JP4421309B2 - Agricultural and horticultural granule wettable powder - Google Patents
Agricultural and horticultural granule wettable powder Download PDFInfo
- Publication number
- JP4421309B2 JP4421309B2 JP2004011758A JP2004011758A JP4421309B2 JP 4421309 B2 JP4421309 B2 JP 4421309B2 JP 2004011758 A JP2004011758 A JP 2004011758A JP 2004011758 A JP2004011758 A JP 2004011758A JP 4421309 B2 JP4421309 B2 JP 4421309B2
- Authority
- JP
- Japan
- Prior art keywords
- wettable powder
- agricultural
- sodium
- parts
- granulated
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Lifetime
Links
- 239000004563 wettable powder Substances 0.000 title claims description 111
- 239000008187 granular material Substances 0.000 title claims description 84
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 claims description 69
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- 238000002844 melting Methods 0.000 claims description 50
- 230000008018 melting Effects 0.000 claims description 48
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 48
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical group O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 47
- 150000003839 salts Chemical class 0.000 claims description 32
- 238000001179 sorption measurement Methods 0.000 claims description 32
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- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 claims description 22
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- XOAAWQZATWQOTB-UHFFFAOYSA-N taurine Chemical compound NCCS(O)(=O)=O XOAAWQZATWQOTB-UHFFFAOYSA-N 0.000 claims description 18
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- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 claims description 8
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- CKLJMWTZIZZHCS-REOHCLBHSA-N L-aspartic acid Chemical compound OC(=O)[C@@H](N)CC(O)=O CKLJMWTZIZZHCS-REOHCLBHSA-N 0.000 claims description 2
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- WHUUTDBJXJRKMK-VKHMYHEASA-N L-glutamic acid Chemical compound OC(=O)[C@@H](N)CCC(O)=O WHUUTDBJXJRKMK-VKHMYHEASA-N 0.000 claims description 2
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- FFEARJCKVFRZRR-BYPYZUCNSA-N L-methionine Chemical compound CSCC[C@H](N)C(O)=O FFEARJCKVFRZRR-BYPYZUCNSA-N 0.000 claims description 2
- COLNVLDHVKWLRT-QMMMGPOBSA-N L-phenylalanine Chemical compound OC(=O)[C@@H](N)CC1=CC=CC=C1 COLNVLDHVKWLRT-QMMMGPOBSA-N 0.000 claims description 2
- KZSNJWFQEVHDMF-BYPYZUCNSA-N L-valine Chemical compound CC(C)[C@H](N)C(O)=O KZSNJWFQEVHDMF-BYPYZUCNSA-N 0.000 claims description 2
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- 239000004472 Lysine Substances 0.000 claims description 2
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- OQFSQFPPLPISGP-UHFFFAOYSA-N beta-carboxyaspartic acid Natural products OC(=O)C(N)C(C(O)=O)C(O)=O OQFSQFPPLPISGP-UHFFFAOYSA-N 0.000 claims description 2
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 claims description 2
- XUJNEKJLAYXESH-UHFFFAOYSA-N cysteine Natural products SCC(N)C(O)=O XUJNEKJLAYXESH-UHFFFAOYSA-N 0.000 claims description 2
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- 239000000203 mixture Substances 0.000 description 50
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- WODOUQLMOIMKAL-FJSYBICCSA-L disodium;(2s)-2-(octadecanoylamino)pentanedioate Chemical compound [Na+].[Na+].CCCCCCCCCCCCCCCCCC(=O)N[C@H](C([O-])=O)CCC([O-])=O WODOUQLMOIMKAL-FJSYBICCSA-L 0.000 description 42
- 239000004480 active ingredient Substances 0.000 description 41
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- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 33
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- YDEXUEFDPVHGHE-GGMCWBHBSA-L disodium;(2r)-3-(2-hydroxy-3-methoxyphenyl)-2-[2-methoxy-4-(3-sulfonatopropyl)phenoxy]propane-1-sulfonate Chemical compound [Na+].[Na+].COC1=CC=CC(C[C@H](CS([O-])(=O)=O)OC=2C(=CC(CCCS([O-])(=O)=O)=CC=2)OC)=C1O YDEXUEFDPVHGHE-GGMCWBHBSA-L 0.000 description 15
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- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 description 1
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- PSZYNBSKGUBXEH-UHFFFAOYSA-M naphthalene-1-sulfonate Chemical compound C1=CC=C2C(S(=O)(=O)[O-])=CC=CC2=C1 PSZYNBSKGUBXEH-UHFFFAOYSA-M 0.000 description 1
- CRVVHBFLWWQMPT-UHFFFAOYSA-N naphthalene-1-sulfonic acid;sodium Chemical compound [Na].C1=CC=C2C(S(=O)(=O)O)=CC=CC2=C1 CRVVHBFLWWQMPT-UHFFFAOYSA-N 0.000 description 1
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- YEBIHIICWDDQOL-YBHNRIQQSA-N polyoxin Polymers O[C@@H]1[C@H](O)[C@@H](C(C=O)N)O[C@H]1N1C(=O)NC(=O)C(C(O)=O)=C1 YEBIHIICWDDQOL-YBHNRIQQSA-N 0.000 description 1
- 229920002503 polyoxyethylene-polyoxypropylene Polymers 0.000 description 1
- 229920002223 polystyrene Polymers 0.000 description 1
- 229920002451 polyvinyl alcohol Polymers 0.000 description 1
- 235000019422 polyvinyl alcohol Nutrition 0.000 description 1
- 229920000036 polyvinylpyrrolidone Polymers 0.000 description 1
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- 239000011148 porous material Substances 0.000 description 1
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- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 1
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- 239000000454 talc Substances 0.000 description 1
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- 239000004408 titanium dioxide Substances 0.000 description 1
- 125000002023 trifluoromethyl group Chemical group FC(F)(F)* 0.000 description 1
- 235000015112 vegetable and seed oil Nutrition 0.000 description 1
- 239000008158 vegetable oil Substances 0.000 description 1
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Landscapes
- Agricultural Chemicals And Associated Chemicals (AREA)
Description
本発明は水に投入後、速やかに崩壊、分散する農園芸用顆粒水和剤に関する。 The present invention relates to a granulating wettable powder for agricultural and horticultural use that disintegrates and disperses quickly after being introduced into water.
従来の水和剤は、農薬原体、湿潤剤、分散剤および増量剤を混合粉砕して製造される。しかし、これらの水和剤は、農薬原体が無機鉱物質などと共に微細に粉砕された微粉末であるために見掛け比重が小さく嵩張ること、水に懸濁させて散布液を調製する際に該微粉末が舞い上がり、作業者の健康上好ましくないこと、微粉末であるため計量に手間がかかることなどの問題点があり、近年、水和剤を顆粒化した顆粒水和剤を開発する試みがなされている。 Conventional wettable powders are produced by mixing and grinding an agrochemical raw material, a wetting agent, a dispersing agent and a bulking agent. However, these wettable powders are fine powders that are finely pulverized together with inorganic minerals and the like, so that the specific gravity is small and bulky. When preparing the spray liquid by suspending in water, There is a problem that fine powder soars and is unfavorable for the health of workers, and it is troublesome to measure because it is fine powder. In recent years, attempts have been made to develop a granular wettable powder in which a wettable powder is granulated. Has been made.
顆粒水和剤は、農薬原体、湿潤剤、分散剤、結合剤および必要に応じて、その他の補助剤を混合・粉砕して顆粒状に造粒したものである。顆粒水和剤は水に投入後、速やかに崩壊、分散する必要性があり、崩壊、分散させるための種々の工夫がなされ、例えば、分散剤としてアルキルナフタレンスルホン酸塩ホルマリン縮合物、リグニンスルホン酸塩、ポリアクリル酸塩、アルキルアリールスルホン酸塩、ポリカルボン酸塩、ポリオキシエチレンポリオキシプロピレンブロックポリマー、ポリスチレンポリオキシエチレンブロックポリマー等を用い、また、湿潤剤として、アルキルナフタレンスルホン酸ナトリウム、アルキル硫酸ナトリウム、アルキルベンゼンスルホン酸ナトリウム、アルキルスルホコハク酸ナトリウム、ポリオキシエチレンアルキルアリールエーテル等を用いる農園芸用顆粒水和剤の製造方法が報告されている（例えば、非特許文献１）。 The granule wettable powder is granulated into a granular form by mixing and pulverizing an agrochemical raw material, a wetting agent, a dispersing agent, a binder and, if necessary, other auxiliary agents. Granule wettable powder needs to disintegrate and disperse quickly after being added to water, and various devices for disintegrating and dispersing are used. For example, alkylnaphthalene sulfonate formalin condensate, lignin sulfonic acid as a disperser. Salts, polyacrylates, alkylaryl sulfonates, polycarboxylates, polyoxyethylene polyoxypropylene block polymers, polystyrene polyoxyethylene block polymers, etc. are used, and sodium alkylnaphthalene sulfonates, alkyls are used as wetting agents. A method for producing a granulating wettable powder for agriculture and horticulture using sodium sulfate, sodium alkylbenzenesulfonate, sodium alkylsulfosuccinate, polyoxyethylene alkylaryl ether, or the like has been reported (for example, Non-Patent Document 1).
また、製造が難しい常温で液体の農薬原体や低融点の農薬原体を用いる農園芸用顆粒水和剤の製造方法に関しては、常温で液体の農薬原体や低融点の農薬原体を多量の不活性物質と混合して製剤化する方法や該農薬原体を溶剤に溶解させたものを吸着担体に吸着させて製剤化する方法が提案されている（例えば、非特許文献１）。 In addition, with regard to the production method of granulated wettable powder for agricultural and horticultural use that is difficult to produce at room temperature and a low-melting pesticide active ingredient, a large amount of liquid pesticide active substance and low-melting pesticide active ingredient are used at room temperature. There are proposed a method of preparing a mixture by mixing with an inert substance and a method of preparing a preparation by adsorbing an agrochemical base dissolved in a solvent onto an adsorption carrier (for example, Non-Patent Document 1).
しかし、それらの方法を用いて、７０℃以下の融点又は軟化点を有する農薬原体を顆粒水和剤として製剤化しようとしても、その原因は不明であるが、良好な水中での崩壊性と分散性を有する顆粒水和剤を製造することは困難であった。そのため、更に改良を加えた顆粒水和剤の製造方法として、例えば、融点７０℃以下の農薬原体に湿式法シリカの焼成品と分散剤を加えることにより顆粒水和剤を製造する方法が提案されている（例えば、特許文献１参照）。 However, even if those methods are used to formulate an agrochemical base having a melting point or softening point of 70 ° C. or lower as a granulating wettable powder, the cause is unknown, but the disintegration in water is good. It has been difficult to produce a dispersible granular wettable powder. Therefore, as a method for producing granulated wettable powder with further improvements, for example, a method for producing granulated wettable powder by adding a wet-processed silica fired product and a dispersant to an agrochemical base having a melting point of 70 ° C. or less is proposed. (For example, refer to Patent Document 1).
しかし、この方法では、７０℃以下の融点又は軟化点を有する農薬原体を用いる場合には、十分な崩壊性と分散性を有する顆粒水和剤を得ることはできなかった。 However, in this method, when using an agrochemical raw material having a melting point or softening point of 70 ° C. or lower, it was not possible to obtain a granular wettable powder having sufficient disintegration and dispersibility.
本発明の目的は、７０℃以下の融点又は軟化点を有する農薬原体を用いて水中での崩壊性と分散性に優れ、かつ薬害がない農園芸用顆粒水和剤を提供することにある。 An object of the present invention is to provide a granulating wettable powder for agricultural and horticultural use which is excellent in disintegration and dispersibility in water and has no phytotoxicity, using an agrochemical base having a melting point or softening point of 70 ° C. or lower. .
本発明者らは、分散剤の構造が顆粒水和剤の水中での崩壊性と分散性に与える影響につき種々検討した結果、７０℃以下の融点又は軟化点を有する農薬原体と分散剤としてのＮ−アシルアミノ酸塩と吸着担体との混合物を造粒することにより、優れた水中での崩壊性と分散性を有する顆粒水和剤が得られることを見出した。Ｎ−アシルアミノ酸塩は低刺激性で安全性が高い界面活性剤として洗剤クリーム等に従来から用いられてきたが、顆粒水和剤に用いた例はない。Ｎ−アシルアミノ酸塩という特定の分散剤と７０℃以下の融点又は軟化点を有する農薬原体との組合せが本発明の目的を達成する上で顕著な効果を奏したものである。
本発明はこれらの知見に基づいて完成されたものである。
As a result of various studies on the influence of the structure of the dispersing agent on the disintegration property and dispersibility of the granular wettable powder in water, the present inventors have found that as an agrochemical base and a dispersing agent having a melting point or softening point of 70 ° C. or lower. It was found that a granulated wettable powder having excellent disintegration and dispersibility in water can be obtained by granulating a mixture of the N-acylamino acid salt of and an adsorbent carrier. N-acyl amino acid salts have been conventionally used in detergent creams and the like as surfactants with low irritation and high safety, but there are no examples of using them in granulated wettable powders. A combination of a specific dispersant called N-acylamino acid salt and an agrochemical raw material having a melting point or softening point of 70 ° C. or lower has a remarkable effect in achieving the object of the present invention.
The present invention has been completed based on these findings.
すなわち、本発明は、７０℃以下の融点又は軟化点を有する農薬原体、Ｎ−アシルアミノ酸塩及び吸着担体を含有することを特徴とする農園芸用顆粒水和剤を提供する。 That is, the present invention provides an agro-horticultural granule wettable powder characterized by containing an agrochemical base having a melting point or softening point of 70 ° C. or lower, an N-acylamino acid salt, and an adsorption carrier.
また、本発明は、上記水和物に芳香族スルホン酸塩のホルマリン縮合物及びリグニンスルホン酸塩の少なくとも１種を更に含有する農園芸用顆粒水和剤を提供する。 The present invention also provides an agricultural and horticultural granule wettable powder further containing at least one of a formalin condensate of an aromatic sulfonate and a lignin sulfonate in the hydrate.
さらに、本発明は、上記水和物にＮ−アシルメチルタウリン酸塩を更に含有する農園芸用顆粒水和剤を提供する。 Furthermore, the present invention provides a granulating wettable powder for agriculture and horticulture, which further contains N-acylmethyl taurate in the hydrate.
本発明の農園芸用顆粒水和剤は、従来、顆粒水和剤の製造が困難であった７０℃以下の融点又は軟化点を有する農薬原体を使用するにも拘わらず、分散剤としてＮ−アシルアミノ酸塩を使用することにより、水中での崩壊性及び分散性に優れる。 The granulated wettable powder for agricultural and horticultural use according to the present invention is N as a dispersant, despite the use of an agrochemical base having a melting point or softening point of 70 ° C. or lower, which has heretofore been difficult to produce a granular wettable powder. -By using an acylamino acid salt, it is excellent in disintegration and dispersibility in water.
また、本発明の農園芸用顆粒水和剤は、有効成分である農薬原体が安定して作用すると共に、薬害が生じず、かつ分散剤として使用するＮ−アシルアミノ酸塩が人体や動物への刺激性が低く、また自然環境で分解されるために、人や環境への毒性を低減することができる。 In addition, the agricultural and horticultural granule wettable powder of the present invention has a stable action of the active ingredient of an agricultural chemical, does not cause phytotoxicity, and an N-acylamino acid salt used as a dispersant is suitable for humans and animals. Is less irritating and decomposes in the natural environment, which can reduce human and environmental toxicity.
更に、本発明の農園芸用顆粒水和剤は、Ｎ−アシルメチルタウリン酸塩を更に含有することによって、ＣａやＭｇを多量に含有する硬水に適用した場合でも水中での崩壊性及び分散性に優れる。 Furthermore, the granulated wettable powder for agricultural and horticultural use of the present invention further contains N-acylmethyl taurate, so that it can be disintegrated and dispersed in water even when applied to hard water containing a large amount of Ca and Mg. Excellent.
［農薬原体］
本発明の農園芸用顆粒水和剤に用いる農薬原体としては、７０℃以下の融点又は軟化点を有するものであれば、殺菌剤、除草剤または植物成長調整剤などの一般に農薬として使用される化合物を使用でき、これらの化合物は単独又は２種以上混合して使用できる。
[Pesticide active ingredient]
As an agrochemical raw material used for the granulated wettable powder for agriculture and horticulture of the present invention, as long as it has a melting point or softening point of 70 ° C. or less, it is generally used as an agrochemical such as a bactericide, herbicide or plant growth regulator. These compounds can be used alone or in admixture of two or more.
