JP6645016B2 - Pesticide granules - Google Patents
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Description
本発明は、農薬粒剤に関する。 The present invention relates to pesticide granules.
水稲の栽培においては、育苗箱に農薬製剤を施用することにより、該育苗箱で生育した幼苗を水田に移植するに際し、前記農薬製剤に含有される農薬活性化合物も水田に施用され、該農薬活性化合物の効力が持続している間は、水田へのあらたな農薬活性化合物の施用を必要としない。それ故、このような施用形態に好適な多くの農薬製剤が開発されている。 In the cultivation of paddy rice, a pesticide formulation is applied to a nursery box, so that when the seedlings grown in the nursery box are transplanted to a paddy field, the pesticide active compound contained in the pesticide formulation is also applied to the paddy field, As long as the potency of the compound is sustained, there is no need to apply a new pesticidally active compound to the paddy field. Therefore, many pesticide formulations suitable for such application forms have been developed.
一方、殺虫活性化合物としてシアントラニリプロールが知られている（例えば、特許文献１及び特許文献２参照）。
また、下記式（Ｉ）
Ｒ1は、ハロゲン原子又はＣ１−Ｃ４ハロアルキル基を表し、
Ｒ2は、水素原子、ハロゲン原子又はＣ１−Ｃ４アルキル基を表し、
Ｒ3は、水素原子、シアノ基、ハロゲン原子又はＣ１−Ｃ４アルキル基を表し、
Ｒ4は、水素原子又はＣ１−Ｃ４アルキル基を表し、
Ｒ5は、Ｃ１−Ｃ４アルキル基、Ｃ３−Ｃ７シクロアルキル基、（Ｃ３−Ｃ７シクロアルキル）Ｃ１−Ｃ４アルキル基、（Ｃ１−Ｃ４アルコキシ）カルボニル基、（Ｃ１−Ｃ４アルコキシ）カルボニルアミノ基、｛（Ｃ１−Ｃ４アルコキシ）カルボニル｝（Ｃ１−Ｃ４アルキル）アミノ基を表し、
Ｒ6は、ハロゲン原子を表す。〕
で示される化合物を含有する農薬粒剤が実用に供されている（例えば、特許文献３参照）。
On the other hand, cyantraniliprole is known as an insecticidal active compound (for example, see Patent Documents 1 and 2).
Further, the following formula (I)
R 1 represents a halogen atom or a C1-C4 haloalkyl group,
R 2 represents a hydrogen atom, a halogen atom or a C1-C4 alkyl group,
R 3 represents a hydrogen atom, a cyano group, a halogen atom or a C1-C4 alkyl group,
R 4 represents a hydrogen atom or a C1-C4 alkyl group,
R 5 is a C1-C4 alkyl group, a C3-C7 cycloalkyl group, a (C3-C7 cycloalkyl) C1-C4 alkyl group, a (C1-C4 alkoxy) carbonyl group, a (C1-C4 alkoxy) carbonylamino group, (C1-C4 alkoxy) carbonyl represents a (C1-C4 alkyl) amino group;
R 6 represents a halogen atom. ]
Pesticide granules containing the compound represented by the formula (1) have been put to practical use (for example, see Patent Document 3).
本発明は、シアントラニリプロールを含有し、その安定性が向上している農薬粒剤を提供することを課題とする。 An object of the present invention is to provide an agricultural chemical granule containing cyantraniliprole and having improved stability.
