonic acid Na salts, polycarboxylic acid
`Na salts, ammonium polyoxyethylene distyryl phenyl ether sulfate, higher alcohol
`sulfonates, higher alcohol ether sulfonates, dialkyl sulfosuccinates, and higher fatty acid
`alkali metal salts. The surfactant used in the present invention is preferably an anionic
`surfactant or a nonionic surfactant. Among nonionic surfactants, those having an HLB value
`in a range from 9 to 13 are preferred from the standpoint of solubility in water and wetting
`action. Among anionic surfactants, those whose main component is sodium dioctyl
`sulfosuccinate or ammonium polyoxyethylene distyryl phenyl ether sulfate are preferred.
`Specific examples of anionic surfactants that can be used include Newcalgen EP-70GTM (from
`Takemoto Yushi), Neocor SW-CTM (from Dai-ichi Kogyo Seiyaku) and Sanmorin OT-70TM
`(from Sanyo Kasei) whose main component is sodium dioctylsulfosuccinate, and Dixsol WK
`and Dixsol 60A (both from Daiichi Kogyo Seiyaku) whose main component is
`polyoxyethylene distyryl phenyl ether sulfate ammonium. Examples of nonionic surfactants
`whose HLB value is from 9 to 12 include polyoxyethylene alkylphenyl ethers (such as
`polyoxyethylene nonylphenyl ether (NP-85TM from Takemoto Yushi) and block copolymers of
`ethylene oxide and propylene oxide (such as Newpol PE-64TM from Sanyo Chemical).
`
`[0011]
`
` A
`
` water-soluble binder is preferably used as a binder. Examples of water-soluble binders
`include dextrin, polyvinyl alcohol, gum arabic, sodium alginate, polyvinylpyrrolidone,
`glucose, and sucrose. Dextrin is especially preferred. Including a water-soluble binder
`improves the granule strength of pesticide granules of the present invention without
`undermining disintegration and dispersibility in water. Phosphoric acid or a PAP (isopropyl
`acid phosphate) aid can be used as a stabilizer. Cyanine Green G or Erio Green B400 can be
`used as a colorant. Butylparaben or potassium sorbate can be used as a preservative.
`Lactose, sodium bicarbonate, ammonium sulfate, urea, or sucrose can be used as a bulking
`agent.
`
`[0012]
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`JP H09-315902 A
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`The amount of pesticide active ingredient in pesticide granules of the present invention
`relative to the overall formulation is usually about 5 to 95% by weight, preferably about 10
`to 95% by weight, more preferably about 30 to 95% by weight, and even more preferably
`about 50 to 95% by weight. The amount of anhydrous silica relative to the overall
`formulation is usually about 0.1 to 3% by weight, preferably about 0.3 to 3% by weight,
`and more preferably about 0.5 to 2% by weight. The amount of surfactant relative to the
`overall formulation is usually about 10% by weight or less and preferably about 5% by
`weight or less. The amount of binder relative to the overall formulation is usually about 20%
`by weight or less and preferably about 10% by weight or less. The amount of colorant
`relative to the overall formulation is usually about 0.3% by weight or less and preferably
`about 0.1% by weight or less. The amount of other additives such as stabilizers and
`preservatives relative to the overall formulation is about 10% by weight or less.
`
`[0013]
`
`[Embodiment of the Invention]
`
`Pesticide granules of the present invention can be prepared using a wet extrusion
`granulation method or dry granulation method commonly used to prepare pesticide
`granules. In the wet extrusion granulation method, extrusion granulation is commonly
`performed using from about 1 to 10 parts by weight water per 100 parts by weight
`formulation in terms of solid content. The dry granulation method produces granules by
`compaction without using water. In the wet granulation method, the pesticide active
`ingredient, anhydrous silica and, if necessary, a surfactant and binder, etc. are thoroughly
`mixed together using, for example, a kneading machine. The components are mixed
`together in terms of the proper solid content, liquid components are instilled, and mixing is
`continued. When the solid components are lumpy, they may be coarsely ground to obtain a
`suitable powder so that the mixing operation goes more smoothly. A particle size of about 1
`to 100 μm is suitable for a powder. Next, the proper amount of water is added to the
`mixture, and the mixture is kneaded further in the kneading machine. The kneading is
`performed until the kneaded material has a smooth viscousness suitable for extrusion
`granulation. The kneaded material is granulated in a wet extrusion granulator, dried, and
`then sized in a sieve to obtain granules.