７０℃以下の融点を有する農薬原体としては、例えば、２−（１，２−ジメチルプロピルアミノ）−４−エチルアミノ−６−メチルチオ−１，３，５−トリアジン（一般名：ジメタメトリン、融点：６５℃）、Ｓ，Ｓ−ジメチル−２−（ジフルオロメチル）−４−イソブチル−６−（トリフルオロメチル）−３，５−ピリジンジカルボチオナート（一般名：ジチオピル、融点：６５℃）、２，３−ジヒドロ−３，３−ジメチルベンゾフラン−５−イルエタンスルホナート（一般名：ベンフレセート、融点：３２〜３５℃）、ブチル（Ｒ）−２−［４−（４−シアノ−２−フルオロフェノキシ）フェノキシ］プロピオナート（一般名：シハロホップブチル、融点：５０℃）、Ｓ−１−メチル−１−フェニルエチルピペリジン−１−カルボチオアート（一般名：ジメピペレート、融点：３８．８〜３９．３℃）等が挙げられる。また、常温で液体である農薬原体としては、例えば、２−クロロ−２’，６’−ジエチル−Ｎ−（２−プロポキシエチル）−アセトアニリド（一般名：プレチラクロール）、Ｓ−ベンジル−Ｎ−（１，２−ジメチルプロピル）−Ｎ−エチルチオカルバマート（一般名：エスプロカルブ）等が挙げられる。 As an agrochemical raw material having a melting point of 70 ° C. or lower, for example, 2- (1,2-dimethylpropylamino) -4-ethylamino-6-methylthio-1,3,5-triazine (generic name: dimetamethrin, melting point) : 65 ° C.), S, S-dimethyl-2- (difluoromethyl) -4-isobutyl-6- (trifluoromethyl) -3,5-pyridinedicarbothionate (generic name: dithiopyr, melting point: 65 ° C.) 2,3-dihydro-3,3-dimethylbenzofuran-5-ylethanesulfonate (generic name: benfrate, melting point: 32-35 ° C.), butyl (R) -2- [4- (4-cyano-2 -Fluorophenoxy) phenoxy] propionate (generic name: cihalohop butyl, melting point: 50 ° C.), S-1-methyl-1-phenylethylpiperidine-1-carbothioa Doo (common name: dimepiperate, mp: 38.8 to 39.3 ° C.), and the like. Moreover, as an agrochemical raw material which is liquid at normal temperature, for example, 2-chloro-2 ′, 6′-diethyl-N- (2-propoxyethyl) -acetanilide (generic name: pretilachlor), S-benzyl-N— (1,2-Dimethylpropyl) -N-ethylthiocarbamate (generic name: Esprocarb) and the like.
７０℃以下の軟化点を有する農薬原体としては、例えば、１，１’−イミノジ（オクタメチレン）ジグアニジニウム＝トリス（アルキルベンゼンスルホナート）（一般名：イミノクタジンアルベシル酸塩、軟化点：５５〜６０℃）が挙げられる。 As an agrochemical base having a softening point of 70 ° C. or less, for example, 1,1′-iminodi (octamethylene) diguanidinium = tris (alkylbenzenesulfonate) (generic name: iminoctazine albesylate, softening point: 55-60) ° C).
本発明の農園芸用顆粒水和剤は７０℃を超える融点又は軟化点を有する農薬原体を含有しても構わない。かかる農薬原体としては、例えば、２−イソプロピルフェニル−Ｎ−メチルカルバマート（一般名：ＭＩＰＣ、融点：８８〜９３℃）、３，５−キシリル−Ｎ−メチルカルバマート（一般名：ＸＭＣ、融点：９９〜１００℃）、３−（４−ｔｅｒｔ−ブチル−２−エトキシフェニル）−２−（２，６−ジフルオロフェニル）−４，５−ジヒドロオキサゾール（一般名：エトキサゾール、融点：１０１〜１０２℃）Ｏ−３−ｔｅｒｔ−ブチルフェニル−６−メトキシ−２−ピリジル（メチル）チオカルバマート（一般名：ピリブチカルブ、融点：８５．７〜８６．２℃）、５−（２，４−ジクロロフェノキシ）−２−ニトロメチルベンゾアート（一般名：ビフェノックス、融点：８４〜８６℃）、１−（α，α−ジメチルベンジル）−３−（パラトリル）尿素（一般名：ダイムロン、融点：２０３℃）、Ｎ，Ｎ−ジエチル−３−メシチルスルホニル−１Ｈ−１，２，４−トリアゾール−１−カルボキサミド（一般名：カフェンストロール、融点：１１４〜１１６℃）、メチル−α−（４，６−ジメトキシピリミジン−２−イル）カルバモイルスルファモイル］−ｏ−トルアート（一般名：ベンスルフロンメチル、融点：１８５〜１８８℃）、２−ブロモ−Ｎ−（α，α−ジメチルベンジル）−３，３−ジメチルブタナミド（一般名：ブロモブチド、融点：１８０．１℃）、１−（２−クロロイミダゾ［１，２−ａ］ピリジン−３−イルスルホニル）−３−（４，６−ジメトキシピリジン−２−イル）尿素（一般名：イマゾスルフロン、融点：１８３〜１８４℃）、１−｛［Ｏ−（シクロプロピルカルボニル）フェニル］スルファモイル｝−３（４，６−ジメトキシ−２−ピリミジニル）−尿素（一般名：シクロスルファムロン、融点：１４９．６〜１５３．２℃）、メチル（Ｅ）−２−メトキシイミノ［α−（ｏ−トリルオキシ）ｏ−トリル］アセタート（一般名：クレソキシムメチル、融点：１０１．６〜１０２．５℃）、メチル（Ｅ）−２−［２−｛６−（２−シアノフェノキシ）ピリミジン−４−イルオキシ｝フェニル］−３−メトキシアクリラート（一般名：アゾキシストロビン、融点：１１６℃）、５−〔〔２−アミノ−５−Ｏ−（アミノカルボニル）−２−デオキシ−Ｌ−キシロニル〕アミノ〕−１，５−ジデオキシ−１−〔３，４−ジヒドロ−５−（ヒドロキシメチル）−２，４−ジオキソ−１（２Ｈ）−ピリミジル〕−β−Ｄ−アロフラヌロニック酸（一般名：ポリオキシン、融点：１６０℃以上）、ビス（ジメチルチオカルバモイル）ジスルフィド（一般名：チウラム、融点：１５５〜１５６℃）、Ｎ−（２，３−ジクロロ−４−ヒドロキシフェニル）−１−メチルシクロヘキサンカルボキサミド（一般名：フェンヘキサミド、融点：１５３℃）、亜鉛イオン配位マンガニーズエチレンビスジチオカルバマート（一般名：マンコゼブ、融点：１９２℃以上）、３−（３，５−ジクロロフェニル）−Ｎ−イソプロピル−２，４−ジオキソイミダゾリジン−１−カルボキサミド（一般名：イプロジオン、融点：１３４℃）、３’−イソプロポキシ−２−メチルベンズアニリド（一般名：メプロニル、融点：９２〜９３℃）（１ＲＳ，２ＳＲ，５ＳＲ；１ＲＳ，２ＳＲ，５ＳＲ）−２−（４−クロロベンジル）−５−イソプロピル−１−（１Ｈ−１，２，４−トリアゾール−１−イルメチル）シクロペンタノール（一般名：イプコナゾール、融点：９１〜１１９℃）等が挙げられる。 The granulated wettable powder for agricultural and horticultural use of the present invention may contain an agrochemical base having a melting point or softening point exceeding 70 ° C. Examples of the agrochemical substance include 2-isopropylphenyl-N-methylcarbamate (generic name: MIPC, melting point: 88-93 ° C.), 3,5-xylyl-N-methylcarbamate (generic name: XMC, Melting point: 99-100 ° C.), 3- (4-tert-butyl-2-ethoxyphenyl) -2- (2,6-difluorophenyl) -4,5-dihydrooxazole (generic name: etoxazole, melting point: 101- 102 ° C.) O-3-tert-butylphenyl-6-methoxy-2-pyridyl (methyl) thiocarbamate (generic name: pyributicalb, melting point: 85.7-86.2 ° C.), 5- (2,4- Dichlorophenoxy) -2-nitromethylbenzoate (generic name: biphenox, melting point: 84-86 ° C.), 1- (α, α-dimethylbenzyl) -3- (para Tolyl) Urea (generic name: Daimlon, melting point: 203 ° C.), N, N-diethyl-3-mesitylsulfonyl-1H-1,2,4-triazole-1-carboxamide (generic name: cavenstrol, melting point: 114- 116 ° C.), methyl-α- (4,6-dimethoxypyrimidin-2-yl) carbamoylsulfamoyl] -o-toluate (generic name: bensulfuron methyl, melting point: 185-188 ° C.), 2-bromo-N -(Α, α-dimethylbenzyl) -3,3-dimethylbutanamide (generic name: bromobutide, melting point: 180.1 ° C), 1- (2-chloroimidazo [1,2-a] pyridin-3-yl Sulfonyl) -3- (4,6-dimethoxypyridin-2-yl) urea (generic name: imazosulfuron, melting point: 183 to 184 ° C.), 1-{[O- (cyclopropyl Pyrylcarbonyl) phenyl] sulfamoyl} -3 (4,6-dimethoxy-2-pyrimidinyl) -urea (generic name: cyclosulfamuron, melting point: 149.6-153.2 ° C.), methyl (E) -2- Methoxyimino [α- (o-tolyloxy) o-tolyl] acetate (generic name: cresoxime methyl, melting point: 101.6-102.5 ° C.), methyl (E) -2- [2- {6- (2-cyano Phenoxy) pyrimidin-4-yloxy} phenyl] -3-methoxyacrylate (generic name: azoxystrobin, melting point: 116 ° C.), 5-[[2-amino-5-O- (aminocarbonyl) -2- Deoxy-L-xylonyl] amino] -1,5-dideoxy-1- [3,4-dihydro-5- (hydroxymethyl) -2,4-dioxo-1 (2H) -pyrimidi L] -β-D-Allofuranuronic acid (generic name: polyoxin, melting point: 160 ° C. or higher), bis (dimethylthiocarbamoyl) disulfide (generic name: thiuram, melting point: 155-156 ° C.), N- (2 , 3-Dichloro-4-hydroxyphenyl) -1-methylcyclohexanecarboxamide (generic name: phenhexamide, melting point: 153 ° C.), zinc ion coordinated Manganese ethylenebisdithiocarbamate (generic name: mancozeb, melting point: 192 ° C. or higher), 3- (3,5-dichlorophenyl) -N-isopropyl-2,4-dioxoimidazolidine-1-carboxamide (generic name: iprodione, melting point: 134 ° C.), 3′-isopropoxy-2- Methylbenzanilide (generic name: mepronil, melting point: 92-93 ° C.) (1RS, 2SR, 5SR; 1R , 2SR, 5SR) -2- (4-chlorobenzyl) -5-isopropyl-1- (1H-1,2,4-triazol-1-ylmethyl) cyclopentanol (generic name: ipconazole, melting point: 91-119) ° C) and the like.
［Ｎ−アシルアミノ酸塩］
本発明の農園芸用顆粒水和剤に用いるＮ−アシルアミノ酸塩は、アミノ酸を主原料として合成されるアニオン界面活性剤であり、顆粒水和剤の分散剤として用いられる。Ｎ−アシルアミノ酸塩のアシル基は、炭素原子数８〜２４のものが好ましく、そのようなアシル基としては、例えば、ラウロイル基、ミリストイル基、ステアロイル基等が挙げられる。
[N-acyl amino acid salt]
The N-acyl amino acid salt used in the agricultural and horticultural granule wettable powder of the present invention is an anionic surfactant synthesized using an amino acid as a main raw material, and is used as a dispersant for the granule wettable powder. The acyl group of the N-acyl amino acid salt preferably has 8 to 24 carbon atoms, and examples of such an acyl group include a lauroyl group, a myristoyl group, a stearoyl group, and the like.
Ｎ−アシルアミノ酸塩のアミノ酸としては、例えば、グリシン、サルコシン、アラニン、バリン、ロイシン、リジン、アルギニン、グルタミン酸、アスパラギン酸、メチオニン、シスチン、システイン、フェニルアラニンなどが挙げられ、それらの塩としては生理学的に許容される塩、具体的には、ナトリウム、カリウム、リチウム等のアルカリ金属塩、マダネシウム、カルシウム等のアルカリ土類金属塩、塩酸、硫酸等の酸塩、アンモニア、トリエタノールアミン、トリエチルアミン等のアミン塩類が挙げられる。 Examples of the amino acid of the N-acyl amino acid salt include glycine, sarcosine, alanine, valine, leucine, lysine, arginine, glutamic acid, aspartic acid, methionine, cystine, cysteine, and phenylalanine. Salts, specifically, alkali metal salts such as sodium, potassium and lithium, alkaline earth metal salts such as madanesium and calcium, acid salts such as hydrochloric acid and sulfuric acid, ammonia, triethanolamine, triethylamine and the like Examples include amine salts.
Ｎ−アシルアミノ酸塩の具体例とその市販品としては、例えば、味の素株式会社製の商品名「アミソフトＨＳ−１１」（Ｎ−ステアロイル−Ｌ−グルタミン酸ナトリウム）、「アミソフトＨＳ−２１」（Ｎ−ステアロイル−Ｌ−グルタミン酸二ナトリウム）、「アミソフトＣＳ−１１」（Ｎ−ヤシ油脂肪酸アシル−Ｌ−グルタミン酸ナトリウム）、「アミソフトＬＳ−１１」（Ｎ−ラウロイル−Ｌ−グルタミン酸ナトリウム）、「アミソフトＭＳ−１１」（Ｎ−ミリストイル−Ｌ−グルタミン酸ナトリウム）、川研ファインケミカル株式会社製の商品名「ソイポンＳＬＰ」（ラウロイルサルコシンナトリウム）及び「アラノンＡＭＰ」（Ｎ−ミリストイル−Ｎ−メチル−β−アラニンナトリウム）等が挙げられる。これらのＮ−アシルアミノ酸塩は、単独で用いることも２種類以上を組み合わせて用いることもできる。 Specific examples of N-acylamino acid salts and commercially available products thereof include, for example, trade names “Amisoft HS-11” (N-stearoyl-L-glutamate sodium), “Amisoft HS-21” (N— Stearoyl-L-glutamate disodium), “Amisoft CS-11” (N-coconut oil fatty acid acyl-L-glutamate sodium), “Amisoft LS-11” (N-lauroyl-L-glutamate sodium), “Amisoft MS- 11 ”(sodium N-myristoyl-L-glutamate), trade names“ Soipon SLP ”(lauroyl sarcosine sodium) and“ alanone AMP ”(sodium N-myristoyl-N-methyl-β-alanine) manufactured by Kawaken Fine Chemical Co., Ltd. Etc. These N-acyl amino acid salts can be used alone or in combination of two or more.
これらの中でも、良好な崩壊性と分散性を付与できることから、味の素株式会社製の商品名「アミソフトＨＳ−１１」（Ｎ−ステアロイル−Ｌ−グルタミン酸ナトリウム）、「アミソフトＨＳ−２１」（Ｎ−ステアロイル−Ｌ−グルタミン酸二ナトリウム）、「アミソフトＣＳ−１１」（Ｎ−ヤシ油脂肪酸アシル−Ｌ−グルタミン酸ナトリウム）及び川研ファインケミカル株式会社製の商品名「ソイポンＳＬＰ」（ラウロイルサルコシンナトリウム）が特に好ましい。 Among these, since good disintegration and dispersibility can be imparted, trade names “Amisoft HS-11” (N-stearoyl-L-glutamate sodium), “Amisoft HS-21” (N-stearoyl) manufactured by Ajinomoto Co., Inc. -L-glutamate disodium), "Amisoft CS-11" (N-coconut oil fatty acid acyl-L-glutamate sodium) and trade name "Soipon SLP" (lauroyl sarcosine sodium) manufactured by Kawaken Fine Chemical Co., Ltd. are particularly preferred.
［吸着担体］
また、本発明の農園芸用顆粒水和剤に用いる吸着担体は、吸収油量が多い鉱物質微粉が好ましい。そのような鉱物質微粉末からなる吸着単体としては、例えば、合成非晶質シリカ、珪藻土、ゼオライト、アタパルジャイト、酸性白土等が挙げられるが、特にこれらに限定されない。農薬原体をこれら吸着担体に吸収または吸着させるか、吸着担体と混合して使用する。また、農薬原体を有機溶剤に溶かして吸着担体に吸着させても良い。
[Adsorption carrier]
Moreover, the adsorption carrier used for the granulated wettable powder for agricultural and horticultural use of the present invention is preferably a fine mineral powder with a large amount of absorbed oil. Examples of the adsorbing simple substance composed of such mineral fine powder include, but are not limited to, synthetic amorphous silica, diatomaceous earth, zeolite, attapulgite, and acid clay. The agrochemical substance is absorbed or adsorbed on these adsorbent carriers, or mixed with an adsorbent carrier. Alternatively, the agrochemical raw material may be dissolved in an organic solvent and adsorbed on an adsorption carrier.