本発明者は、このような農薬粒剤を見出すべく検討の結果、シアントラニリプロール含有農薬粒剤１０ｇとイオン交換水９０ｇとを混合したときの２０℃におけるｐＨが８．３〜９．３の範囲を呈する粒剤とすることにより、シアントラニリプロールの安定性が向上することを見出した。
すなわち本発明は、以下の〔１〕〜〔７〕の通りである。
〔１〕 増量剤１ｇとイオン交換水９９ｇとを混合したときの２０℃におけるｐＨが９．０以上である増量剤、及びシアントラニリプロールを含有する農薬粒剤であって、該農薬粒剤１０ｇとイオン交換水９０ｇとを混合したときの２０℃におけるｐＨが８．３〜９．３の範囲である農薬粒剤。
〔２〕 病害抵抗性誘導活性化合物を含有する〔１〕に記載の農薬粒剤。
〔３〕 前記病害抵抗性誘導活性化合物がイソチアニル、チアジニル、プロベナゾール及びアシベンゾラル−Ｓ−メチルからなる群より選ばれる少なくとも１種である〔２〕に記載の農薬粒剤。
〔４〕 前記病害抵抗性誘導活性化合物がイソチアニルである〔２〕に記載の農薬粒剤。
〔５〕 ノニオン性界面活性剤を含有する〔１〕〜〔４〕のいずれかに記載の農薬粒剤。
〔６〕 前記増量剤が炭酸カルシウム、酸化マグネシウム、セピオライト及びアタパルジャイトからなる群より選ばれる少なくとも１種である〔１〕〜〔５〕のいずれかに記載の農薬粒剤。
〔７〕 前記増量剤が炭酸カルシウムである〔１〕〜〔５〕のいずれかに記載の農薬粒剤。
As a result of study to find such pesticide granules, the present inventor found that the pH at 20 ° C when 10 g of cyantraniliprole-containing pesticide granules and 90 g of ion-exchanged water were mixed was 8.3 to 9.3. It has been found that the stability of cyantraniliprole is improved by using a granule having the range of
That is, the present invention is as follows [1] to [7].
[1] A pesticide granule containing 1 g of a bulking agent and 99 g of ion-exchanged water and having a pH at 20 ° C. of 9.0 or more, and a pesticide granule containing cyantraniliprole, wherein the pesticide granule is used. A pesticide granule having a pH at 20 ° C of 8.3 to 9.3 when 10 g and 90 g of ion-exchanged water are mixed.
[2] The pesticide granule according to [1], which comprises a disease resistance-inducing active compound.
[3] The agricultural chemical granule according to [2], wherein the disease resistance-inducing active compound is at least one selected from the group consisting of isotianil, thiazinyl, probenazole, and acibenzolar-S-methyl.
[4] The pesticide granule according to [2], wherein the disease resistance-inducing compound is isotianil.
[5] The pesticide granule according to any one of [1] to [4], containing a nonionic surfactant.
[6] The pesticide granule according to any one of [1] to [5], wherein the extender is at least one selected from the group consisting of calcium carbonate, magnesium oxide, sepiolite and attapulgite.
[7] The pesticide granule according to any one of [1] to [5], wherein the extender is calcium carbonate.
本発明により、シアントラニリプロールを含有し、その安定性が向上している農薬粒剤を提供することができる。 According to the present invention, an agricultural chemical granule containing cyantraniliprole and having improved stability can be provided.
本発明の農薬粒剤（以下、本粒剤と記す）はシアントラニリプロール（cyantraniliprole）を含有する。本粒剤におけるシアントラニリプロールの含有量は、通常０．１〜５重量％、好ましくは０．５〜２重量％の範囲である。 The pesticide granule of the present invention (hereinafter, referred to as the present granule) contains cyantraniliprole. The content of cyantraniliprole in the present granules is generally in the range of 0.1 to 5% by weight, preferably 0.5 to 2% by weight.
本粒剤は、増量剤１ｇとイオン交換水９９ｇとを混合したときの２０℃におけるｐＨ（以下、増量剤のｐＨと記す）が９．０以上である増量剤（以下、本増量剤と記す）を含有する。増量剤のｐＨは、増量剤１ｇを１００ｍＬ容量のスクリュー管等の容器に入れ、２０℃に温度調整したイオン交換水９９ｇを加えて１分間混合した後、ガラス電極式のｐＨメーターのガラス電極を混合液に浸漬して静置し、５分後に測定される値である。本発明においてイオン交換水とは、電気伝導率が０．５ｍＳ／ｍ以下の水を指す。本増量剤としては、炭酸カルシウム（増量剤のｐＨ：９．７）、酸化マグネシウム（増量剤のｐＨ：１０．８）、セピオライト（増量剤のｐＨ：９．５）及びアタパルジャイト（増量剤のｐＨ：９．１）が挙げられる。また、本発明においては、増量剤のｐＨが９．０〜１１．０の範囲である増量剤が好ましく、炭酸カルシウムがさらに好ましい。
本粒剤における本増量剤の合計含有量は、通常０．０１〜５０重量％、好ましくは０．０５〜２０重量％の範囲である。
The present granule has a pH at 20 ° C. (hereinafter, referred to as the pH of the extender) of 9.0 g or more when 1 g of the extender and 99 g of ion-exchanged water are mixed (hereinafter, referred to as the present extender). ). After adding 1 g of the bulking agent to a container such as a screw tube having a capacity of 100 mL, adding 99 g of ion-exchanged water whose temperature was adjusted to 20 ° C. and mixing for 1 minute, the pH of the glass electrode of the glass electrode type pH meter was measured. It is a value measured after immersion in the mixed solution and standing after 5 minutes. In the present invention, ion-exchanged water refers to water having an electric conductivity of 0.5 mS / m or less. Examples of the bulking agent include calcium carbonate (pH of the bulking agent: 9.7), magnesium oxide (pH of the bulking agent: 10.8), sepiolite (pH of the bulking agent: 9.5), and attapulgite (pH of the bulking agent). : 9.1). In the present invention, the extender having a pH of 9.0 to 11.0 is preferable, and calcium carbonate is more preferable.