`
`[0014]
`
`In the dry granulation method, the pesticide active ingredient and anhydrous silica are
`thoroughly mixed together using a mixer. The mixture is then granulated using a dry
`granulator. A product of the dry granulation method has poorer disintegration in water and
`dispersibility in water compared to a product of the wet granulation method, but no
`surfactant or binder is required and kneading and drying steps are not required. If
`necessary, the granules can be sized to obtain the desired pesticide granules. The sizing is
`performed by passing the granules through a 1,700 μm mesh but not through a 300 μm
`mesh. The major axis of the resulting granules is preferably in the range from 0.5 to 5.0
`mm. The bulk density of the resulting pesticide granules of the present invention is usually
`in the range from about 0.1 to 1.2 g/ml and preferably in the range from about 0.5 to 1.0
`g/ml. The amount of pesticide granules of the present invention that are used depends on
`the type and amount of pesticide active ingredient in the granules, but is usually from about
`100 to 5,000 g per 100 square meters and preferably from about 200 to 4,000 g per 100
`square meters. The pesticide granules of the present invention are commonly used as a
`granular water-soluble powder. Because anhydrous silica does not usually dissolve in water,
`water-soluble powder in the present specification means 97% by weight or more dissolves
`relative to the entire formulation. Pesticide granules of the present invention can be sprayed
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`JP H09-315902 A
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`using any method common in the art. For example, the pesticide granules can be dissolved
`and diluted in water prior to use. The pesticide granules are preferably diluted by a factor of
`about 100 to 20,000 (from about 1 g/100 ml to 1 g/20,000 ml). In order to avoid moisture,
`pesticide granules of the present invention are preferably stored in a moisture-proof
`container. Examples include plastic jars, polyethylene bottles, polyethylene-laminated
`aluminum foil packaging, and polyethylene bags.
`
`[0015]
`
`[Examples]
`
`The following is a more detailed description of the present invention with reference to
`reference examples, working examples, and test examples. Note that the scope of the
`present invention is not limited to these examples. Note also that all parts and percentages
`used in the following description are parts by weight and weight percentages except where
`otherwise indicated.
`
`[Reference Example 1]
`
`Preparation of Granules A Containing 50% Acephate
`
`After thoroughly mixing together 50 parts acephate, 0.5 parts Newpol PE-64 surfactant, 0.1
`parts Cyanine Green G, and 49.4 parts lactose, 6 parts water was added per 100 parts by
`weight formulation in terms of solid content, and the mixture was kneaded using a kneading
`machine (Kikusui Seisakusho KM-1.5) at room temperature until a smooth viscousness was
`produced. The kneaded material was then granulated into cylindrical granules using an
`extrusion granulator (Kikusui Seisakusho RG-5M) with a 0.8 mm diameter screen. The
`resulting granules were then dried for one hour at 60°C to obtain Granules A containing
`50% acephate.
`
`[0016]
`
`[Reference Example 2]
`
`Preparation of Granules B Containing 50% Acephate
`
`After thoroughly mixing together 50 parts acephate, 0.5 parts surfactant NP-85, 3.0 parts
`dextrin, 0.1 part Cyanine Green G, 2.0 parts titanium oxide, and 44.4 parts lactose, 7 parts
`water was added per 100 parts by weight formulation in terms of solid content, and the
`resulting mixture was prepared in the same manner as Reference Example 1 to obtain
`Granules B containing 50% acephate.
`
`[0017]
`
`[Reference Example 3]
`
`Preparation of Granules C Containing 50% Acephate
`
`After thoroughly mixing together 50 parts acephate, 0.2 parts Dixsol WK surfactant, 0.1
`part Cyanine Green G, 2.0 parts white carbon (Carplex CS-5 from Shionogi
`Pharmaceuticals), and 47.7 parts lactose, 9 parts water was added per 100 parts by weight
`formulation in terms of solid content, and the resulting mixture was prepared in the same
`manner as Reference Example 1 to obtain Granules C containing 50% acephate.
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`JP H09-315902 A
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`[0018]
`
`[Reference Example 4]
`
`Preparation of Granules D Containing 95% Acephate
`
`After thoroughly mixing together 95 parts acephate, 0.5 parts Newpol PE-64 surfactant, 1.0
`part dextrin, 0.1 part Cyanine Green G, and 3.4 parts lactose, 8 parts water was added per
`100 parts by weight formulation in terms of solid content, and the resulting mixture was
`prepared in the same manner as Reference Example 1 to obtain Granules D containing 95%
`acephate.