吸着単体として用いる合成非晶質シリカは、含水珪酸、湿式シリカまたは合成珪酸などと呼ばれ、Ｓｉ−Ｏの網目構造から成り一定の結晶構造を持たないものである。合成非晶質シリカの市販品としては、例えば、塩野義製薬株式会社製の商品名「カープレックス＃８０」、「カープレックスＸＲ」、「カープレックスＦＰＳ−３」、「カープレックスＣＳ−８」（合成非晶質シリカ焼成品）、「カープレックスＢＳ−３０４」（合成非晶質シリカ、ゲルタイプ）、日本シリカ工業株式会社製の商品名「ニップシールＮＳ−Ｋ」、「ニップシールＮＳ−ＫＲ」、株式会社トクヤマ製の商品名「トクシールＮＳＫ」、「トクシールＰ」、などが挙げられる。 Synthetic amorphous silica used as a single adsorbent is called hydrous silicic acid, wet silica, or synthetic silicic acid, and has a Si—O network structure and does not have a certain crystal structure. Examples of commercially available synthetic amorphous silica include trade names “Carplex # 80”, “Carplex XR”, “Carplex FPS-3” and “Carplex CS-8” manufactured by Shionogi & Co., Ltd. (Synthetic amorphous silica calcined product), “Carplex BS-304” (synthetic amorphous silica, gel type), trade names “Nip Seal NS-K”, “Nip Seal NS-KR” manufactured by Nippon Silica Kogyo Co., Ltd. And trade names “Tokuseal NSK” and “Tokuseal P” manufactured by Tokuyama Corporation.
吸着単体として用いる珪藻土は、単細胞の藻類である珪藻が海底・湖底に堆積し体内の原形質が分解して珪酸を主体とした遺殻が地層を形成した軽質岩石または土壌で、円形、針状、舟形などの多孔質な殻の集合体よりなり、通常８０％以上の珪酸分（ＳｉＯ２）を含み、大部分は非晶質珪酸から成る。吸着担体として用いる珪藻土には、特に限定がないが、その市販品としては、例えば、白山工業株式会社製の商品名「ゼムライト３Ｙ」や昭和化学工業株式会社製の商品名「ラヂオライト」等が挙げられる。 Diatomaceous earth used as a simple substance is light rock or soil in which diatoms, which are single-celled algae, are deposited on the bottom of the sea and lake, and the protoplasm in the body decomposes to form a crustal layer of siliceous husks. It consists of an aggregate of porous shells such as boats, and usually contains 80% or more of silicic acid (SiO 2 ), and most consists of amorphous silicic acid. The diatomaceous earth used as the adsorption carrier is not particularly limited, but examples of commercially available products include the trade name “Zemlite 3Y” manufactured by Hakusan Kogyo Co., Ltd. and the trade name “Radiolite” manufactured by Showa Chemical Industry Co., Ltd. Can be mentioned.
吸着単体として用いるゼオライトは、アルカリおよびアルカリ土類金属の含水アルミノ珪酸塩で、結晶中に微細な細孔を有するものである。吸着担体として用いるゼオライトには、特に限定がないが、その市販品としては、例えば、日東粉化工業株式会社製の商品名「日東ゼオライト＃１５０」やカサネン工業株式会社製の商品名「出雲ゼオライト」、などが挙げられる。 Zeolite used as an adsorbent alone is a hydrous aluminosilicate of alkali and alkaline earth metals, and has fine pores in the crystal. There are no particular limitations on the zeolite used as the adsorption carrier, but examples of commercially available products include the product name “Nitto Zeolite # 150” manufactured by Nitto Flour Chemical Co., Ltd. and the product name “Izumo Zeolite” manufactured by Kasanen Industry Co., Ltd. ", Etc.
吸着単体として用いるアタパルジャイトは、含水マグネシウム・アルミニウム珪酸塩鉱物であり、吸着担体として用いるアタパルジャイトには、特に限定がないが、その市販品としては、例えば、エンゲルハード社製の商品名「マイクロソーブ３００ＬＶＭ」や「マイクロソーブ３００ＲＶＭ」、などが挙げられる。 The attapulgite used as the adsorption simple substance is a hydrous magnesium / aluminum silicate mineral, and the attapulgite used as the adsorption carrier is not particularly limited, but as a commercially available product, for example, trade name “Microsorb 300 LVM” manufactured by Engelhard Inc. And “Microsorb 300RVM”.
吸着単体として用いる酸性白土には、特に限定がないが、その市販品としては、例えば、水澤化学工業株式会社製の商品名「ミズカエース＃２００」、などが挙げられる。また、モンモリロナイトを主成分とする粘土鉱物である活性白土も、本発明の農園芸用顆粒水和剤の吸着単体として、特に限定なく使用することができる。 Although there is no limitation in particular in the acidic clay used as an adsorption | suction simple substance, As a commercial item, the brand name "Mizuka Ace # 200" by Mizusawa Chemical Industry Co., Ltd. etc. are mentioned, for example. Moreover, the activated clay which is a clay mineral which has a montmorillonite as a main component can also be used as an adsorption | suction simple substance of the granule wettable powder for agriculture and horticulture of this invention without a limitation.
これら鉱物質微粉末の中でも、入手が容易なことから、合成非晶質シリカと珪藻土が吸着担体として特に好ましく用いられる。 Among these mineral fine powders, synthetic amorphous silica and diatomaceous earth are particularly preferably used as the adsorption carrier because they are easily available.
［芳香族スルホン酸塩のホルマリン縮合物とリグニンスルホン酸塩］
本発明の農園芸用顆粒水和剤の水和性をさらに向上させる目的で、湿潤剤として、芳香族スルホン酸塩のホルマリン縮合物とリグニンスルホン酸塩の少なくとも１種を含有させることが好ましい。これらの湿潤剤は、単独で用いることも、複数を組み合わせて用いることもできる。
[Formalin condensate of aromatic sulfonate and lignin sulfonate]
For the purpose of further improving the hydrating property of the granulated wettable powder for agriculture and horticulture of the present invention, it is preferable to contain at least one of a formalin condensate of an aromatic sulfonate and a lignin sulfonate as a wetting agent. These wetting agents can be used alone or in combination.
本発明の農園芸用顆粒水和剤に使用できる芳香族スルホン酸塩のホルマリン縮合物には、特に限定がないが、その市販品としては、例えば、花王株式会社製の商品名「デモールＳＮＢ」（芳香族スルホン酸ナトリウムホルマリン縮合物）、「デモールＭＳ」（芳香族スルホン酸ナトリウムホルマリン縮合物）、「デモールＮ」（ナフタレンスルホン酸ナトリウムホルマリン縮合物）、「デモールＲＮ」（ナフタレンスルホン酸ナトリウムホルマリン縮合物）及び「デモールＴ」（ナフタレンスルホン酸ナトリウムホルマリン縮合物）、ローディア日華株式会社製の商品名「スープラジルＮＭＳ／９０」（メチルナフタレンスルホン酸ナトリウムホルマリン縮合物）や「スープラジルＲＭ／２１０−ＥＩ」（アルキルナフタレンスルホンナトリウム塩ホルマリン縮合物）、竹本油脂株式会社製の商品名「ニューカルゲンＰＳ−Ｐ」（アルキルナフタレンスルホン酸ナトリウムホルマリン縮合物）、「ニューカルゲン２０７」（ナフタレンスルホン酸ナトリウムホルマリン縮合物）及び「ニューカルゲンＷＧ−２」（ナフタレンスルホン酸ナトリウムホルマリン縮合物）、東邦化学工業株式会社製の商品名「ルノックス１０００Ｃ」（ナフタレンスルホン酸ナトリウムホルマリン縮合物）、日本乳化剤株式会社製の商品名「ディスロールＳＨ」（ナフタレンスルホン酸ナトリウムホルマリン縮合物）、第一工業製薬株式会社製の商品名「ラベリンＦＡ」（ナフタレンスルホン酸ナトリウムホルマリン縮合物）や「ラベリンＦＷ」（ナフタレンスルホン酸ナトリウムホルマリン縮合物）、などが挙げられる。 There is no particular limitation on the aromatic sulfonate formalin condensate that can be used in the granulated wettable powder for agriculture and horticulture of the present invention, but as a commercial product, for example, trade name “Demol SNB” manufactured by Kao Corporation. (Aromatic sulfonic acid sodium formalin condensate), “Demol MS” (Aromatic sulfonic acid sodium formalin condensate), “Demol N” (Naphthalene sodium sulfonate formalin condensate), “Demol RN” (Naphthalene sulfonic acid sodium formalin condensate) Condensate) and “Demol T” (Naphthalenesulfonate sodium formalin condensate), Rhodia Nikka Co., Ltd. trade name “Souprazil NMS / 90” (Sodium Formaldehyde sodium naphthalenesulfonate formalin condensate) and “Suprasil RM / 210-EI "(alkyl naphthalene sulfone sodium Salt formaldehyde condensate), trade names “New Calgen PS-P” (sodium alkyl naphthalene sulfonate formalin condensate), “New Calgen 207” (sodium naphthalene sulfonate formalin condensate) and “New” “Calgen WG-2” (Naphthalenesulfonate sodium formalin condensate), trade name “LUNOX 1000C” (Naphthalenesulfonate sodium formalin condensate) manufactured by Toho Chemical Industry Co., Ltd., trade name “DISROLL SH” manufactured by Nippon Emulsifier Co., Ltd. "(Naphthalene sulfonate sodium formalin condensate), trade name" Labelin FA "(Naphthalene sulfonate sodium formalin condensate) and" Labelin FW "(Naphthalene sulfonate sodium formalin condensate) manufactured by Daiichi Kogyo Seiyaku Co., Ltd., Etc., and the like.
本発明の顆粒水和剤に使用できるリグニンスルホン酸塩の市販品としては、例えば、日本製紙株式会社製の商品名「サンエキスＰ２５２」（リグニンスルホン酸ナトリウム）、「サンエキスＰ２０１」（リグニンスルホン酸カルシウム）、「バニレックスＮ」（部分脱スルホンリグニンスルホン酸ナトリウム）、「バニレックスＲＮ」（部分脱スルホンリグニンスルホン酸ナトリウム）、「パールレックスＮＰ」（高分子量リグニンスルホン酸ナトリウム）、「パールレックスＤＰ」（変性リグニンスルホン酸ナトリウム）、竹本油脂株式会社製の商品名「ニューカルゲンＲＸ−Ｂ」（リグニンスルホン酸ナトリウム）、「ニューカルゲンＲＸ−Ｃ」（リグニンスルホン酸ナトリウム）、「ニューカルゲンＷＧ−４」（リグニンスルホン酸ナトリウム）、東邦化学工業株式会社製の商品名「ソルポール９０４７Ｋ」（リグニンスルホン酸ナトリウム）、ローディア日華株式会社製の商品名「スープラジルＬ／３９３」（リグニンスルホン酸カルシウム）、などが挙げられる。 Examples of commercially available lignin sulfonates that can be used in the granular wettable powder of the present invention include trade names “Sun Extract P252” (sodium lignin sulfonate) and “Sun Extract P201” (lignin sulfone) manufactured by Nippon Paper Industries Co., Ltd. Calcium Acid), “Vanilex N” (partially desulfonated lignin sulfonate sodium), “Vanilex RN” (partially desulfonated lignin sulfonate sodium), “Pearl Rex NP” (high molecular weight sodium lignin sulfonate), “Pearl Rex DP ”(Modified lignin sulfonate sodium), trade names“ New Calgen RX-B ”(sodium lignin sulfonate),“ New Calgen RX-C ”(sodium lignin sulfonate),“ New Calgen WG- ”manufactured by Takemoto Yushi Co., Ltd. 4 "(lignin sulfonic acid sodium Lium), trade name “Solpol 9047K” (sodium lignin sulfonate) manufactured by Toho Chemical Co., Ltd., trade name “Soprasil L / 393” (calcium lignin sulfonate) manufactured by Rhodia Nikka Co., Ltd. .
［Ｎ−アシルメチルタウリン酸塩］
本発明の農園芸用顆粒水和剤を使用する際に展開液として水を用いるが、かかる水がＣａイオンやＭｇイオンなどを多く含有する水、所謂硬水であった場合、かかるイオンの影響により該顆粒水和物の分散性が低下する危険性がある。本発明の農園芸用顆粒水和剤にＮ−アシルメチルタウリン酸塩を併用することにより、前記問題を解決することができる。
[N-acylmethyl taurate]
When using the granulating wettable powder for agricultural and horticultural use of the present invention, water is used as a developing solution. When such water is water containing a large amount of Ca ions, Mg ions, etc., so-called hard water, There is a risk that the dispersibility of the granule hydrate is lowered. The above-mentioned problem can be solved by using N-acylmethyl taurate in combination with the granulated wettable powder for agriculture and horticulture of the present invention.
Ｎ−アシルメチルタウリン酸塩は、人や動物の胆汁中に存在する生体内界面活性剤であるタウロコール酸と非常に類似した構造を有し、低刺激性で安全性が高いアニオン界面活性剤であり、従来から、代表的なものがシャンプー基剤、クリーム等に用いられている。かかる本発明のＮ−アシルメチルタウリン酸塩を含有する農園芸用顆粒水和物は、ＣａやＭｇを多量に含有する硬水に分散させた場合、多量のＣａイオンなどの影響を受けることなく、水中で優れた崩壊性及び分散性を示す。 N-acylmethyl taurate is an anionic surfactant that has a structure very similar to that of taurocholic acid, an in vivo surfactant present in human and animal bile, and is mild and safe. Conventionally, representative ones have been used for shampoo bases, creams and the like. Such a granulated hydrate for agricultural and horticultural use containing the N-acylmethyl taurate of the present invention, when dispersed in hard water containing a large amount of Ca or Mg, without being affected by a large amount of Ca ions, Excellent disintegration and dispersibility in water.
Ｎ−アシルメチルタウリン酸塩のアシル基は、炭素原子数８〜２４のアシル基が好ましく、そのようなアシル基としては、例えば、ラウロイル基、ミリストイル基、ステアロイル基、などが挙げられる。 The acyl group of N-acylmethyl taurate is preferably an acyl group having 8 to 24 carbon atoms, and examples of such an acyl group include a lauroyl group, a myristoyl group, and a stearoyl group.
また、Ｎ−アシルメチルタウリン酸塩の塩としては、生理学的に許容される塩、具体的には、ナトリウム、カリウム、リチウムの如きアルカリ金属塩、マダネシウム、カルシウムの如きアルカリ土類金属塩、塩酸、硫酸の如き無機酸塩、アンモニア、トリエタノールアミン、トリエチルアミンの如きアミン塩、などが挙げられる。 The N-acylmethyl taurate salt includes physiologically acceptable salts, specifically, alkali metal salts such as sodium, potassium and lithium, alkaline earth metal salts such as madanesium and calcium, hydrochloric acid. And inorganic acid salts such as sulfuric acid, and amine salts such as ammonia, triethanolamine, and triethylamine.
Ｎ−アシルメチルタウリン酸の具体例とその市販品としては、例えば、日光ケミカルズ株式会社製の商品名「ＮＩＫＫＯＬ ＬＭＴ」（Ｎ−ラウロイルメチルタウリン酸ナトリウム）、「ＮＩＫＫＯＬ ＭＭＴ」（Ｎ−ミリストイルメチルタウリン酸ナトリウム）、「ＮＩＫＫＯＬ ＰＭＴ」（Ｎ−パルミトイルメチルタウリン酸ナトリウム）、「ＮＩＫＫＯＬ ＳＭＴ」（Ｎ−ステアロイルメチルタウリン酸ナトリウム）、「ＮＩＫＫＯＬ ＣＭＴ−３０」（Ｎ−ヤシ油脂肪酸メチルタウリン酸ナトリウム）、松本油脂製薬株式会社製の商品名「マーポンＴ」（Ｎ−オレイルメチルタウリン酸ナトリウム）、ライオン株式会社製「リポタックＴＥ」（Ｎ−ステアロイルメチルタウリン酸ナトリウム）、日本油脂株式会社製「ダイヤポンＫ−ＭＧ」（Ｎ−ヤシ油脂肪酸メチルタウリン酸マグネシウム）、「ダイヤポンＫ−ＳＦ」（Ｎ−ヤシ油脂肪酸メチルタウリン酸ナトリウム）、などが挙げられる。これらのＮ−アシルメチルタウリン酸塩は、単独で用いることも、複数種組み合わせて用いることもできる。 Specific examples of N-acylmethyl tauric acid and its commercial products include, for example, trade names “NIKKOL LMT” (sodium N-lauroylmethyl taurate) and “NIKKOL MMT” (N-myristoyl methyl taurine) manufactured by Nikko Chemicals Corporation. Acid sodium), "NIKKOL PMT" (sodium N-palmitoylmethyl taurate), "NIKKOL SMT" (sodium N-stearoylmethyl taurate), "NIKKOL CMT-30" (sodium N-coconut oil fatty acid methyl taurate), Trade name “Marpon T” (N-oleylmethyl taurate sodium) manufactured by Matsumoto Yushi Seiyaku Co., Ltd., “Lipotack TE” (sodium N-stearoylmethyl taurate) manufactured by Lion Corporation, “Diapon K-” manufactured by Nippon Oil & Fats Co., Ltd. MG “(N-coconut oil fatty acid methyl taurate magnesium)”, “Diapon K-SF” (N-coconut oil fatty acid methyl taurate sodium), and the like. These N-acylmethyl taurates can be used alone or in combination.