The total content of the extender in the present granules is generally in the range of 0.01 to 50% by weight, preferably 0.05 to 20% by weight.
本粒剤は、本粒剤１０ｇとイオン交換水９０ｇとを混合したときの２０℃におけるｐＨ（以下、本粒剤のｐＨと記す）が８．３〜９．３の範囲であることを特徴とする。本粒剤のｐＨは、本粒剤１０ｇを、粉砕機を用いて粉砕し、得られる粉砕物を１００ｍＬ容量のスクリュー管等の容器に入れ、２０℃に温度調整したイオン交換水９０ｇを加えて１分間混合した後、ガラス電極式のｐＨメーターのガラス電極を混合液に浸漬して静置し、５分後に測定される値である。粒剤の粉砕は、コーヒーミル（ミニブレンダーＭＢ−２、メリタ製）等の粉砕機を用い、１分程度粉砕することにより行うことができる。 The present granule is characterized in that the pH at 20 ° C. (hereinafter referred to as the pH of the present granule) when 10 g of the present granule is mixed with 90 g of ion-exchanged water is in the range of 8.3 to 9.3. And The pH of the present granules is obtained by crushing 10 g of the present granules using a crusher, placing the obtained crushed product in a container such as a 100-mL screw tube, and adding 90 g of ion-exchanged water whose temperature has been adjusted to 20 ° C. After mixing for 1 minute, the glass electrode of a glass electrode type pH meter is immersed in the mixed solution and allowed to stand, and the value is measured after 5 minutes. The pulverization of the granules can be performed by using a pulverizer such as a coffee mill (Mini Blender MB-2, manufactured by Melita) or the like for about 1 minute.
本粒剤は、ノニオン性界面活性剤を含有することが好ましい。かかるノニオン性界面活性剤としては、ポリオキシエチレンアルキルエーテル、ポリオキシエチレンアルキルアリールエーテル、ポリオキシエチレンラノリンアルコール、ポリオキシエチレンアルキルフェノールホルマリン縮合物、ポリオキシエチレンソルビタン脂肪酸エステル、ポリオキシエチレングリセリルモノ脂肪酸エステル、ポリオキシプロピレングリコールモノ脂肪酸エステル、ポリオキシエチレンソルビトール脂肪酸エステル、ポリオキシエチレンヒマシ油誘導体、ポリオキシエチレン脂肪酸エステル、高級脂肪酸グリセリンエステル、ソルビタン脂肪酸エステル、ショ糖脂肪酸エステル、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、ポリオキシエチレン脂肪酸アミド、アルキロールアミド、ポリオキシエチレンアルキルアミン等が挙げられ、ポリオキシエチレンアルキルエーテル及びポリオキシエチレンアルキルアリールエーテルからなる群より選ばれる少なくとも１種が好ましく、ポリオキシエチレントリスチリルフェニルエーテルがさらに好ましい。
本粒剤がノニオン性界面活性剤を含有する場合、その合計含有量は、通常０．１〜５重量％、好ましくは０．５〜２重量％の範囲である。
The present granules preferably contain a nonionic surfactant. Such nonionic surfactants include polyoxyethylene alkyl ether, polyoxyethylene alkyl aryl ether, polyoxyethylene lanolin alcohol, polyoxyethylene alkylphenol formalin condensate, polyoxyethylene sorbitan fatty acid ester, polyoxyethylene glyceryl mono fatty acid ester , Polyoxypropylene glycol monofatty acid ester, polyoxyethylene sorbitol fatty acid ester, polyoxyethylene castor oil derivative, polyoxyethylene fatty acid ester, higher fatty acid glycerin ester, sorbitan fatty acid ester, sucrose fatty acid ester, polyoxyethylene polyoxypropylene block Polymer, polyoxyethylene fatty acid amide, alkylolamide, polyoxyethylene Alkylamines, and the like, is preferably at least one selected from the group consisting of polyoxyethylene alkyl ethers and polyoxyethylene alkyl aryl ethers, polyoxyethylene tristyryl phenyl ether is more preferable.