`
`[0019]
`
`[Example 1]
`
`Preparation of Granules E Containing 10% Nitenpyram
`
`After thoroughly mixing together 10 parts nitenpyram, 0.5 parts Dixsol WK surfactant, 0.1
`part Cyanine Green G, 2.0 parts Aerosil 200, and 87.4 parts sodium bicarbonate, 5 parts
`water was added per 100 parts by weight formulation in terms of solid content, and the
`resulting mixture was prepared in the same manner as Reference Example 1 to obtain
`Granules E containing 10% nitenpyram.
`
`[0020]
`
`[Example 2]
`
`Preparation of Granules F Containing 25% Acephate and 25% Cartap Hydrochloride
`
`After thoroughly mixing together 25 parts acephate, 25 parts cartap hydrochloride, 0.5
`parts NP-85 surfactant, 0.3 parts phosphoric acid, 0.1 part Cyanine Green G, 2.0 copies of
`Aerosil 200, and 47.1 parts lactose, 5 parts water was added per 100 parts by weight
`formulation in terms of solid content, and the resulting mixture was prepared in the same
`manner as Reference Example 1 to obtain Granules F containing 25% acephate and 25%
`cartap hydrochloride.
`
`[0021]
`
`[Example 3]
`
`Preparation of Granules G Containing 50% Acephate
`
`After thoroughly mixing together 50 parts acephate, 0.2 parts Dixsol WK surfactant, 0.1
`part Cyanine Green G, 2.0 parts Aerosil 200, and 47.7 parts lactose, 6 parts water was
`added per 100 parts by weight formulation in terms of solid content, and the resulting
`mixture was prepared in the same manner as Reference Example 1 to obtain Granules G
`containing 50% acephate.
`
`[0022]
`
`[Example 4]
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`JP H09-315902 A
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`
`Preparation of Granules H Containing 75% Cartap Hydrochloride
`
`After thoroughly mixing together 75 parts cartap hydrochloride, 0.5 parts Newpol PE-64
`surfactant, 0.3 parts phosphoric acid, 0.1 part cyanine green G, 1.0 part Aerosil 200, and
`23.1 parts lactose, 4 parts water was added per 100 parts by weight formulation in terms of
`solid content, and the resulting mixture was prepared in the same manner as Reference
`Example 1 to obtain
`
`Granules H containing 75% cartap hydrochloride.
`
`[0023]
`
`[Example 5]
`
`Preparation of Granules I Containing 50% Cartap Hydrochloride and 5% Validamycin A
`
`After thoroughly mixing together 50 parts cartap hydrochloride, 5 parts validamycin, 0.5
`parts NP-85 surfactant, 0.3 parts phosphoric acid, 0.1 part Cyanine Green G, 2.0 parts
`Aerosil 200, 0.05 parts butyl paraben, and 42.05 parts lactose, 4 parts water was added per
`100 parts by weight formulation in terms of solid content, and the resulting mixture was
`prepared in the same manner as Reference Example 1 to obtain Granules I containing 50%
`cartap hydrochloride and 5% validamycin A.
`
`[0024]
`
`[Example 6]
`
`Preparation of Granules J Containing 95% Acephate
`
`After thoroughly mixing together 95 parts acephate, 0.2 parts Dixsol WK surfactant, 0.1
`part Cyanine Green G, 0.5 part Aerosil 200, and 4.2 parts lactose, 4 parts water was added
`per 100 parts by weight formulation in terms of solid content, and the resulting mixture was
`prepared in the same manner as Reference Example 1 to obtain Granules J containing 95%
`acephate.
`
`[0025]
`
`[Example 7]
`
`Preparation of Granules K Containing 50% Acephate
`
`After thoroughly mixing together 50 parts acephate, 0.5 parts Newpol PE-64 surfactant, 0.1
`part Cyanine Green G, 2.0 parts Aerosil 200, and 47.4 parts lactose, 6 parts water was
`added per 100 parts by weight formulation in terms of solid content, and the resulting
`mixture was prepared in the same manner as Reference Example 1 to obtain Granules K
`containing 50% acephate.
`
`[0026]
`
`[Example 8]
`
`Preparation of Granules L Containing 10% Nitenpyram and 5% Validamycin A
`
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`JP H09-315902 A
`
`
`After thoroughly mixing together 10 parts nitenpyram, 5 parts validamycin, 0.5 parts
`Newpol PE-64 surfactant, 0.1 part Cyanine Green G, 1.0 part Aerosil 200, 0.05 parts butyl
`paraben, and 83.35 parts sodium bicarbonate, 3 parts water was added per 100 parts by
`weight formulation in terms of solid content, and the resulting mixture was prepared in the
`same manner as Reference Example 1 to obtain Granules L Containing 10% nitenpyram and
`5% validamycin A.