本発明の農園芸用顆粒水和剤を構成する各成分の配合割合は、農薬原体が１０〜６０質量％、より好ましくは２０〜５０質量％、Ｎ−アシルアミノ酸が１０〜３０質量％、より好ましくは２０〜３０質量％、及び吸着担体が１０〜８０質量％、より好ましくは２０〜６０質量％である。 The blending ratio of each component constituting the granulating wettable powder for agricultural and horticultural use of the present invention is 10 to 60% by mass of the pesticide active ingredient, more preferably 20 to 50% by mass, 10 to 30% by mass of N-acylamino acid, More preferably, it is 20-30 mass%, and an adsorption carrier is 10-80 mass%, More preferably, it is 20-60 mass%.
また、本発明の農園芸用顆粒水和剤に芳香族ホルマリン縮合物とリグニンスルホン酸塩との少なくとも１種を更に配合する場合、芳香族ホルマリン縮合物及びリグニンスルホン酸塩の配合割合は、前記農薬原体、前記Ｎ−アシルアミノ酸、前記吸着担体、前記芳香族スルホン酸塩のホルマリン縮合物及びリグニンスルホン酸塩の合計質量の５〜２５質量％が好ましい。 Further, when further blending at least one of an aromatic formalin condensate and a lignin sulfonate in the agricultural and horticultural granule wettable powder of the present invention, the blending ratio of the aromatic formalin condensate and the lignin sulfonate is as described above. 5-25 mass% of the total mass of an agrochemical raw material, the said N-acylamino acid, the said adsorption carrier, the formalin condensate of the said aromatic sulfonate, and a lignin sulfonate is preferable.
具体的には、農薬原体が１０〜５５質量％、より好ましくは２０〜５０質量％、Ｎ−アシルアミノ酸が５〜２０質量％、より好ましくは１０〜１５質量％、吸着担体が５〜８０質量％、より好ましくは２０〜６０質量％、芳香族ホルマリン縮合物及びリグニンスルホン酸塩が５〜２５質量％、より好ましくは１０〜２０質量％である。 Specifically, the agrochemical base is 10 to 55% by mass, more preferably 20 to 50% by mass, the N-acylamino acid is 5 to 20% by mass, more preferably 10 to 15% by mass, and the adsorption carrier is 5 to 80%. The mass%, more preferably 20 to 60 mass%, the aromatic formalin condensate and the lignin sulfonate are 5 to 25 mass%, more preferably 10 to 20 mass%.
本発明の農園芸用顆粒水和剤にさらにＮ−アシルメチルタウリン酸塩を併用する場合、Ｎ−アシルメチルタウリン酸塩の配合割合は、前記農薬原体、前記Ｎ−アシルアミノ酸、前記吸着担体、前記芳香族スルホン酸塩のホルマリン縮合物及びリグニンスルホン酸塩、及び前記Ｎ−アシルタウリン酸塩の合計質量の０．５〜１０質量％が好ましい。 When N-acylmethyl taurate is further used in combination with the agricultural and horticultural granule wettable powder of the present invention, the blending ratio of N-acylmethyl taurate is determined based on the agrochemical substance, the N-acyl amino acid, and the adsorption carrier. The aromatic sulfonate formalin condensate and lignin sulfonate, and the total mass of the N-acyl taurate are preferably 0.5 to 10% by mass.
具体的には、農薬原体が１０〜５５質量％、より好ましくは２０〜５０質量％、Ｎ−アシルアミノ酸が５〜２０質量％、より好ましくは１０〜１５質量％、吸着担体が５〜７９．５質量％、より好ましくは２０〜５９質量％、芳香族ホルマリン縮合物及びリグニンスルホン酸塩が５〜２５質量％、より好ましくは１０〜２０質量％、Ｎ−アシルメチルタウリン酸塩０．５〜１０質量％、好ましくは１〜５質量％である。 Specifically, the agrochemical base is 10 to 55% by mass, more preferably 20 to 50% by mass, the N-acylamino acid is 5 to 20% by mass, more preferably 10 to 15% by mass, and the adsorption carrier is 5 to 79%. 0.5 mass%, more preferably 20-59 mass%, aromatic formalin condensate and lignin sulfonate 5-25 mass%, more preferably 10-20 mass%, N-acylmethyl taurate 0.5 -10 mass%, preferably 1-5 mass%.
本発明の農園芸用顆粒水和剤には、更に必要に応じて、上記以外の湿潤剤、増量剤、結合剤を含有させることもできる。その場合、上記の構成成分の配合割合は上記の範囲内に維持するのが好ましい。 The granulating wettable powder for agricultural and horticultural use according to the present invention may further contain a wetting agent, a bulking agent, and a binder other than those described above, if necessary. In that case, it is preferable to maintain the blending ratio of the above components within the above range.
上記以外の湿潤剤としては、例えば、アルキルナフタレンスルホン酸ナトリウム、アルキル硫酸ナトリウム、アルキルベンゼンスルホン酸ナトリウム、アルキルスルホコハク酸ナトリウム、ポリオキシエチレンアルキルアリールエーテル、などが挙げられる。 Examples of the wetting agent other than the above include sodium alkylnaphthalene sulfonate, sodium alkyl sulfate, sodium alkylbenzene sulfonate, sodium alkylsulfosuccinate, polyoxyethylene alkylaryl ether, and the like.
増量剤としては、例えば、雲母、炭酸カルシウム、カオリンクレー、クレー、ベントナイト、酸性白土、タルク、炭酸マグネシウム、二酸化チタン、ブドウ糖、乳糖、ショ糖、硫酸アンモニウム、硫酸ナトリウム、尿素、などが挙げられる。 Examples of the bulking agent include mica, calcium carbonate, kaolin clay, clay, bentonite, acid clay, talc, magnesium carbonate, titanium dioxide, glucose, lactose, sucrose, ammonium sulfate, sodium sulfate, urea, and the like.
また、結合剤としては、例えば、カルボキシメチルセルロース、ポリビニルアルコール、ポリビニルピロリドン、デキストリン、可溶性デンプン、などが挙げられる。 Examples of the binder include carboxymethyl cellulose, polyvinyl alcohol, polyvinyl pyrrolidone, dextrin, and soluble starch.
本発明の農園芸用顆粒水和剤は、通常、所謂軟水に分散させた後、薬剤散布に供されるが、地域によっては前記のような硬水に分散される。かかる硬水としては、例えばＣＩＰＡＣ（Collaborative International Pesticide Analytical Council；国際農薬分析法協議会）法で謂うCIPAC 標準水Ｄ（342ppm（Ｃａ２＋：Ｍｇ２＋＝４：１））を挙げることができる。 The granulated wettable powder for agricultural and horticultural use of the present invention is usually dispersed in so-called soft water and then used for chemical spraying, but depending on the region, it is dispersed in hard water as described above. Examples of such hard water include CIPAC standard water D (342 ppm (Ca 2+ : Mg 2+ = 4: 1)), which is a CIPAC (Collaborative International Pesticide Analytical Council) method.
本発明の農園芸用顆粒水和剤の形状は、特に制限される訳ではないが、球形、円柱形、不定形であって、その大きさは、好ましくは、最大長部分で０．１〜５mmのものである。 The shape of the granulating wettable powder for agricultural and horticultural use of the present invention is not particularly limited, but it is spherical, cylindrical, or indeterminate, and its size is preferably 0.1 to the maximum length portion. It is 5mm.
［顆粒水和剤の製造方法］
本発明の顆粒水和剤は、例えば、下記の製法で製造できるが、特にこれらに限定されるものではない。
[Production method of granule wettable powder]
Although the granule wettable powder of this invention can be manufactured with the following manufacturing method, for example, it is not specifically limited to these.
［７０℃以下の融点を有する農薬原体を用いる顆粒水和剤の製造方法］
７０℃以下の融点を有する農薬原体を用いる場合は、該農薬原体を融点以上に加熱して液状化した該農薬原体と吸着担体とを、あるいは、該農薬原体を揮発性の溶媒或いは不揮発性の溶媒に溶解させた溶液と吸着担体とを、例えば、リボンミキサー、ナウタミキサー、混合造粒機等の混合機を用いて混合して、農薬原体を吸着担体に吸着させた粉末状の混合物を作製する。その際に、揮発性の溶媒を使用した場合は、混合造粒機等の混合機で混合した後、加温して溶媒を除去し、粉末状の混合物を調製する。
[Method for producing granular wettable powder using agrochemical bulk having melting point of 70 ° C. or lower]
When using a pesticide raw material having a melting point of 70 ° C. or lower, the pesticide raw material and the adsorbent which are liquefied by heating the pesticide raw material to the melting point or higher, or the pesticide raw material is volatile solvent Alternatively, a solution in which a solution dissolved in a non-volatile solvent and an adsorption carrier are mixed using, for example, a mixer such as a ribbon mixer, a nauta mixer, or a mixing granulator to adsorb the agrochemical substance to the adsorption carrier. To make a mixture. At that time, when a volatile solvent is used, after mixing with a mixer such as a mixing granulator, the solvent is removed by heating to prepare a powdery mixture.
揮発性の溶媒は、農薬原体を溶解または均一に混合し、更に加熱により除去できるものが望ましく、そのような揮発性の溶媒としては、例えば、メタノール、エタノールの如き低級アルコール、アセトン、メチルエチルケトンの如き低級ケトンが挙げられる。また、不揮発性の溶媒としては、芳香族系炭化水素、ケトン類、脂肪酸エステル類、フタル酸エステル類、植物油、などが挙げられる。 The volatile solvent is preferably one in which the agrochemical substance is dissolved or homogeneously mixed and further removed by heating. Examples of such a volatile solvent include lower alcohols such as methanol and ethanol, acetone, and methyl ethyl ketone. And lower ketones. Nonvolatile solvents include aromatic hydrocarbons, ketones, fatty acid esters, phthalic acid esters, vegetable oils, and the like.
また、常温で液体である農薬原体あるいは農薬原体を不揮発性の溶媒に溶解させた溶液を用いて顆粒水和剤を製造する場合は、該農薬原体あるいはその溶液と吸着担体とを、例えば、リボンミキサー、ナウタミキサー、混合造粒機等の混合機で混合して、農薬原体を吸着担体に吸着させた粉末状の混合物を調製する。 In addition, when producing a wettable granule using a pesticide active ingredient that is liquid at room temperature or a solution obtained by dissolving a pesticide active ingredient in a non-volatile solvent, the pesticide active ingredient or a solution thereof and an adsorption carrier For example, it mixes with mixers, such as a ribbon mixer, a Nauta mixer, a mixing granulator, and prepares the powdery mixture which adsorb | sucked the agrochemical raw material to the adsorption carrier.
次に、得られた粉末状の混合物を、ピンミル、ハンマーミル、ボールミル、ジェットミル等の乾式粉砕機を用いて粉砕して得られる粉砕物に、Ｎ−アシルアミノ酸塩および必要に応じて、湿潤剤、その他の添加剤を加え、前記した混合機を用いて混合する。得られた混合物に加水し、混練、造粒し、次いで乾燥させることにより顆粒水和剤を製造する。尚、農薬原体および吸着担体以外の成分の一部または全部を前記粉砕前に農薬原体と吸着担体の混合物として予め混合しておいてもよい。 Next, the obtained powdery mixture is pulverized using a dry pulverizer such as a pin mill, hammer mill, ball mill, jet mill or the like into a pulverized product, and the N-acyl amino acid salt and, if necessary, wet. Agents and other additives are added and mixed using the mixer described above. The resulting mixture is hydrated, kneaded, granulated and then dried to produce a granular wettable powder. In addition, some or all of the components other than the pesticide raw material and the adsorption carrier may be mixed in advance as a mixture of the pesticide raw material and the adsorption carrier before the pulverization.
［７０℃以下の軟化点を有する農薬原体を用いる顆粒水和剤の製造方法］
７０℃以下の軟化点を有する農薬原体を用いて顆粒水和剤を製造する場合は、該農薬原体と吸着担体とを、あるいは該農薬原体を上記の揮発性の溶媒或いは上記の不揮発性の溶媒に溶解させた溶液と吸着担体とを、例えば、リボンミキサー、ナウタミキサー、混合造粒機等の混合機を用いて混合して、該溶液を吸着担体に吸着させた粉末状の混合物を作製する。その際に揮発性の溶媒を使用した場合は、混合造粒機等の混合機を用いて混合した後、加温して溶媒を除去し、粉末状の混合物を作製する。また、不揮発性の溶媒を用いる場合には、農薬原体を吸着した吸着担体が塊状か粉末状となるように使用される。その後、該混合物をピンミル、ハンマーミル、ボールミル、ジェットミル等の乾式粉砕機を用いて粉砕する。得られた粉砕物にＮ−アシルアミノ酸塩及び必要に応じて湿潤剤、その他の添加剤を加えて前記混合機を用いて混合する。得られた混合物に、上述の製造方法と同様に加水し、混練、造粒し、次いで乾燥させることにより顆粒水和剤を製造する。その際の造粒方法としては、押出造粒、転動造粒、混合造粒、流動層造粒、噴霧乾燥造粒、圧縮造粒等が挙げられる。
[Method for producing granular wettable powder using agrochemical raw material having a softening point of 70 ° C. or lower]
In the case of producing a granulated wettable powder using an agrochemical base having a softening point of 70 ° C. or less, the agrochemical base and the adsorption carrier, or the agrochemical base is mixed with the above volatile solvent or the above non-volatile. A powdery mixture in which a solution dissolved in a soluble solvent and an adsorption carrier are mixed using, for example, a mixer such as a ribbon mixer, a nauta mixer, or a mixing granulator, and the solution is adsorbed on the adsorption carrier. Is made. In this case, when a volatile solvent is used, the mixture is mixed using a mixer such as a mixing granulator, and then heated to remove the solvent to prepare a powdery mixture. Moreover, when using a non-volatile solvent, it is used so that the adsorption carrier which adsorb | sucked the agrochemical raw material may become a block shape or a powder form. Thereafter, the mixture is pulverized using a dry pulverizer such as a pin mill, a hammer mill, a ball mill, or a jet mill. An N-acylamino acid salt and, if necessary, a wetting agent and other additives are added to the obtained pulverized product and mixed using the mixer. The obtained mixture is hydrated, kneaded and granulated in the same manner as in the above production method, and then dried to produce a granular wettable powder. Examples of the granulation method at that time include extrusion granulation, rolling granulation, mixed granulation, fluidized bed granulation, spray drying granulation, and compression granulation.
［顆粒水和剤の施用方法］
本発明の顆粒水和剤の施用方法としては、顆粒水和剤を水に投入し、分散希釈させた後、スプレーヤー等で作物や土壌等に施用する。水への希釈倍率は、顆粒水和剤中の農薬原体の種類、含有量、施用目的によって異なるが、通常は１０〜１００００倍程度、好ましくは５０〜８０００倍程度、より好ましくは５００〜４０００倍程度である。
[Method of applying granule wettable powder]
As a method for applying the granule wettable powder of the present invention, the granule wettable powder is poured into water, dispersed and diluted, and then applied to crops, soil and the like with a sprayer or the like. The dilution ratio in water varies depending on the type, content and application purpose of the agrochemical substance in the granular wettable powder, but is usually about 10 to 10,000 times, preferably about 50 to 8000 times, more preferably 500 to 4000. It is about twice.
［顆粒水和剤の包装形態］
本発明の顆粒水和剤の包装形態として、アルミ袋、紙袋、紙パック、ポリボトルなど、通常の粒剤や水和剤で使用可能な容器を使用することができる。保存時の吸湿を避けるためには、アルミ袋や内装がアルミコーテイングされた紙袋、ポリ袋、ポリボトル等が好ましい。また、水溶性パックに梱包したものを、これらの吸湿を防止した袋に充填することにより、保存時の吸湿防止、安全性の向上、希釈時の取扱性を向上させることもできる。
[Packaging form of granule wettable powder]
As a packaging form of the granule wettable powder of the present invention, a container that can be used as a normal granule or wettable powder, such as an aluminum bag, a paper bag, a paper pack, or a plastic bottle, can be used. In order to avoid moisture absorption during storage, a paper bag, a plastic bag, a plastic bottle, or the like with an aluminum bag or an interior coated with aluminum is preferable. In addition, by packing what is packed in a water-soluble pack into a bag that prevents moisture absorption, it is possible to prevent moisture absorption during storage, improve safety, and improve handling during dilution.
既に述べたように、本発明は、従来、顆粒水和剤化が困難であった７０℃以下の融点又は軟化点を有する農薬原体を用いた場合であっても、水に投入後の崩壊性と分散性が良好な農園芸用顆粒水和剤の製造を可能としたものである。また、分散剤として使用するＮ−アシルアミノ酸塩の人体への刺激、環境毒性が低いことから、本発明の顆粒水和剤は安全性が高く、薬害が無く、対象有害生物に対し安定した作用を示す。 As already mentioned, the present invention is a conventional disintegration after being poured into water even when using an agrochemical base having a melting point or softening point of 70 ° C. or lower, which has been difficult to make into a granulated wettable powder. This makes it possible to produce a granulating wettable powder for agriculture and horticulture that has good properties and dispersibility. In addition, since the N-acylamino acid salt used as a dispersant has low irritation to humans and low environmental toxicity, the granule wettable powder of the present invention has high safety, no phytotoxicity, and stable action against target pests. Indicates.