When the present granules contain a nonionic surfactant, the total content is usually in the range of 0.1 to 5% by weight, preferably 0.5 to 2% by weight.
本粒剤のｐＨが８．３〜９．３の範囲を呈するように、本増量剤の含有量を前記の範囲内で調整することにより、本粒剤を得ることができる。また、本粒剤は、本粒剤のｐＨが８．３〜９．３の範囲を呈するように、増量剤のｐＨが９．０未満である増量剤（以下、ｐＨ９．０未満の増量剤と記す）、結合剤、溶剤、安定剤、防腐剤、着色料及び香料等の製剤用補助剤を含有していてもよい。 The present granules can be obtained by adjusting the content of the present extender within the above range so that the pH of the present granules exhibits a range of 8.3 to 9.3. In addition, the present granule is a bulking agent having a pH of less than 9.0 (hereinafter referred to as a bulking agent having a pH of less than 9.0) so that the pH of the present granule exhibits a range of 8.3 to 9.3. ), A formulation auxiliary such as a binder, a solvent, a stabilizer, a preservative, a coloring agent and a fragrance may be contained.
ｐＨ９．０未満の増量剤としては、例えば、ロウ石が挙げられる。
本粒剤がｐＨ９．０未満の増量剤を含有する場合、その合計含有量は、通常０．５０〜９５重量％、好ましくは５０〜９５重量％の範囲である。
Examples of the extender having a pH of less than 9.0 include fluorite.
When the present granules contain a bulking agent having a pH of less than 9.0, the total content is usually in the range of 0.50 to 95% by weight, preferably 50 to 95% by weight.
かかる結合剤としては、例えば、カルボキシメチルセルロースナトリウム、ヒドロキシプロピルメチルセルロース、メチルセルロース、メチルエチルセルロース、ヒドロキシプロピルセルロース、ポリアクリル酸ナトリウム、トラガントガム、ポリビニルピロリドン、ポリビニルアルコール、アルファー澱粉、デキストリン、アルギン酸及びアルギン酸ナトリウムが挙げられ、アルファー澱粉が好ましい。
本粒剤が結合剤を含有する場合、その合計含有量は、通常１〜２０重量％、好ましくは１〜１０重量％の範囲である。
結合剤としてアルファー澱粉を含有する本粒剤は、水中非崩壊農薬粒剤である。本発明において水中非崩壊農薬粒剤とは、水中における崩壊時間が２４時間以上である農薬粒剤を意味する。水中における崩壊時間とは、直径９ｃｍのガラス製シャーレに３度硬水５０ｍＬを入れて静置し、そこへ供試粒剤５粒をほぼ均一になるように投入し、その直後から供試粒剤が原形をとどめなくなるまでに要する時間である。
Such binders include, for example, sodium carboxymethylcellulose, hydroxypropylmethylcellulose, methylcellulose, methylethylcellulose, hydroxypropylcellulose, sodium polyacrylate, tragacanth, polyvinylpyrrolidone, polyvinyl alcohol, alpha starch, dextrin, alginic acid and sodium alginate. , Alpha starch is preferred.
When the present granules contain a binder, the total content is usually in the range of 1 to 20% by weight, preferably 1 to 10% by weight.
The present granules containing alpha-starch as a binder are non-disintegrating pesticide granules in water. In the present invention, the underwater non-disintegrating pesticide granule means an agrochemical granule having a disintegration time in water of 24 hours or more. The disintegration time in water means that 50 mL of hard water is placed in a glass dish of 9 cm in diameter three times and left to stand, and 5 granules of the test granules are poured so as to be substantially uniform. Is the time it takes for the original to stay intact.