`
`[0027]
`
`[Example 9]
`
`Preparation of Granules M Containing 75% Acephate
`
`After thoroughly mixing together 75 parts acephate, 0.5 parts Newpol PE-64 surfactant, 1.0
`part dextrin, 0.1 part Cyanine Green G, 2.0 parts Aerosil 200, and 21.4 parts lactose, 6
`parts water was added per 100 parts by weight formulation in terms of solid content, and
`the resulting mixture was prepared in the same manner as Reference Example 1 to obtain
`Granules M containing 75% acephate.
`
`[0028]
`
`[Test Example 1]
`
`Disintegration in Water
`
`500 ml of water was poured into a 500 ml cylinder and a sample was added to reach an
`active ingredient concentration of 500 ppm. The disintegration properties were then
`evaluated according to the following three levels.
`
`A: More than half of the formulation had disintegrated before reaching the bottom of the
`cylinder
`
`B: More than half of the formulation had not disintegrated before reaching the bottom of the
`cylinder
`
`[0029]
`
`[Test Example 2]
`
`Dispersibility in Water
`
`500 ml of water was poured into a 500 ml cylinder and a sample was added to reach an
`active ingredient concentration of 500 ppm. Sample dispersion was checked each time the
`cylinder was turned over (180 degrees x 2), and the number of times the cylinder had to be
`turned over before the sample became primary particles was measured.
`
`[0030]
`
`[Test Example 3]
`
`Caking
`
`
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`JP H09-315902 A
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`Test granules were added to a rigid cylindrical pot made of polyvinyl chloride (inner
`diameter: 8 cm, height: 12 cm) to a height of 6 cm and the surface was smoothed out. A
`hard disk made of polyvinyl chloride that was 1 to 2 mm smaller than the inner diameter of
`the pot was placed on top and weights were added to adjust the load to 25 g/cm2. A plastic
`bag (thickness: 0.03 mm) was placed over the pot, and the mouth was secured with a
`rubber band so as not to apply any pressure. This was allowed to stand at 40°C for 3 days
`and then at 0°C for 2 days, before removing the load and tipping the pot to observe the
`caking conditions.
`
`{Evaluation Method}
`
` -
`
` The pot was tipped and no caking was observed.
`+ The pot was tipped and caking was observed, but the caking readily disintegrated with
`light tapping. Alternatively, masses of less than 5 mm were observed.
`++ The pot was tipped, caking was observed, and about half disintegrated with light
`tapping. Alternatively, masses of 5 mm or more were observed.
`+++ The pot was tipped, caking was observed, and most did not disintegrate even after
`vigorous tapping.
`
`The results from Test Examples 1 to 3 are shown in Table 1.
`
`[0031]
`
`[Table 1]
`
`
`Results of Testing Formulations for Disintegration in Water,
`Dispersibility in Water, and Caking
`Disintegration in
`Dispersibility in
`Water
`Water
`A
`0
`B
`5
`A
`1
`A
`1
`A
`1
`A
`1
`A
`0
`A
`1
`A
`1
`A
`0
`A
`0
`A
`1
`A
`1
`
`Example
`
`Granules A
`Granules B
`Granules C
`Granules D
`Granules E
`Granules F
`Granules G
`Granules H
`Granules I
`Granules J
`Granules K
`Granules L
`Granules M
`
`Caking
`
`++
`++
`++
`+++
`-
`-
`-
`-
`-
`-
`-
`-
`-
`
`
`It is clear from Table 1 that the granular water-soluble powders of the present invention
`have excellent disintegration in water, dispersibility in water, and caking properties.
`
`[0032]
`
`[Effect of the Invention]
`
`The pesticide granules of the present invention suppressed dusting when chemical agents
`were measured and liquid chemical agents were prepared and were thus easy to measure
`
`
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`JP H09-315902 A
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`and handle. These pesticide granules also prevented caking during long-term storage and
`had fewer harmful chemical effects. In addition, the pesticide granules readily disintegrated
`and dispersed in water to create easy-to-use formulations that can be used in place of
`conventional powdery water-soluble formulations and liquid formulations.
`
`
`
`
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`13
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`14
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`