以下に本発明の実施例及び比較例を示し、本発明を更に詳細に説明するが、本発明はこれらの範囲に限定されるものではない。なお、以下の実施例及び比較例において、「部」及び「％」は、特に断りがない限り、それぞれ「質量部」及び「質量％」を表わす。 EXAMPLES Examples and comparative examples of the present invention will be shown below, and the present invention will be described in more detail. However, the present invention is not limited to these ranges. In the following examples and comparative examples, “parts” and “%” represent “parts by mass” and “% by mass”, respectively, unless otherwise specified.
用いた測定方法と評価方法を以下に記載する。 The measurement method and evaluation method used are described below.
（水中崩壊性試験Ａ）
２５０ｍｌ共栓付シリンダー中に農薬公定検査法に基づく３度硬水を２５０ｍｌ入れ、恒温水槽中で２０℃に保った。該シリンダー内に５００ｍｇの顆粒水和剤を投入し、その崩壊性を観察して次の５段階で評価した。
Ａ：顆粒水和剤がシリンダー底部に到達する迄に殆どが崩壊する。崩壊性良好。
Ｂ：顆粒水和剤がＡとＣの中間の状態で崩壊する。崩壊性は概ね良好。
Ｃ：顆粒水和剤が水中で糸を引きながら崩壊、あるいはシリンダー底部に到達するまでに約５割程度が崩壊する。崩壊性やや良好。
Ｄ：顆粒水和剤がＣとＥの中間の状態で崩壊する。崩壊性はやや不良。
Ｅ：顆粒水和剤が殆どが崩壊せずにシリンダー底部にまで到達する。崩壊性不良。
(Underwater disintegration test A)
250 ml of 3 degree hard water based on the official inspection method for agricultural chemicals was put in a 250 ml stoppered cylinder and kept at 20 ° C. in a constant temperature water bath. 500 mg of granule wettable powder was put into the cylinder, and its disintegration property was observed and evaluated in the following five stages.
A: Most of the granulated wettable powder disintegrates before reaching the bottom of the cylinder. Good disintegration.
B: Granule wettable powder disintegrates in a state between A and C. Disintegration is generally good.
C: About 50% of the granule wettable powder collapses while pulling the thread in water or reaches the bottom of the cylinder. Good disintegration.
D: Granule wettable powder disintegrates in an intermediate state between C and E. Disintegration is slightly poor.
E: Most of the granular wettable powder reaches the bottom of the cylinder without disintegrating. Poor disintegration.
（水中崩壊性試験Ｂ）
２５０ｍｌ共栓付シリンダー中に農薬公定検査法に基づく３度硬水を２５０ｍｌ入れ、恒温水槽中で２０℃に保った。該シリンダー内に５００ｍｇの顆粒水和剤を投入して、その１分間後に１秒に１回の割合でシリンダーの反転を繰り返し、該顆粒水和剤が完全に崩壊するまでの回数を測定し、下記の基準で評価した。
(Underwater disintegration test B)
250 ml of 3 degree hard water based on the official inspection method for agricultural chemicals was put in a 250 ml stoppered cylinder and kept at 20 ° C. in a constant temperature water bath. 500 mg of the granule wettable powder was put into the cylinder, and after 1 minute, the cylinder was inverted at a rate of once per second, and the number of times until the granule wettable powder was completely disintegrated was measured. Evaluation was made according to the following criteria.
（水中崩壊性試験Ｃ）
前記（水中崩壊性試験Ａ）において、農薬公定検査法に基づく３度硬水をＣＩＰＡＣ（Collaborative International Pesticide Analytical Council；国際農薬分析法協議会）法に基づくCIPAC 標準水Ｄに代えた以外は、（水中崩壊性試験Ａ）と同様に操作して試験した。
(Underwater disintegration test C)
(Underwater disintegration test A), except that the 3rd hard water based on the official pesticide inspection method was replaced with CIPAC standard water D based on the CIPAC (Collaborative International Pesticide Analytical Council) method. The test was conducted in the same manner as in the disintegration test A).
（水中崩壊性試験Ｄ）
前記（水中崩壊性試験Ｂ）において、農薬公定検査法に基づく３度硬水をＣＩＰＡＣ（Collaborative International Pesticide Analytical Council；国際農薬分析法協議会）法に基づくCIPAC 標準水Ｄに代えた以外は、（水中崩壊性試験Ａ）と同様に操作して試験した。
(Underwater disintegration test D)
In the above (Underwater Disintegration Test B), except that the 3rd hard water based on the official pesticide inspection method was replaced with CIPAC standard water D based on the CIPAC (Collaborative International Pesticide Analytical Council) method, The test was conducted in the same manner as in the disintegration test A).
転倒回数０〜４回：速やかに崩壊する。最適。
転倒回数５〜９回：実用に耐えうる範囲で崩壊する。良好。
転倒回数１０〜１４回：崩壊にやや時間がかかる。やや不適。
転倒回数１５〜１９回：崩壊に時間がかかる。不適。
転倒回数２０回以上：崩壊せず。不適。
Number of falls 0 to 4 times: Collapses quickly. Optimal.
Number of falls: 5 to 9: Collapses within a practical range. Good.
Number of falls 10-14: It takes some time to collapse. Somewhat inappropriate.
Number of falls 15-19: It takes time to collapse. Unsuitable.
More than 20 falls: No collapse. Unsuitable.
（懸垂性試験１）
前記水中崩壊性試験Ｂを実施した後、該シリンダーを更に２０回転倒し、５分後の沈殿物量を目視で観察し、下記の基準で評価した。
○：沈殿物が少ない。懸垂性良好。
△：沈降物がやや多い。懸垂性やや不良。
×：沈殿物が多い。懸垂性不良。
(Suspension test 1)
After carrying out the underwater disintegration test B, the cylinder was further tilted 20 times, and the amount of precipitate after 5 minutes was visually observed and evaluated according to the following criteria.
○: There is little precipitate. Good suspension.
Δ: Slightly much sediment. Slightly poor suspension.
X: There are many precipitates. Poor suspension.
（懸垂性試験２）
前記水中崩壊性試験Ｄを実施した後に、該シリンダーを更に２０回転倒し、５分後の沈殿物量を目視で観察し、下記の基準で評価した。
○：沈殿物が少ない。懸垂性良好。
△：沈降物がやや多い。懸垂性やや不良。
×：沈殿物が多い。懸垂性不良。
(Suspension test 2)
After carrying out the underwater disintegration test D, the cylinder was further tilted 20 times, and the amount of precipitate after 5 minutes was visually observed and evaluated according to the following criteria.
○: There is little precipitate. Good suspension.
Δ: Slightly much sediment. Slightly poor suspension.
X: There are many precipitates. Poor suspension.
（分散性試験１）
前記懸垂性試験１を実施した後、該シリンダーを更に２〜３回転倒し、分散液を光学顕微鏡（倍率４００倍）を用いて凝集物の形成の有無を確認し、下記の基準で評価した。
○：凝集物がない。分散性良好。
△：少量の凝集物が存在する。分散性やや不良。
×：多くの凝集物が存在する。分散性不良。
(Dispersibility test 1)
After carrying out the suspension test 1, the cylinder was further turned 2-3 times, and the dispersion was checked for the presence or absence of aggregate formation using an optical microscope (400 times magnification), and evaluated according to the following criteria.
○: There is no aggregate. Good dispersibility.
Δ: A small amount of aggregate is present. Dispersibility is slightly poor.
X: Many aggregates exist. Dispersibility is poor.
（分散性試験２）
前記懸垂性試験２を実施した後、該シリンダーを更に２〜３回転倒し、分散液を光学顕微鏡（倍率４００倍）を用いて凝集物の形成の有無を確認し、下記の基準で評価した。
○：凝集物がない。分散性良好。
△：少量の凝集物が存在する。分散性やや不良。
×：多くの凝集物が存在する。分散性不良。
(Dispersibility test 2)
After carrying out the suspension test 2, the cylinder was further turned 2-3 times, and the dispersion was checked for the formation of aggregates using an optical microscope (400 times magnification), and evaluated according to the following criteria.
○: There is no aggregate. Good dispersibility.
Δ: A small amount of aggregate is present. Dispersibility is slightly poor.
X: Many aggregates exist. Dispersibility is poor.
（分散性試験３）
前記分散性試験２を実施した後、シリンダーを静置したまま６時間経過後、該シリンダーを更に２〜３回転倒し、分散液を光学顕微鏡（倍率４００倍）を用いて凝集物の形成の有無を確認し、下記の基準で評価した。
○：凝集物がない。分散性良好。
△：少量の凝集物が存在する。分散性やや不良。
×：多くの凝集物が存在する。分散性不良。
(Dispersibility test 3)
After carrying out the dispersibility test 2, after 6 hours with the cylinder still standing, the cylinder was further turned down 2-3 times, and the dispersion was subjected to the presence or absence of aggregate formation using an optical microscope (400 times magnification). Was confirmed and evaluated according to the following criteria.
○: There is no aggregate. Good dispersibility.
Δ: A small amount of aggregate is present. Dispersibility is slightly poor.
X: Many aggregates exist. Dispersibility is poor.
（水分散粒径の測定）
懸垂性試験１を実施した後、シリンダーを更に２〜３回転倒し、粒度分布測定装置（コールター社製、ＬＳ２３０）を用いて分散液の平均粒径（μｍ）を測定した。この評価方法においては、平均粒径が小さいものほど、分散性が高く（凝集物が少なく）良好である、と評価される。
(Measurement of water-dispersed particle size)
After carrying out the suspension test 1, the cylinder was further turned 2-3 times, and the average particle size (μm) of the dispersion was measured using a particle size distribution measuring device (LS230, manufactured by Coulter Inc.). In this evaluation method, it is evaluated that the smaller the average particle size, the better the dispersibility (the fewer aggregates).
（油膜形成の観察）
懸垂性試験１を実施した後、分散液の水面の状態を目視で観察し、油膜形成の有無を確認し、下記の基準で評価した。
○：油膜形成がなく、均一に分散する。良好。
△：少量の油膜形成が観察されるが、均一に分散する。良好。
×：油膜形成が観察され、かつ不均一な分散である。不良。
(Observation of oil film formation)
After carrying out the suspension test 1, the state of the water surface of the dispersion was visually observed to confirm the presence or absence of oil film formation, and evaluated according to the following criteria.
○: No oil film is formed, and the oil is uniformly dispersed. Good.
Δ: A small amount of oil film formation is observed, but it is uniformly dispersed. Good.
X: Oil film formation was observed and non-uniform dispersion. Bad.
（造粒性の観察）
顆粒状物の造粒を行った際に、造粒粒子の成形性を目視で確認した。
○：造粒性は良好であり、所望の造粒物が得られる。
×：造粒性が悪く、造粒できない、または造粒後の成形が崩れる。
(Observation of granulation)
When granulating the granular material, the moldability of the granulated particles was visually confirmed.
○: Granulation property is good, and a desired granulated product is obtained.
X: Granulation property is poor, granulation cannot be performed, or molding after granulation is broken.
（実施例１）
イミノクタジンアルベシル酸塩（軟化点：６０℃）５０部をメタノール５０部に溶解した後、この溶液を合成非晶質シリカ（塩野義製薬株式会社製の商品名「カープレックスＸＲ」）５０部と混合し、５０℃で加温してメタノールを留去した。得られた粉末状混合物をジェットミル（日本ニューマチック工業株式会社製の商品名「スーパーソニックジェットミルＰＪＭ」）を用いて粉砕して、イミノクタジンアルベシル酸塩を５０％含有する粉末１００部を得た。
Example 1
After dissolving 50 parts of iminotadine albecyl salt (softening point: 60 ° C.) in 50 parts of methanol, this solution was mixed with 50 parts of synthetic amorphous silica (trade name “Carplex XR” manufactured by Shionogi & Co., Ltd.). The mixture was mixed and heated at 50 ° C. to distill off methanol. The obtained powdery mixture was pulverized using a jet mill (trade name “Supersonic Jet Mill PJM” manufactured by Nippon Pneumatic Industry Co., Ltd.) to obtain 100 parts of a powder containing 50% iminoctadine albesylate. It was.
作製したイミノクタジンアルベシル酸塩を５０％含有する粉末６０部、Ｎ−ステアロイル−Ｌ−グルタミン酸２ナトリウム（味の素株式会社製の商品名「アミソフトＨＳ−２１」）２０部、Ｎ−ヤシ油脂肪酸アシル−Ｌ−グルタミン酸ナトリウム（味の素株式会社製の商品名「アミソフトＣＳ−１１」）１０部および珪藻土（白山工業株式会社製の商品名「ゼムライト３Ｙ」）１０部を混合し、「エックサンプルミルＫII−１型」（株式会社ダルトン製のハンマーミル）を用いて粉砕して、平均粒子径約１０μｍの混合物を得た。得られた混合物を混合造粒機「ラボラトリーマトリックスＬＭＡ５−Ｖ」（奈良機械株式会社製）に投入し、水１５部を滴下しながら混合して不定形の顆粒に造粒した。得られた顆粒を４５℃で３時間乾燥し、篩い分け操作を行い、１２５〜４２５μｍの粒度分布範囲を有し、かつ、有効成分としてイミノクタジンアルベシル酸塩を３０％含有する顆粒水和剤を得た。 60 parts of powder containing 50% of iminotadine albesylate prepared, 20 parts of N-stearoyl-L-glutamate disodium (trade name “Amisoft HS-21” manufactured by Ajinomoto Co., Inc.), N-coconut oil fatty acid acyl- 10 parts of L-sodium glutamate (trade name “Amisoft CS-11” manufactured by Ajinomoto Co., Inc.) and 10 parts of diatomaceous earth (trade name “Zemlite 3Y” manufactured by Hakusan Kogyo Co., Ltd.) are mixed together to prepare “EX Sample Mill KII-1”. The mixture was pulverized using a “type” (a hammer mill manufactured by Dalton Co., Ltd.) to obtain a mixture having an average particle size of about 10 μm. The obtained mixture was put into a mixing granulator “Laboratory Matrix LMA5-V” (manufactured by Nara Machinery Co., Ltd.), mixed while dropping 15 parts of water, and granulated into amorphous granules. The obtained granule was dried at 45 ° C. for 3 hours, subjected to a sieving operation, and a granule wettable powder having a particle size distribution range of 125 to 425 μm and containing 30% iminoctazine albesylate as an active ingredient. Obtained.
（実施例２）
０．１〜２０ｍｍ程度の大きさに砕いた農薬原体であるジチオピル（融点：６５℃）５０部と珪藻土（「ゼムライト３Ｙ」）５０部を混合し、「スーパーソニックジェットミルＰＪＭ」を用いて粉砕した。得られた粉砕物を２週間室温で静置して安定化させた後、更に「エックサンプルミルＫII−１型」を用いて粉砕して、ジチオピルを５０％含有する粉末を得た。
(Example 2)
50 parts of dithiopyr (melting point: 65 ° C.) which is an agrochemical raw material crushed to a size of about 0.1 to 20 mm and 50 parts of diatomaceous earth (“Zemlite 3Y”) are mixed, and “Super Sonic Jet Mill PJM” is used. Crushed. The obtained pulverized product was allowed to stand at room temperature for 2 weeks for stabilization, and then pulverized using “EK sample mill KII-1 type” to obtain a powder containing 50% of dithiopyr.
作製したジチオピルを５０％含有する粉末６０部、Ｎ−ステアロイル−Ｌ−グルタミン酸２ナトリウム（「アミソフトＨＳ−２１」）１５部、Ｎ−ヤシ油脂肪酸アシル−Ｌ−グルタミン酸ナトリウム（「アミソフトＣＳ−１１」）５部および珪藻土（「ゼムライト３Ｙ」）２０部を混合し、万能粉砕機（JANKE & KUNKEL GMBH & CO.KG製の「Ｍ２０型」）を用いて粉砕して、平均粒子径約７μｍの混合物を得た。得られた混合物を混練機（株式会社入江商会製の商品名「卓上型ニーダーＰＮＶ−５型」）に投入し、水２５部を滴下しながら混練し、押出造粒機（筒井理化学器械株式会社製の商品名「ＫＡＲ−１８０型」）０．５ｍｍスクリーンで押し出し造粒し、得られた顆粒を４５℃で３時間乾燥し、篩い分け操作を行い、１８０〜１０００μｍの粒度分布範囲を有し、かつ、有効成分としてジチオピルを３０％含有する顆粒水和剤を得た。 60 parts of powder containing 50% of the prepared dithiopyr, 15 parts of N-stearoyl-L-glutamate disodium (“Amisoft HS-21”), N-coconut oil fatty acid acyl-L-glutamate sodium (“Amisoft CS-11”) ) 5 parts and 20 parts of diatomaceous earth ("Zemlite 3Y") are mixed and pulverized using a universal crusher ("M20 type" manufactured by JANKE & KUNKEL GMBH & CO.KG) to obtain a mixture having an average particle size of about 7 μm Got. The obtained mixture was put into a kneader (trade name “Desktop Kneader PNV-5” manufactured by Irie Shokai Co., Ltd.), kneaded while dripping 25 parts of water, and an extrusion granulator (Tsutsui Rikenki Co., Ltd.). Product name “KAR-180 type”) Extruded and granulated with a 0.5 mm screen, the obtained granules are dried at 45 ° C. for 3 hours, and subjected to a sieving operation, having a particle size distribution range of 180 to 1000 μm And the granule wettable powder which contains 30% of dithiopyr as an active ingredient was obtained.