本粒剤は、シアントラニリプロールに加えて、その他の農薬活性化合物を含有することができる。かかるその他の農薬活性化合物としては、例えば、殺虫活性化合物、殺菌活性化合物、昆虫成長制御活性化合物、除草活性化合物及び植物成長制御活性化合物が挙げられる。本発明においては、病害抵抗性誘導剤の有効成分である病害抵抗性誘導活性化合物の使用が好ましい。病害抵抗性誘導剤は、病原体に直接作用するのではなく、植物の病害抵抗性を発現させることにより病害を防除する薬剤であり、主にいもち病の防除に利用されている。本発明においては、病害抵抗性誘導活性化合物として、チアジニル（tiadinil）、イソチアニル（isotianil）、プロベナゾール（probenazole）及びアシベンゾラル−Ｓ−メチル（acibenzolar-S-methyl）からなる群より選ばれる少なくとも１種が好ましく、これらの中でもイソチアニルが好ましい。本粒剤がイソチアニルを含有する場合、イソチアニルの溶出とシアントラニリプロールの安定化とを両立させることができるため、有用である。
本粒剤が他の農薬活性化合物を含有する場合、その合計含有量は、通常０．１〜５０重量％、好ましくは０．５〜１０重量％の範囲である。
The present granules can contain other pesticidally active compounds in addition to cyantraniliprole. Such other pesticidally active compounds include, for example, insecticidal active compounds, fungicidal active compounds, insect growth controlling active compounds, herbicidal active compounds and plant growth controlling active compounds. In the present invention, it is preferable to use a disease resistance-inducing active compound which is an active ingredient of the disease resistance inducer. Disease resistance inducers are agents that do not act directly on pathogens but control disease by expressing plant disease resistance, and are mainly used for controlling blast. In the present invention, at least one selected from the group consisting of thiazinyl (tiadinil), isotianil (isotianil), probenazole (probenazole) and acibenzolar-S-methyl (acibenzolar-S-methyl) is used as the disease resistance inducing active compound. Preferably, among these, isotianil is preferable. When the present granule contains isotianil, it is useful because both elution of isotianil and stabilization of cyantraniliprole can be achieved at the same time.
When the present granules contain other pesticidally active compounds, the total content is usually in the range of 0.1 to 50% by weight, preferably 0.5 to 10% by weight.
本粒剤は、シアントラニリプロール、本増量剤、並びに必要に応じ、製剤用補助剤及び／又は他の農薬活性化合物を含有する混合物に、水を加えて混練して得られた混練物を造粒し、次いで、得られた造粒物を乾燥し、必要により解砕、篩分、整粒等を行うことにより製造することができる。混練の際に加えられる水の量は、前記混合物１００重量部に対して、通常３〜５０重量部である。混練の際に用いられる練合機としては、ニーダー、ナウターミキサー、レディゲミキサー、バーチカルグラニュレーター等が挙げられる。 This granule is obtained by kneading a mixture containing cyantraniliprole, the present bulking agent, and, if necessary, water with a mixture containing a formulation auxiliary agent and / or other pesticidally active compounds. It can be manufactured by granulating, then drying the obtained granulated material and, if necessary, crushing, sieving, sizing and the like. The amount of water added during kneading is usually 3 to 50 parts by weight based on 100 parts by weight of the mixture. Examples of the kneading machine used for kneading include a kneader, a Nauter mixer, a Loedige mixer, a vertical granulator, and the like.
前記混練物を押出造粒する際は、通常０．５〜２．０ｍｍφ、好ましくは０．７〜１．５ｍｍφのスクリーンを用いて行われる。押出造粒して得られる造粒物は、通常３０〜９０℃、好ましくは３０〜８０℃で乾燥される。乾燥された後の本粒剤の粒長は、通常０．５〜６．０ｍｍ、好ましくは０．７〜４．０ｍｍである。なお、本発明における粒長とは、粒が取り得る最大長さを意味する。押出造粒機としては、スクリュー型押出造粒機、ロール型押出造粒機、ディスクペレッター型押出造粒機、ペレットミル型押出造粒機、バスケット型押出造粒機、ブレード型押出造粒機、オシレーティング型押出造粒機、ギア式押出造粒機、リングダイス式押出造粒機等が挙げられる。 When extruding and granulating the kneaded material, it is usually performed using a screen having a diameter of 0.5 to 2.0 mmφ, preferably 0.7 to 1.5 mmφ. The granulated product obtained by extrusion granulation is usually dried at 30 to 90 ° C, preferably 30 to 80 ° C. The particle length of the present granules after drying is usually 0.5 to 6.0 mm, preferably 0.7 to 4.0 mm. In addition, the grain length in the present invention means the maximum length that a grain can take. Examples of the extrusion granulator include a screw extrusion granulator, a roll extrusion granulator, a disk pelletizer extrusion granulator, a pellet mill extrusion granulator, a basket extrusion granulator, and a blade extrusion granulator. Machine, oscillating type extrusion granulator, gear type extrusion granulator, ring die type extrusion granulator and the like.
本粒剤は、水稲育苗箱処理用途に適している。水稲育苗箱とはその大きさが３０ｃｍ×６０ｃｍ（内径：２８ｃｍ×５８ｃｍ）であり、イネ苗を田植えまで（一般的には２０〜４０日間）育苗する苗箱である。水稲育苗箱処理とは、田植え後、本田で発生する病害虫を防除するために、育苗箱に粒剤を散布する簡易防除手段である。 This granule is suitable for use in processing rice nursery boxes. The paddy rice nursery box has a size of 30 cm × 60 cm (inner diameter: 28 cm × 58 cm), and is a nursery box for raising rice seedlings until planting rice (generally for 20 to 40 days). The paddy rice nursery box treatment is a simple control means for spraying granules on a nursery box in order to control pests and insects that occur in Honda after planting rice.
次に本発明を製造例、試験例等によりさらに詳しく説明するが、本発明はこれらの例のみに限定されるものではない。 Next, the present invention will be described in more detail with reference to Production Examples and Test Examples, but the present invention is not limited to only these examples.
参考製造例１ 粉状農薬組成物１の調製
７０．０重量部のシアントラニリプロール及び３０．０重量部のロウ石（勝光山クレーＳ、勝光山鉱業所製）を均一に混合し、遠心粉砕機にて全量粉砕して、体積中位径が３．３μｍ（ＭＡＬＶＥＲＮ製ＭＡＳＴＥＲＳＩＺＥＲ２０００により測定）のシアントラニリプロールを含有する粉状農薬組成物（以下、粉状農薬組成物１と記す。）を得た。
Reference Production Example 1 Preparation of Powdery Pesticide Composition 1 70.0 parts by weight of cyantraniliprole and 30.0 parts by weight of ragite (Katsumitsuyama Clay S, manufactured by Katsumitsuyama Mining Works) were uniformly mixed and centrifuged. A pulverulent pesticide composition containing cyantraniliprole having a volume median diameter of 3.3 μm (measured by MASTERSIZER 2000 manufactured by MALVERN) and pulverized by a pulverizer (hereinafter referred to as powdery pesticide composition 1). I got
参考製造例２ 粉状農薬組成物２の調製
７０．０重量部のイソチアニル及び３０．０重量部のロウ石（勝光山クレーＳ、勝光山鉱業所製）を均一に混合し、遠心粉砕機にて全量粉砕して、体積中位径が４．１μｍ（ＭＡＬＶＥＲＮ製ＭＡＳＴＥＲＳＩＺＥＲ２０００により測定）のイソチアニルを含有する粉状農薬組成物（以下、粉状農薬組成物２と記す。）を得た。
Reference Production Example 2 Preparation of Powdered Pesticide Composition 2 70.0 parts by weight of isotianil and 30.0 parts by weight of laurite (Katsumitsuyama Clay S, manufactured by Katsumitsuyama Mining Works) were uniformly mixed and centrifuged. And pulverized to obtain a powdery pesticide composition containing isotianil having a volume median diameter of 4.1 μm (measured by MASTERSIZER2000 manufactured by MALVERN) (hereinafter referred to as powdery pesticide composition 2).