（実施例３）
農薬原体であるベンフレセート（融点：３２〜３５℃）４０部と珪藻土（商品名「ゼムライト３Ｙ」）３０部および合成非晶質シリカ（塩野義製薬株式会社製の商品名「カープレックス＃１１２０」）３０部を混合し、「エックサンプルミルＫII−１型」を用いて粉砕しベンフレセートを４０％含有する粉末を得た。
(Example 3)
Benfresate (melting point: 32 to 35 ° C.) 40 parts, diatomaceous earth (trade name “Zemlite 3Y”) 30 parts, and synthetic amorphous silica (trade name “Carplex # 1120” manufactured by Shionogi & Co., Ltd.) ) 30 parts were mixed and pulverized using “Ek sample mill KII-1 type” to obtain a powder containing 40% benfrecetate.
作製したベンフレセートを４０％含有する粉末７５部、Ｎ−ステアロイル−Ｌ−グルタミン酸２ナトリウム（「アミソフトＨＳ−２１」）１２部およびＮ−ヤシ油脂肪酸アシル−Ｌ−グルタミン酸ナトリウム（「アミソフトＣＳ−１１」）１３部を混合し、前出の万能粉砕機を用いて粉砕して、平均粒子径約１０μｍの混合物を得た。得られた混合物を混練機（「卓上型ニーダーＰＮＶ−５型」）に投入し、水２５部を滴下しながら混練し、押出造粒機（「ＫＡＲ−１３０型」）を用いて０．５ｍｍスクリーンで押し出し造粒し、得られた顆粒を５０℃で３時間乾燥させた後、篩い分け操作を行い、１８０〜１０００μｍの粒度分布範囲を有し、かつ、有効成分としてベンフレセートを３０％含有する顆粒水和剤を得た。 75 parts of powder containing 40% of the prepared benfrate, 12 parts of N-stearoyl-L-glutamate disodium (“Amisoft HS-21”) and N-coconut oil fatty acid acyl-L-glutamate sodium (“Amisoft CS-11”) ) 13 parts were mixed and pulverized using the above-mentioned universal pulverizer to obtain a mixture having an average particle size of about 10 μm. The obtained mixture was put into a kneader (“desk type kneader PNV-5 type”), kneaded while dropping 25 parts of water, and 0.5 mm using an extrusion granulator (“KAR-130 type”). After extruding and granulating with a screen, the resulting granules are dried at 50 ° C. for 3 hours, and then subjected to a sieving operation, having a particle size distribution range of 180 to 1000 μm, and containing 30% benfrate as an active ingredient. Granule wettable powder was obtained.
（実施例４）
実施例１で作製したイミノクタジンアルベシル酸塩を５０％含有する粉末６０部、Ｎ−ステアロイル−Ｌ−グルタミン酸２ナトリウム（「アミソフトＨＳ−２１」）１５部、珪藻土（「ゼムライト３Ｙ」）５部および部分脱スルホンリグニンスルホン酸ナトリウム（日本製紙株式会社製の商品名「バニレックスＮ」）２０部を混合し、「エックサンプルミルＫII−１型」を用いて粉砕して、平均粒子径約１０μｍの混合物を得た。得られた混合物を「ラボラトリーマトリックスＬＭＡ５−Ｖ」に投入し、水１５部を滴下しながら混合して不定形の顆粒に造粒した。得られた顆粒を４５℃で３時間乾燥させた後、篩い分け操作を行い、１２５〜４２５μｍの粒度分布範囲を有し、かつ、有効成分としてイミノクタジンアルベシル酸塩を３０％含有する顆粒水和剤を得た。
Example 4
60 parts of a powder containing 50% iminoctazine albesylate prepared in Example 1, 15 parts of N-stearoyl-L-glutamate disodium (“Amisoft HS-21”), 5 parts of diatomaceous earth (“Zemlite 3Y”) and 20 parts of partially desulphonated sodium lignin sulfonate (trade name “Vanilex N” manufactured by Nippon Paper Industries Co., Ltd.) is mixed and pulverized using “Ek sample mill KII-1 type” to obtain a mixture having an average particle size of about 10 μm. Got. The obtained mixture was put into “Laboratory Matrix LMA5-V”, mixed while dropping 15 parts of water, and granulated into irregular shaped granules. The obtained granules were dried at 45 ° C. for 3 hours, and then subjected to a sieving operation. Granule hydration having a particle size distribution range of 125 to 425 μm and containing 30% iminocazine albesylate as an active ingredient An agent was obtained.
（実施例５）
実施例１において、合成非晶質シリカ（「カープレックスＸＲ」）に代えて、合成非晶質シリカ焼成品（塩野義製薬株式会社製の商品名「カープレックスＣＳ−７」）を用いた以外は、実施例１と同様にして、イミノクタジンアルベシル酸塩を５０％含有する粉末１００部を得た。
(Example 5)
In Example 1, instead of synthetic amorphous silica (“Carplex XR”), a synthetic amorphous silica fired product (trade name “Carplex CS-7” manufactured by Shionogi & Co., Ltd.) was used. Produced 100 parts of powder containing 50% of iminotadine albesylate in the same manner as in Example 1.
作製したイミノクタジンアルベシル酸塩を５０％含有する粉末６０部、Ｎ−ステアロイル−Ｌ−グルタミン酸２ナトリウム（「アミソフトＨＳ−２１」）１５部、珪藻土（「ゼムライト３Ｙ」）５部および部分脱スルホンリグニンスルホン酸ナトリウム（「バニレックスＮ」）２０部を混合し、「エックサンプルミルＫII−１型」を用いて粉砕して、平均粒子径約１０μｍの混合物を得た。得られた混合物を「ラボラトリーマトリックスＬＭＡ５−Ｖ」に投入し、水１５部を滴下しながら混合して不定形の顆粒に造粒した。得られた顆粒を４５℃で３時間乾燥させた後、篩い分け操作を行い、１２５〜４２５μｍの粒度分布範囲を有し、かつ、有効成分イミノクタジンアルベシル酸塩を３０％含有する顆粒水和剤を得た。 60 parts of powder containing 50% of iminotadine albesylate prepared, 15 parts of N-stearoyl-L-glutamate ("Amisoft HS-21"), 5 parts of diatomaceous earth ("Zemlite 3Y") and partially desulfonated lignin 20 parts of sodium sulfonate (“Vanilex N”) was mixed and pulverized using “EK sample mill KII-1 type” to obtain a mixture having an average particle size of about 10 μm. The obtained mixture was put into “Laboratory Matrix LMA5-V”, mixed while dropping 15 parts of water, and granulated into irregular shaped granules. The obtained granules are dried at 45 ° C. for 3 hours and then subjected to a sieving operation. The granule wettable powder has a particle size distribution range of 125 to 425 μm and contains 30% of the active ingredient iminoctadine albesylate. Got.
（実施例６）
実施例１で作製したイミノクタジンアルベシル酸塩を５０％含有する粉末４０部、農薬原体であるフェンヘキサミド（融点：１５３℃）３０部、Ｎ−ステアロイル−Ｌ−グルタミン酸２ナトリウム（「アミソフトＨＳ−２１」）１０部、Ｎ−ヤシ油脂肪酸アシル−Ｌ−グルタミン酸ナトリウム（「アミソフトＣＳ−１１」）７部および珪藻土（「ゼムライト３Ｙ」）１３部を混合し、「エックサンプルミルＫII−１型」を用いて粉砕して、平均粒子径約１０μｍの混合物を得た。得られた混合物を「ラボラトリーマトリックスＬＭＡ５−Ｖ」に投入し、水１２部を滴下しながら混合して不定形の顆粒に造粒した。得られた顆粒を４５℃で３時間乾燥させた後、篩い分け操作を行い、１５０〜４２５μｍの粒度分布範囲を有し、かつ、有効成分としてイミノクタジンアルベシル酸塩２０％とフェンヘキサミド３０％を含有する顆粒水和剤を得た。
(Example 6)
40 parts of powder containing 50% of iminoctadine albecyl salt prepared in Example 1, 30 parts of fenhexamide (melting point: 153 ° C.) as an agrochemical base, disodium N-stearoyl-L-glutamate (“Amisoft HS -21 ") 10 parts, N-coconut oil fatty acid acyl-L-glutamate sodium (" Amisoft CS-11 ") 7 parts and diatomaceous earth (" Zemlite 3Y ") 13 parts, To obtain a mixture having an average particle size of about 10 μm. The obtained mixture was put into “Laboratory Matrix LMA5-V”, mixed while dropping 12 parts of water, and granulated into irregular shaped granules. The obtained granule was dried at 45 ° C. for 3 hours and then subjected to a sieving operation. It had a particle size distribution range of 150 to 425 μm, and 20% iminotadine albesylate and 30% fenhexamide as active ingredients. A granular wettable powder containing was obtained.
（実施例７）
実施例１で作製したイミノクタジンアルベシル酸塩を５０％含有する粉末４０部、農薬原体であるフェンヘキサミド（融点：１５３℃）３０部、Ｎ−ステアロイル−Ｌ−グルタミン酸２ナトリウム（「アミソフトＨＳ−２１」）１５部、珪藻土（「ゼムライト３Ｙ」）２部および部分脱スルホンリグニンスルホン酸ナトリウム（「バニレックスＮ」）１３部を混合し、「エックサンプルミルＫII−１型」を用いて粉砕して、平均粒子径約１０μｍの混合物を得た。得られた混合物を「ラボラトリーマトリックスＬＭＡ５−Ｖ」に投入し、水１２部を滴下しながら混合して不定形の顆粒に造粒した。得られた顆粒を４５℃で３時間乾燥させた後、篩い分け操作を行い、１５０〜４２５μｍの粒度分布範囲を有し、かつ、有効成分としてイミノクタジンアルベシル酸塩２０％とフェンヘキサミド３０％を含有する顆粒水和剤を得た。
(Example 7)
40 parts of powder containing 50% of iminoctadine albecyl salt prepared in Example 1, 30 parts of fenhexamide (melting point: 153 ° C.) as an agrochemical base, disodium N-stearoyl-L-glutamate (“Amisoft HS -21 ") 15 parts, 2 parts of diatomaceous earth (" Zemlite 3Y ") and 13 parts of partially desulphonated sodium lignin sulfonate (" Vanilex N ") are mixed and pulverized using" EX sample mill KII-1 type " Thus, a mixture having an average particle size of about 10 μm was obtained. The obtained mixture was put into “Laboratory Matrix LMA5-V”, mixed while dropping 12 parts of water, and granulated into irregular shaped granules. The obtained granule was dried at 45 ° C. for 3 hours and then subjected to a sieving operation. It had a particle size distribution range of 150 to 425 μm, and 20% iminotadine albesylate and 30% fenhexamide as active ingredients. A granular wettable powder containing was obtained.
（実施例８）
実施例１で作製したイミノクタジンアルベシル酸塩を５０％含有する粉末４０部、農薬原体であるピリブチカルブ（融点：８５．７〜８６．２℃）３０部、Ｎ−ステアロイル−Ｌ−グルタミン酸２ナトリウム（「アミソフトＨＳ−２１」）１５部および芳香族スルホン酸ナトリウムホルマリン縮合物（花王株式会社製の商品名「デモールＳＮＢ」）１５部を混合し、前出の万能粉砕機を用いて粉砕して、平均粒子径約１０μｍの混合物を得た。得られた混合物を「ラボラトリーマトリックスＬＭＡ５−Ｖ」に投入し、水１５部を滴下しながら混合して不定形の顆粒に造粒した。得られた顆粒を４５℃で３時間乾燥させた後、篩い分け操作を行い、１８０〜６００μｍの粒度分布範囲を有し、かつ、有効成分としてイミノクタジンアルベシル酸塩２０％とピリブチカルブ３０％を含有する顆粒水和剤を得た。
(Example 8)
40 parts of powder containing 50% of iminotadine albecyl salt prepared in Example 1, 30 parts of pyributicarb (melting point: 85.7-86.2 ° C.) as an agrochemical base, disodium N-stearoyl-L-glutamate ("Amisoft HS-21") 15 parts and 15 parts aromatic sodium sulfonate formalin condensate (trade name "Demol SNB" manufactured by Kao Corporation) are mixed and pulverized using the above-mentioned universal crusher. A mixture having an average particle size of about 10 μm was obtained. The obtained mixture was put into “Laboratory Matrix LMA5-V”, mixed while dropping 15 parts of water, and granulated into irregular shaped granules. The obtained granules were dried at 45 ° C. for 3 hours and then subjected to a sieving operation, having a particle size distribution range of 180 to 600 μm, and containing 20% iminoctadine arbesylate and 30% pyributycarb as active ingredients A granulated wettable powder was obtained.
（実施例９）
実施例１で作製したイミノクタジンアルベシル酸塩を５０％含有する粉末４０部、農薬原体であるイプコナゾール（融点：９１〜１１９℃）３０部、Ｎ−ステアロイル−Ｌ−グルタミン酸２ナトリウム（「アミソフトＨＳ−２１」）１５部および部分脱スルホンリグニンスルホン酸ナトリウム（「バニレックスＮ」）１５部を混合し、「エックサンプルミルＫII−１型」を用いて粉砕して、平均粒子径約１０μｍの混合物を得た。得られた混合物を「ラボラトリーマトリックスＬＭＡ５−Ｖ」に投入し、水１２部を滴下しながら混合して不定形の顆粒に造粒した。得られた顆粒を４５℃で３時間乾燥させた後、篩い分け操作を行い、１８０〜６００μｍの粒度分布範囲を有し、かつ、有効成分としてイミノクタジンアルベシル酸塩２０％とイプコナゾール３０％を含有する顆粒水和剤を得た。
Example 9
40 parts of a powder containing 50% of iminoctadine albecyl salt prepared in Example 1, 30 parts of ipconazole (melting point: 91-119 ° C.) as an agrochemical base, disodium N-stearoyl-L-glutamate (“Amisoft HS”) -21 ") and 15 parts of partially desulfonated lignin sodium sulfonate (" Vanilex N "), and pulverized using" Eck sample mill KII-1 type "to obtain a mixture having an average particle size of about 10 [mu] m. Obtained. The obtained mixture was put into “Laboratory Matrix LMA5-V”, mixed while dropping 12 parts of water, and granulated into irregular shaped granules. The obtained granule was dried at 45 ° C. for 3 hours and then subjected to a sieving operation, having a particle size distribution range of 180 to 600 μm, and containing 20% iminoctadine albecylate and 30% ipconazole as active ingredients A granulated wettable powder was obtained.
（実施例１０）
実施例２で作製したジチオピルを５０％含有する粉末８０部、Ｎ−ステアロイル−Ｌ−グルタミン酸２ナトリウム（「アミソフトＨＳ−２１」）１５部および部分脱スルホンリグニンスルホン酸ナトリウム（「バニレックスＮ」）５部を混合し、前出の万能粉砕機を用いて粉砕して、平均粒子径約７μｍの混合物を得た。得られた混合物を混練機（「卓上型ニーダーＰＮＶ−５型」）に投入し、水２５部を滴下しながら混練し、押出造粒機（ＫＡＲ−１３０型）０．５ｍｍスクリーンで押し出し造粒し、得られた顆粒を４５℃で３時間乾燥させた後、篩い分け操作を行い、１８０〜１０００μｍの粒度分布範囲を有し、かつ、有効成分としてジチオピル４０％を含有する顆粒水和剤を得た。
(Example 10)
80 parts of powder containing 50% dithiopyr prepared in Example 2, 15 parts of N-stearoyl-L-glutamate disodium ("Amisoft HS-21") and partially desulfonated sodium lignin sulfonate ("Vanilex N") 5 The parts were mixed and pulverized using the above-mentioned universal pulverizer to obtain a mixture having an average particle size of about 7 μm. The obtained mixture was put into a kneading machine ("desk type kneader PNV-5 type"), kneaded while dripping 25 parts of water, and extruded and granulated with an extrusion granulator (KAR-130 type) 0.5 mm screen. The granules obtained were dried at 45 ° C. for 3 hours, and then subjected to a sieving operation. A granule wettable powder having a particle size distribution range of 180 to 1000 μm and containing 40% of dithiopyr as an active ingredient was obtained. Obtained.