製造例１ 本発明農薬粒剤１の調製
粉状農薬組成物１ １．１重量部、粉状農薬組成物２ ２．９重量部、アルファー澱粉（アミロックスNo.1A、日本コーンスターチ製）５．０重量部、炭酸カルシウム（ＳＳ♯８０、日東粉化工業製）１．０重量部及びロウ石（勝光山クレーＳ、勝光山鉱業所製）８９．０重量部の混合物に、ノニオン性界面活性剤（ポリオキシエチレントリスチリルフェニルエーテル、Sorpol T-20、東邦化学工業製）１．０重量部を含有する水 約２０重量部を加えて、混練した。得られた混練物約１．０kgを、１．２ｍｍφのスクリーン付きバスケット型押出造粒機（ＨＵ−Ｇ型畑式造粒機、株式会社畑鐵工所製）に投入し、１０秒間該造粒機を運転させた。１０秒間で得られた造粒物を取り除いた後、該造粒機の運転を再開し、３０秒間で得られた造粒物を７０℃で３０分間乾燥して、本発明農薬粒剤１を得た。
Production Example 1 Preparation of Pesticide Granule 1 of the Present Invention Powdery pesticide composition 1 1.1 parts by weight, powdery pesticide composition 2 2.9 parts by weight, alpha starch (Amilox No. 1A, manufactured by Nippon Cornstarch) 5.0 A nonionic surfactant was added to a mixture of 1.0 parts by weight of calcium carbonate (SS @ 80, manufactured by Nitto Powder Chemical Industry) and 89.0 parts by weight of rubble (Katsumitsuyama Clay S, manufactured by Katsumitsu Mining Co., Ltd.). (Polyoxyethylene tristyryl phenyl ether, Sorpol T-20, manufactured by Toho Chemical Industry) About 20 parts by weight of water containing 1.0 part by weight was added and kneaded. About 1.0 kg of the obtained kneaded material was put into a basket-type extrusion granulator (HU-G type field granulator, manufactured by Hata Iron Works Co., Ltd.) having a screen of 1.2 mmφ, and the granulation was performed for 10 seconds. The granulator was operated. After removing the granules obtained in 10 seconds, the operation of the granulator was restarted, and the granules obtained in 30 seconds were dried at 70 ° C. for 30 minutes to obtain the pesticide granule 1 of the present invention. Obtained.
製造例２ 本発明農薬粒剤２の調製
炭酸カルシウム（ＳＳ♯８０、日東粉化工業製）１．０重量部を３．０重量部とし、ロウ石（勝光山クレーＳ、勝光山鉱業所製）８９．０重量部を８７．０重量部とした以外は製造例１と同様の操作を行い、本発明農薬粒剤２を得た。
Production Example 2 Preparation of pesticide granule 2 of the present invention 1.0 part by weight of calcium carbonate (SS @ 80, manufactured by Nitto Powder Chemical Co., Ltd.) was changed to 3.0 parts by weight, and wax stone (Katsumitsuyama Clay S, Katsumitsuyama Mining Works) ) The same operation as in Production Example 1 was carried out except that 89.0 parts by weight was changed to 87.0 parts by weight to obtain the pesticide granule 2 of the present invention.
製造例３ 本発明農薬粒剤３の調製
炭酸カルシウム（ＳＳ♯８０、日東粉化工業製）１．０重量部を５．０重量部とし、ロウ石（勝光山クレーＳ、勝光山鉱業所製）８９．０重量部を８５．０重量部とした以外は製造例１と同様の操作を行い、本発明農薬粒剤３を得た。
Production Example 3 Preparation of pesticide granule 3 of the present invention 1.0 part by weight of calcium carbonate (SS @ 80, manufactured by Nitto Powder Chemical Co., Ltd.) was changed to 5.0 parts by weight, and limestone (Katsumitsuyama Clay S, Katsumitsuyama Mining Works) ) The same operation as in Production Example 1 was carried out except that 89.0 parts by weight was changed to 85.0 parts by weight to obtain the pesticide granule 3 of the present invention.
製造例４ 本発明農薬粒剤４の調製
炭酸カルシウム（ＳＳ♯８０、日東粉化工業製）１．０重量部を８．０重量部とし、ロウ石（勝光山クレーＳ、勝光山鉱業所製）８９．０重量部を８２．０重量部とした以外は製造例１と同様の操作を行い、本発明農薬粒剤４を得た。
Production Example 4 Preparation of pesticide granule 4 of the present invention 1.0 part by weight of calcium carbonate (SS # 80, manufactured by Nitto Powder Chemical Co., Ltd.) was changed to 8.0 parts by weight, and laurite (Katsumitsuyama Clay S, manufactured by Katsumitsusan Mining Works) was used. ) Except that 89.0 parts by weight was changed to 82.0 parts by weight, the same operation as in Production Example 1 was carried out to obtain the pesticide granule 4 of the present invention.