（実施例１１）
農薬原体であるベンフレセート（融点：３２〜３５℃）４０部と珪藻土（「ゼムライト３Ｙ」）６０部を混合し、「エックサンプルミルＫII−１型」を用いて粉砕して、ベンフレセートを４０％含有する粉末を得た。作製したベンフレセートを４０％含有する粉末７５部、Ｎ−ステアロイル−Ｌ−グルタミン酸２ナトリウム（「アミソフトＨＳ−２１」）８部、Ｎ−ヤシ油脂肪酸アシル−Ｌ−グルタミン酸ナトリウム（「アミソフトＣＳ−１１」）７部、部分脱スルホンリグニンスルホン酸ナトリウム（「バニレックスＮ」）５部および珪藻土（「ゼムライト３Ｙ」）５部を混合し、前出の万能粉砕機を用いて粉砕して、平均粒子径約１０μｍの混合物を得た。得られた混合物を「ラボラトリーマトリックスＬＭＡ５−Ｖ」に投入し、水１５部を滴下しながら混合して不定形の顆粒に造粒した。得られた顆粒を４５℃で３時間乾燥させた後、篩い分け操作を行い、１８０〜６００μｍの粒度分布範囲を有し、かつ、有効成分としてベンフレセート３０％を含有する顆粒水和剤を得た。
(Example 11)
40 parts of Benfresate (melting point: 32 to 35 ° C.), which is a raw material for agricultural chemicals, and 60 parts of diatomaceous earth (“Zemlite 3Y”) are mixed and pulverized using “Ek sample mill KII-1 type”. A contained powder was obtained. 75 parts of powder containing 40% of the prepared benfrate, 8 parts of N-stearoyl-L-glutamic acid disodium (“Amisoft HS-21”), N-coconut oil fatty acid acyl-sodium L-glutamate (“Amisoft CS-11”) ) 7 parts, 5 parts of partially desulfurized sodium lignin sulfonate ("Vanilex N") and 5 parts of diatomaceous earth ("Zemlite 3Y") are mixed and pulverized using the above-mentioned universal pulverizer to obtain an average particle size of about A 10 μm mixture was obtained. The obtained mixture was put into “Laboratory Matrix LMA5-V”, mixed while dropping 15 parts of water, and granulated into irregular shaped granules. The obtained granule was dried at 45 ° C. for 3 hours and then subjected to a sieving operation to obtain a granule wettable powder having a particle size distribution range of 180 to 600 μm and containing 30% benfrate as an active ingredient. .
（実施例１２）
実施例１１で作製したベンフレセートを４０％含有する粉末７５部、ラウロイルサルコシンナトリウム（川研ファインケミカル株式会社製の商品名「ソイポンＳＬＰ」）１５部、部分脱スルホンリグニンスルホン酸ナトリウム（「バニレックスＮ」）５部および珪藻土（「ゼムライト３Ｙ」）５部を混合し、前出の万能粉砕機を用いて粉砕して、平均粒子径約１０μｍの混合物を得た。得られた混合物を「ラボラトリーマトリックスＬＭＡ５−Ｖ」に投入し、水１５部を滴下しながら混合して不定形の顆粒に造粒した。得られた顆粒を４５℃で３時間乾燥させた後、篩い分け操作を行い、１８０〜６００μｍの粒度分布範囲を有し、かつ、有効成分としてベンフレセート３０％を含有する顆粒水和剤を得た。
Example 12
75 parts of powder containing 40% of benfrate produced in Example 11, 15 parts of sodium lauroyl sarcosine (trade name “Soipon SLP” manufactured by Kawaken Fine Chemical Co., Ltd.), partially desulfonated sodium lignin sulfonate (“Vanilex N”) 5 parts and 5 parts of diatomaceous earth (“Zemlite 3Y”) were mixed and pulverized using the above-mentioned universal pulverizer to obtain a mixture having an average particle diameter of about 10 μm. The obtained mixture was put into “Laboratory Matrix LMA5-V”, mixed while dropping 15 parts of water, and granulated into irregular shaped granules. The obtained granule was dried at 45 ° C. for 3 hours and then subjected to a sieving operation to obtain a granule wettable powder having a particle size distribution range of 180 to 600 μm and containing 30% benfrate as an active ingredient. .
（実施例１３）
実施例３で作製したベンフレセートを４０％含有する粉末７５部、Ｎ−ヤシ油脂肪酸アシル−Ｌ−グルタミン酸ナトリウム（「アミソフトＣＳ−１１」）１５部および部分脱スルホンリグニンスルホン酸ナトリウム（「バニレックスＮ」）１０部を混合し、前出の万能粉砕機を用いて粉砕して、平均粒子径約１０μｍの混合物を得た。得られた混合物を混練機（「卓上型ニーダーＰＮＶ−５型」）に投入し、水２５部を滴下しながら混練し、押出造粒機（「ＫＡＲ−１３０型」）０．５ｍｍスクリーンで押し出し造粒し、得られた顆粒を５０℃で３時間乾燥させた後、篩い分け操作を行い、１８０〜１０００μｍの粒度分布範囲を有し、かつ、有効成分としてベンフレセート３０％を含有する顆粒水和剤を得た。
(Example 13)
75 parts of powder containing 40% of benfrate prepared in Example 3, 15 parts of N-coconut oil fatty acid acyl-L-sodium glutamate (“Amisoft CS-11”) and partially desulfonated lignin sodium sulfonate (“Vanilex N”) ) 10 parts were mixed and pulverized using the above-mentioned universal pulverizer to obtain a mixture having an average particle size of about 10 μm. The obtained mixture is put into a kneader (“desk type kneader PNV-5 type”), kneaded while dripping 25 parts of water, and extruded through an extrusion granulator (“KAR-130 type”) with a 0.5 mm screen. After granulating and drying the resulting granule at 50 ° C. for 3 hours, a sieving operation is performed, a granule hydration having a particle size distribution range of 180 to 1000 μm and containing 30% of benfrate as an active ingredient An agent was obtained.
（実施例１４）
農薬原体であるベンフレセート（融点：３２〜３５℃）３２部、農薬原体希釈剤「ハイゾールＳＡＳ−２９６」（新日本石油化学社製の２環芳香族炭化水素化合物を含有する混合物）１４部からなる均一溶液を合成非晶質シリカ（塩野義製薬株式会社製の商品名「カープレックス＃８０」）３４部と混合した後、「エックサンプルミルＫＩＩ−１型」を用いて粉砕してベンフレセートを４０％含有する粉末を得た。
(Example 14)
Benfresate (melting point: 32 to 35 ° C.) 32 parts as a pesticide raw material, 14 parts of a pesticide raw material diluent “Hysol SAS-296” (a mixture containing a bicyclic aromatic hydrocarbon compound manufactured by Nippon Petrochemical Co., Ltd.) After mixing with 34 parts of a synthetic amorphous silica (trade name “Carplex # 80”, manufactured by Shionogi & Co., Ltd.), the mixture is pulverized using “EX SAMPLE MILL KII-1” and benfresate. Was obtained.
作製したベンフレセートを４０％含有する粉末８０部、Ｎ−ヤシ油脂肪酸アシル−Ｌ−グルタミン酸ナトリウム（「アミソフトＣＳ−１１」）５部、Ｎ−ミリストイルメチルタウリン酸ナトリウム（日光ケミカルズ株式会社製の商品名「ＮＩＫＫＯＬ ＭＭＴ」）２部、増量剤としてベントナイト１１部、および湿潤剤としてジ−２−エチルヘキシルスルホコハク酸ナトリウム２部を混合し、前出の万能粉砕機を用いて粉砕して、平均粒子径約１０μｍの混合物を得た。得られた混合物を混練機（「卓上型ニーダーＰＮＶ−５型」）に投入し、水２５部を滴下しながら混練し、押出造粒機（「ＫＡＲ−１３０型」）を用いて０．５ｍｍスクリーンで押し出し造粒し、得られた顆粒を５０℃で３時間乾燥させた後、篩い分け操作を行い、１８０〜１０００μｍの粒度分布範囲を有し、かつ、有効成分としてベンフレセート３０％を含有する顆粒水和剤を得た。 80 parts of powder containing 40% of the prepared benfrate, 5 parts of N-coconut oil fatty acid acyl-L-sodium glutamate ("Amisoft CS-11"), sodium N-myristoyl methyl taurate (trade name, manufactured by Nikko Chemicals Co., Ltd.) 2 parts of “NIKKOL MMT”), 11 parts of bentonite as a bulking agent, and 2 parts of sodium di-2-ethylhexylsulfosuccinate as a wetting agent are pulverized using the above-mentioned universal pulverizer to obtain an average particle size of about A 10 μm mixture was obtained. The obtained mixture was put into a kneader (“desk type kneader PNV-5 type”), kneaded while dropping 25 parts of water, and 0.5 mm using an extrusion granulator (“KAR-130 type”). After extruding and granulating with a screen, the obtained granules are dried at 50 ° C. for 3 hours, and then subjected to a sieving operation, having a particle size distribution range of 180 to 1000 μm, and containing 30% benfrate as an active ingredient. Granule wettable powder was obtained.
（実施例１５）
実施例１で作製したイミノクタジンアルベシル酸塩を５０％含有する粉末６０部、Ｎ−ステアロイル−Ｌ−グルタミン酸２ナトリウム（「アミソフトＨＳ−２１」）１２．５部、Ｎ−ミリストイルメチルタウリン酸ナトリウム（「ＮＩＫＫＯＬ ＭＭＴ」）２．５部および変性リグニンスルホン酸ナトリウム（日本製紙株式会社製の商品名「パールレックスＤＰ」）２３部およびアタパルジャイト２部を混合し、「エックサンプルミルＫＩＩ−１型」を用いて粉砕して、平均粒子径約１０μｍの混合物を得た。得られた混合物を流動層造粒機「フローコーターＦＬＯ−１」に投入し、流動エアー送風下、水８０部を噴霧して不定形の顆粒に造粒した。得られた顆粒を５０℃で３時間乾燥させた後、篩い分け操作を行い、１２５〜１０００μｍの粒度分布範囲を有し、かつ、有効成分としてイミノクタジンアルベシル酸塩３０％を含有する顆粒水和剤を得た。
(Example 15)
60 parts of powder containing 50% iminoctadine albecyl salt prepared in Example 1, 12.5 parts of N-stearoyl-L-glutamate disodium (“Amisoft HS-21”), sodium N-myristoyl methyl taurate ( 2.5 parts of “NIKKOL MMT”), 23 parts of modified sodium lignin sulfonate (trade name “Pearl Rex DP” manufactured by Nippon Paper Industries Co., Ltd.) and 2 parts of attapulgite are mixed together. To obtain a mixture having an average particle size of about 10 μm. The obtained mixture was put into a fluidized bed granulator “Flow Coater FLO-1” and sprayed with 80 parts of water under flowing air to granulate into irregular shaped granules. The obtained granules are dried at 50 ° C. for 3 hours and then subjected to a sieving operation. The granules have a particle size distribution range of 125 to 1000 μm and contain 30% iminocazine albesylate as an active ingredient. An agent was obtained.
（比較例１）
実施例１において、Ｎ−ステアロイル−Ｌ−グルタミン酸２ナトリウム（「アミソフトＨＳ−２１」）とＮ−ヤシ油脂肪酸アシル−Ｌ−グルタミン酸ナトリウム（「アミソフトＣＳ−１１」）に代えて、部分脱スルホンリグニンスルホン酸ナトリウム（「バニレックスＮ」）を用いた以外は、実施例１と同様にして、１２５〜４２５μｍの粒度分布範囲を有し、かつ、有効成分としてイミノクタジンアルベシル酸塩３０％を含有する顆粒水和剤を得た。
(Comparative Example 1)
Instead of disodium N-stearoyl-L-glutamate (“Amisoft HS-21”) and N-coconut oil fatty acid acyl-sodium sodium L-glutamate (“Amisoft CS-11”) in Example 1, partially desulfonated lignin Granules having a particle size distribution range of 125 to 425 μm and containing 30% iminotadine albesylate as an active ingredient, in the same manner as in Example 1 except that sodium sulfonate (“Vanilex N”) was used A wettable powder was obtained.
（比較例２）
実施例２において、Ｎ−ステアロイル−Ｌ−グルタミン酸２ナトリウム（「アミソフトＨＳ−２１」）とＮ−ヤシ油脂肪酸アシル−Ｌ−グルタミン酸ナトリウム（「アミソフトＣＳ−１１」）に代えて、部分脱スルホンリグニンスルホン酸ナトリウム（「バニレックスＮ））を用いた以外は、実施例２と同様にして、１８０〜１０００μｍの粒度分布範囲を有し、かつ、有効成分としてジチオピル３０％を含有する顆粒水和剤を得た。
(Comparative Example 2)
In Example 2, instead of disodium N-stearoyl-L-glutamate (“Amisoft HS-21”) and N-coconut oil fatty acid acyl-sodium L-glutamate (“Amisoft CS-11”), partially desulfonated lignin A granular wettable powder having a particle size distribution range of 180 to 1000 μm and containing 30% of dithiopyr as an active ingredient is obtained in the same manner as in Example 2 except that sodium sulfonate (“Vanilex N”) is used. Obtained.
（比較例３）
実施例３において、Ｎ−ステアロイル−Ｌ−グルタミン酸２ナトリウム（「アミソフトＨＳ−２１」）とＮ−ヤシ油脂肪酸アシル−Ｌ−グルタミン酸ナトリウム（「アミソフトＣＳ−１１」）に代えて、部分脱スルホンリグニンスルホン酸ナトリウム（「バニレックスＮ」）を用いた以外は、実施例３と同様にして、１８０〜１０００μｍの粒度分布範囲を有し、かつ、有効成分としてベンフレセート３０％を含有する顆粒水和剤を得た。
(Comparative Example 3)
In Example 3, instead of disodium N-stearoyl-L-glutamate (“Amisoft HS-21”) and N-coconut oil fatty acid acyl-L-glutamate sodium (“Amisoft CS-11”), partially desulfonated lignin A granular wettable powder having a particle size distribution range of 180 to 1000 μm and containing 30% of benfrate as an active ingredient, in the same manner as in Example 3 except that sodium sulfonate (“Vanilex N”) was used. Obtained.
（比較例４）
実施例４において、Ｎ−ステアロイル−Ｌ−グルタミン酸２ナトリウム（「アミソフトＨＳ−２１」）に代えて、部分脱スルホンリグニンスルホン酸ナトリウム（「バニレックスＮ」）を用いた以外は、実施例４と同様にして、１２５〜４２５μｍの粒度分布範囲を有し、かつ、有効成分としてイミノクタジンアルベシル酸塩３０％を含有する顆粒水和剤を得た。
(Comparative Example 4)
In Example 4, it replaced with N-stearoyl-L-glutamate disodium ("Amisoft HS-21"), and the same as Example 4 except having used partially desulfonated sodium lignin sulfonate ("Vanilex N"). As a result, a granule wettable powder having a particle size distribution range of 125 to 425 μm and containing 30% iminotadine albesylate as an active ingredient was obtained.
（比較例５）
実施例４において、Ｎ−ステアロイル−Ｌ−グルタミン酸２ナトリウム（「アミソフトＨＳ−２１」）に代えて、ポリカルボン酸ナトリウム（竹本油脂株式会社の商品名「ニューカルゲンＷＧ−５」）を用いた以外は、実施例４と同様にして、１２５〜４２５μｍの粒度分布範囲を有し、かつ、有効成分としてイミノクタジンアルベシル酸塩３０％を含有する顆粒水和剤を得た。
(Comparative Example 5)
In Example 4, in place of disodium N-stearoyl-L-glutamate (“Amisoft HS-21”), sodium polycarboxylate (trade name “New Calgen WG-5” from Takemoto Yushi Co., Ltd.) was used. Obtained a granulated wettable powder having a particle size distribution range of 125 to 425 μm and containing 30% of iminoctadine arbesylate as an active ingredient in the same manner as in Example 4.
（比較例６）
実施例５において、Ｎ−ステアロイル−Ｌ−グルタミン酸２ナトリウム（「アミソフトＨＳ−２１」）に代えて、部分脱スルホンリグニンスルホン酸ナトリウム（「バニレックスＮ」）を用いた以外は、実施例５と同様にして、１２５〜４２５μｍの粒度分布範囲を有し、かつ、有効成分としてイミノクタジンアルベシル酸塩３０％を含有する顆粒水和剤を得た。
(Comparative Example 6)
Example 5 was the same as Example 5 except that partially desulfonated sodium lignin sulfonate (“Vanilex N”) was used instead of disodium N-stearoyl-L-glutamate (“Amisoft HS-21”). As a result, a granule wettable powder having a particle size distribution range of 125 to 425 μm and containing 30% iminotadine albesylate as an active ingredient was obtained.
（比較例７）
実施例６において、Ｎ−ステアロイル−Ｌ−グルタミン酸２ナトリウム（「アミソフトＨＳ−２１」）とＮ−ヤシ油脂肪酸アシル−Ｌ−グルタミン酸ナトリウム（「アミソフトＣＳ−１１」）に代えて、芳香族スルホン酸ナトリウムホルマリン縮合物（花王株式会社製の商品名「デモールＳＮＢ」）を用いた以外は、実施例６と同様にして、１５０〜４２５μｍの粒度分布範囲を有し、かつ、有効成分としてイミノクタジンアルベシル酸塩２０％とフェンヘキサミド３０％を含有する顆粒水和剤を得た。
(Comparative Example 7)
In Example 6, instead of disodium N-stearoyl-L-glutamate (“Amisoft HS-21”) and N-coconut oil fatty acid acyl-L-sodium glutamate (“Amisoft CS-11”), aromatic sulfonic acid Except that a sodium formalin condensate (trade name “Demol SNB” manufactured by Kao Corporation) was used, it had a particle size distribution range of 150 to 425 μm and iminoctazine albecil as an active ingredient in the same manner as in Example 6. A granular wettable powder containing 20% acid salt and 30% fenhexamide was obtained.
（比較例８）
実施例８において、Ｎ−ステアロイル−Ｌ−グルタミン酸２ナトリウム（「アミソフトＨＳ−２１」）に代えて、芳香族スルホン酸ナトリウムホルマリン縮合物（花王株式会社製の商品名「デモールＳＮＢ」）を用いた以外は、実施例８と同様にして、１８０〜６００μｍの粒度分布範囲を有し、かつ、有効成分としてイミノクタジンアルベシル酸塩２０％とピリブチカルブ３０％を含有する顆粒水和剤を得た。
(Comparative Example 8)
In Example 8, instead of disodium N-stearoyl-L-glutamate (“Amisoft HS-21”), an aromatic sodium sulfonate formalin condensate (trade name “Demol SNB” manufactured by Kao Corporation) was used. Except for the above, a granular wettable powder having a particle size distribution range of 180 to 600 μm and containing 20% iminotazine arbesylate and 30% pyributycarb as active ingredients was obtained in the same manner as Example 8.
（比較例９）
実施例９において、Ｎ−ステアロイル−Ｌ−グルタミン酸２ナトリウム（「アミソフトＨＳ−２１」）に代えて、芳香族スルホン酸ナトリウムホルマリン縮合物（「デモールＳＮＢ」）を用いた以外は、実施例９と同様にして、１８０〜６００μｍの粒度分布範囲を有し、かつ、有効成分としてイミノクタジンアルベシル酸塩２０％とイプコナゾール３０％を含有する顆粒水和剤を得た。
(Comparative Example 9)
Example 9 is the same as Example 9 except that, instead of disodium N-stearoyl-L-glutamate (“Amisoft HS-21”), an aromatic sodium sulfonate formalin condensate (“Demol SNB”) was used. Similarly, a granular wettable powder having a particle size distribution range of 180 to 600 μm and containing 20% iminotazine albesylate and 30% ipconazole as active ingredients was obtained.
（比較例１０）
実施例１０において、Ｎ−ステアロイル−Ｌ−グルタミン酸２ナトリウム（「アミソフトＨＳ−２１」）に代えて、芳香族スルホン酸ナトリウムホルマリン縮合物（「デモールＳＮＢ」）を用いた以外は、実施例１０と同様にして、１８０〜１０００μｍの粒度分布範囲を有し、かつ、有効成分としてジチオピル４０％を含有する顆粒水和剤を得た。
(Comparative Example 10)
Example 10 is the same as Example 10 except that, instead of disodium N-stearoyl-L-glutamate (“Amisoft HS-21”), a sodium aromatic sulfonate formalin condensate (“Demol SNB”) was used. Similarly, a granular wettable powder having a particle size distribution range of 180 to 1000 μm and containing 40% dithiopyr as an active ingredient was obtained.
（比較例１１）
実施例１０において、Ｎ−ステアロイル−Ｌ−グルタミン酸２ナトリウム（「アミソフトＨＳ−２１」）に代えて、ポリカルボン酸ナトリウム（竹本油脂株式会社製の商品名「ニューカルゲンＷＧ−５」）を用いた以外は、実施例１０と同様にして、１８０〜１０００μｍの粒度分布範囲を有し、かつ、有効成分としてジチオピル４０％を含有する顆粒水和剤を得た。
(Comparative Example 11)
In Example 10, instead of disodium N-stearoyl-L-glutamate (“Amisoft HS-21”), sodium polycarboxylate (trade name “New Calgen WG-5” manufactured by Takemoto Yushi Co., Ltd.) was used. Except for the above, a granular wettable powder having a particle size distribution range of 180 to 1000 μm and containing 40% of dithiopyr as an active ingredient was obtained in the same manner as in Example 10.
（比較例１２）
実施例１１において、Ｎ−ステアロイル−Ｌ−グルタミン酸２ナトリウム（「アミソフトＨＳ−２１」）とＮ−ヤシ油脂肪酸アシル−Ｌ−グルタミン酸ナトリウム（「アミソフトＣＳ−１１」）に代えて、変性リグニンスルホン酸ナトリウム（「バニレックスＮ」）を用いた以外は、実施例１１と同様にして調製した。その結果、造粒物の形状が崩れやすい粉末状水和剤であって、有効成分としてベンフレセート３０％を含む粉末状水和剤を得た。
(Comparative Example 12)
In Example 11, instead of disodium N-stearoyl-L-glutamate (“Amisoft HS-21”) and N-coconut oil fatty acid acyl-L-sodium glutamate (“Amisoft CS-11”), modified lignin sulfonic acid Prepared in the same manner as in Example 11 except that sodium (“Vanilex N”) was used. As a result, a powdered wettable powder that easily collapsed in the shape of the granulated product and containing 30% benfrecetate as an active ingredient was obtained.
（比較例１３）
実施例１１において、Ｎ−ステアロイル−Ｌ−グルタミン酸２ナトリウム（「アミソフトＨＳ−２１」）とＮ−ヤシ油脂肪酸アシル−Ｌ−グルタミン酸ナトリウム（「アミソフトＣＳ−１１」）に代えて、芳香族スルホン酸ナトリウムホルマリン縮合物（「デモールＳＮＢ」）を用いた以外は、実施例１１と同様にして調製した。その結果、造粒物の形状が崩れやすい粉末状水和剤であって、有効成分としてベンフレセート３０％を含有する粉末状水和剤を得た。
(Comparative Example 13)
In Example 11, instead of disodium N-stearoyl-L-glutamate (“Amisoft HS-21”) and N-coconut oil fatty acid acyl-L-sodium glutamate (“Amisoft CS-11”), aromatic sulfonic acid Prepared in the same manner as in Example 11 except that sodium formalin condensate (“Demol SNB”) was used. As a result, a powdered wettable powder that easily collapsed in the shape of the granulated product and containing 30% benfrecetate as an active ingredient was obtained.
（比較例１４）
実施例１３において、Ｎ−ヤシ油脂肪酸アシル−Ｌ−グルタミン酸ナトリウム（「アミソフトＣＳ−１１」）に代えて、芳香族スルホン酸ナトリウムホルマリン縮合物（「デモールＳＮＢ」）を用いた以外は、実施例１３と同様にして、１８０〜１０００μｍの粒度分布範囲を有し、かつ、有効成分としてベンフレセート３０％を含有する顆粒水和剤を得た。
(Comparative Example 14)
In Example 13, except that an aromatic sodium sulfonate formalin condensate (“Demol SNB”) was used in place of N-coconut oil fatty acid acyl-L-glutamate sodium (“Amisoft CS-11”). In the same manner as in No. 13, a granular wettable powder having a particle size distribution range of 180 to 1000 μm and containing 30% benfrate as an active ingredient was obtained.
（比較例１５）
実施例１で作製したイミノクタジンアルベシル酸塩を５０％含有する粉末６０部に珪藻土（「ゼムライト３Ｙ」）１０部を混合し、更に２６％のドデシルベンゼンスルホン酸ナトリウム水溶液１１５．５部を噴霧した後、混合して混練物を得た。得られた混練物を４５℃で２時間乾燥させた後、更に混合して、不定形の顆粒に造粒した。得られた顆粒を更に４５℃で３時間乾燥させた後、篩い分け操作を行い、１２５〜４２５μｍの粒度分布範囲を有するイミノクタジンアルベシル酸塩３０％を有効成分として含む顆粒水和剤を得た。
(Comparative Example 15)
10 parts of diatomaceous earth (“Zemlite 3Y”) was mixed with 60 parts of powder containing 50% of iminotadine albecyl salt prepared in Example 1, and further 115.5 parts of 26% aqueous sodium dodecylbenzenesulfonate solution was sprayed. Thereafter, mixing was performed to obtain a kneaded product. The obtained kneaded material was dried at 45 ° C. for 2 hours, and further mixed to granulate into irregular shaped granules. The obtained granules were further dried at 45 ° C. for 3 hours and then subjected to a sieving operation to obtain a granule wettable powder containing 30% iminotazine albesylate having a particle size distribution range of 125 to 425 μm as an active ingredient. .
（比較例１６）
実施例２で作製したジチオピルを５０％含有する粉末６０部に珪藻土（「ゼムライト３Ｙ」）２０部を混合し、万能粉砕機（「Ｍ２０型」）で粉砕した。得られた混合物（平均粒子径約７μｍ）を混練機（「卓上型ニーダーＰＮＶ−５型」）に投入し、２６％のドデシルベンゼンスルホン酸ナトリウム水溶液７７部を滴下しながら混練した後、押出造粒機（「ＫＡＲ−１８０型」）０．５ｍｍスクリーンで押し出し造粒した。得られた顆粒を４５℃で３時間乾燥させた後、篩い分け操作を行い、１８０〜１０００μｍの粒度分布範囲を有するジチオピル３０％を有効成分として含む顆粒水和剤を得た。
(Comparative Example 16)
20 parts of diatomaceous earth (“Zemlite 3Y”) was mixed with 60 parts of powder containing 50% of dithiopyr prepared in Example 2, and pulverized with a universal pulverizer (“M20 type”). The obtained mixture (average particle diameter of about 7 μm) was put into a kneader (“desk type kneader PNV-5 type”) and kneaded while dripping 77 parts of a 26% aqueous solution of sodium dodecylbenzenesulfonate, followed by extrusion A granulator (“KAR-180 type”) was extruded and granulated with a 0.5 mm screen. The obtained granule was dried at 45 ° C. for 3 hours and then subjected to a sieving operation to obtain a granule wettable powder containing 30% of dithiopyr having a particle size distribution range of 180 to 1000 μm as an active ingredient.
（比較例１７）
実施例１で作製したイミノクタジンアルベシル酸塩を５０％含有する粉末８０部、ポリオキシエチレンジアルキルフェニルエーテルサルファートアンモニウム塩８部、ラウリル硫酸ナトリウム８部および増量剤としてクレー９部を混合し、前出の万能粉砕機を用いて粉砕して有効成分としてイミノクタジンアルベシル酸塩４０％を含有する水和剤を得た。
(Comparative Example 17)
80 parts of a powder containing 50% of iminotadine albesylate prepared in Example 1, 8 parts of polyoxyethylene dialkylphenyl ether sulfate ammonium salt, 8 parts of sodium lauryl sulfate and 9 parts of clay as an extender were mixed. A wettable powder containing 40% iminoctagine albesylate as an active ingredient was obtained by pulverization using the above-mentioned universal pulverizer.
表１に示すように実施例１〜１４で得た顆粒水和剤は、水中崩壊性、懸垂性および分散性の全ての項目が良好以上であった。 As shown in Table 1, the granule wettable powders obtained in Examples 1 to 14 were all good or better in all the items of disintegration in water, suspension and dispersibility.
表２に示したように、実施例１５で得た顆粒水和剤は、硬度の高い水（ＣＩＰＡＣ標準水Ｄ）での水中崩壊性、懸垂性および分散性の全ての項目が良好であった。 As shown in Table 2, the granule wettable powder obtained in Example 15 was good in all items of disintegration in water, suspension and dispersibility in water with high hardness (CIPAC standard water D). .
表３に示すように比較例１，２，４，６，７，９〜１１および１６で得た顆粒水和剤は水中崩壊性、懸垂性および分散性の全ての項目が不良であった。比較例３，５，８および１４で得た顆粒水和剤は、懸垂性と分散性がやや不良であった。比較例１２と１３で得た水和剤は、水中崩壊性、懸垂性および分散性は良好であったが、造粒性が不良であった。比較例１５で得た水和剤は、懸垂性および分散性は良好であったが、水中崩壊性が不良であった。また、比較例１〜１４および１６で得た顆粒水和剤は、実施例で得た顆粒水和剤と比較して水分散時の平均粒径が大きく、これは、凝集物が多く、界面活性剤の分散力不足のために生じたものと推測された。 As shown in Table 3, the granular wettable powders obtained in Comparative Examples 1, 2, 4, 6, 7, 9 to 11 and 16 were poor in all items of disintegration in water, suspension and dispersibility. The granule wettable powders obtained in Comparative Examples 3, 5, 8 and 14 were slightly poor in suspension and dispersibility. The wettable powder obtained in Comparative Examples 12 and 13 had good disintegration in water, suspension and dispersibility, but poor granulation. The wettable powder obtained in Comparative Example 15 had good suspension and dispersibility, but poor disintegration in water. In addition, the granule wettable powder obtained in Comparative Examples 1 to 14 and 16 had a larger average particle size at the time of water dispersion than the granule wettable powder obtained in the Examples, which had many aggregates, It was speculated that this occurred due to insufficient dispersion of the active agent.
［生物効果試験］
温室において１×１．５ｍの区画に慣行栽培中のキュウリ（品種：トップグリーン）を１薬剤当たり６株供試した。有効成分量が表に示した値となるように各実施例４と比較例１７で得た薬剤を水で希釈し、試験開始時１０葉期のキュウリに、各薬剤の水溶液を１週間間隔で計２回、背負い式全自動噴霧器を用いて十分量（３００Ｌ／１０ａ相当）を散布した。最終散布１８日後に各区全株の第６本葉より上位１０本葉についてその発病程度を調査し、発病葉率および発病度から下記の数式２によって防除価を算出した。薬害は適宜肉眼調査した。
[Biological effect test]
6 strains of cucumber (variety: top green) under conventional cultivation in a 1 × 1.5 m section in a greenhouse were tested. The drug obtained in each Example 4 and Comparative Example 17 was diluted with water so that the amount of the active ingredient became the value shown in the table, and the aqueous solution of each drug was added to the cucumber at the 10th leaf stage at the start of the test at intervals of 1 week. A sufficient amount (equivalent to 300 L / 10a) was sprayed twice using a backpack-type fully automatic sprayer. 18 days after the final spraying, the disease severity was investigated for the top 10 true leaves from the sixth true leaf of all the strains in each ward, and the control value was calculated by the following formula 2 from the disease leaf rate and the disease severity. The phytotoxicity was appropriately examined by visual inspection.
（発病の程度別指数）
０：発病なし。
５：僅かな発病が認められた。
１：発病面積率が５％未満であった。
２：発病面積率が５％以上２５％未満であった。
３：発病面積率が２５％以上５０％未満であった。
４：発病面積率が５０％以上であった。
(Index by disease severity)
0: No illness.
5: Slight onset was observed.
1: Disease area rate was less than 5%.
2: The disease area ratio was 5% or more and less than 25%.
3: The disease area ratio was 25% or more and less than 50%.
4: The disease area ratio was 50% or more.
（数式１）
発病度＝Σ（程度別発病葉数×指数）×１００÷（調査葉数×４）
(Formula 1)
Disease severity = Σ (number of diseased leaves by degree × index) × 100 ÷ (number of leaves surveyed × 4)
（数式２）
防除価＝（無処理の発病度−処理区の発病度）×１００÷無処理の発病度
(Formula 2)
Control value = (Severity of untreated-Severity of treated area) x 100 ÷ Severity of untreated
表４に示すように、実施例４で得た顆粒水和剤は、比較例１７で得た水和剤と同等の防除効果を有するものであり、薬害も生じないことが明らかである。
As shown in Table 4, it is clear that the granule wettable powder obtained in Example 4 has the same control effect as the wettable powder obtained in Comparative Example 17, and no phytotoxicity occurs.
Claims (11)
The N-acyl taurate with respect to the total mass of the agrochemical base, the N-acyl amino acid, the adsorption carrier, the formalin condensate of the aromatic sulfonate, the lignin sulfonate, and the N-acyl taurate A ratio of 0.5 to 10% by mass of the granulated wettable powder for agricultural and horticultural use according to claim 9 or 10.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2004011758A JP4421309B2 (en) | 2003-01-23 | 2004-01-20 | Agricultural and horticultural granule wettable powder |
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| Application Number | Priority Date | Filing Date | Title |
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| JP2003014640 | 2003-01-23 | ||
| JP2003315295 | 2003-09-08 | ||
| JP2004011758A JP4421309B2 (en) | 2003-01-23 | 2004-01-20 | Agricultural and horticultural granule wettable powder |
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| JP2005104959A JP2005104959A (en) | 2005-04-21 |
| JP4421309B2 true JP4421309B2 (en) | 2010-02-24 |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| BRPI0715137B8 (en) * | 2006-08-10 | 2021-10-19 | Nippon Soda Co | Agrochemical composition containing an agrochemically active ingredient having a restricted wetting capacity |
| TWI407905B (en) * | 2008-08-26 | 2013-09-11 | Nippon Soda Co | Water dispersible granule |
| JP7306961B2 (en) * | 2019-10-30 | 2023-07-11 | 水澤化学工業株式会社 | Adsorbent for basic amino acids |
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