製造例５ 本発明農薬粒剤５の調製
炭酸カルシウム（ＳＳ♯８０、日東粉化工業製）１．０重量部に代えて、酸化マグネシウム（和光純薬製）０．１重量部を用い、ロウ石（勝光山クレーＳ、勝光山鉱業所製）８９．０重量部を８９．９重量部とした以外は製造例１と同様の操作を行い、本発明農薬粒剤５を得た。
Preparation Example 5 Preparation of Pesticide Granule 5 of the Present Invention Instead of 1.0 part by weight of calcium carbonate (SS @ 80, manufactured by Nitto Powder Chemical Industry), 0.1 part by weight of magnesium oxide (manufactured by Wako Pure Chemical Industries) was used, and wax was used. The same operation as in Production Example 1 was carried out except that 89.0 parts by weight of the stone (Katsumitsuyama Clay S, manufactured by Katsumitsu Mining Co., Ltd.) was changed to 89.9 parts by weight to obtain pesticide granule 5 of the present invention.
製造例６ 本発明農薬粒剤６の調製
炭酸カルシウム（ＳＳ♯８０、日東粉化工業製）１．０重量部に代えて、セピオライト（ミラクレーＰ３００、近江鉱業製）１０．０重量部を用い、ロウ石（勝光山クレーＳ、勝光山鉱業所製）８９．０重量部を８０．０重量部とした以外は製造例１と同様の操作を行い、本発明農薬粒剤６を得た。
Production Example 6 Preparation of Pesticide Granule 6 of the Present Invention Instead of 1.0 part by weight of calcium carbonate (SS # 80, manufactured by Nitto Powder Chemical Industry), 10.0 parts by weight of sepiolite (Miraclay P300, manufactured by Omi Mining) was used. The same operation as in Production Example 1 was performed except that 89.0 parts by weight of wax stone (Katsumitsuyama Clay S, manufactured by Katsumitsu Mining Co., Ltd.) was used to obtain pesticide granule 6 of the present invention.
製造例７ 本発明農薬粒剤７の調製
炭酸カルシウム（ＳＳ♯８０、日東粉化工業製）１．０重量部に代えて、アタパルジャイト（ＡＴＴＡ−２００、近江鉱業製）１０．０重量部を用い、ロウ石（勝光山クレーＳ、勝光山鉱業所製）８９．０重量部を８０．０重量部とした以外は製造例１と同様の操作を行い、本発明農薬粒剤７を得た。
Production Example 7 Preparation of pesticide granule 7 of the present invention 10.0 parts by weight of attapulgite (ATTA-200, manufactured by Omi Mining) was used instead of 1.0 part by weight of calcium carbonate (SS # 80, manufactured by Nitto Powder Chemical Industry). A pesticide granule 7 of the present invention was obtained in the same manner as in Production Example 1 except that 89.0 parts by weight of wax stone (Katsumitsuyama Clay S, manufactured by Katsumitsu Mining Co., Ltd.) was changed to 80.0 parts by weight.
比較製造例１ 比較農薬粒剤１の調製
炭酸カルシウム（ＳＳ♯８０、日東粉化工業製）１．０重量部を９０．０重量部とし、ロウ石（勝光山クレーＳ、勝光山鉱業所製）を用いなかったこと以外は製造例１と同様の操作を行い、比較農薬粒剤１を得た。
Comparative Production Example 1 Preparation of Comparative Pesticide Granule 1 Preparation of 1.0 part by weight of calcium carbonate (SS @ 80, manufactured by Nitto Powder Chemical Co., Ltd.) as 90.0 parts by weight, and laurite (Katsumitsuyama Clay S, Katsumitsuyama Mining Works) ) Was carried out in the same manner as in Production Example 1, except that Comparative Pesticide Granule 1 was obtained.
本発明農薬粒剤１〜７及び比較農薬粒剤１について、農薬粒剤１０ｇとイオン交換水９０ｇとを混合したときの２０℃におけるｐＨを測定した。結果を表１に示す。 With respect to the pesticide granules 1 to 7 of the present invention and the comparative pesticide granule 1, the pH at 20 ° C. when 10 g of the pesticide granules and 90 g of ion-exchanged water were mixed was measured. Table 1 shows the results.
試験例１
スターラー上に設置した水槽に投込式恒温装置を取り付け、水槽内に水道水を入れた。容量１Ｌのガラスビーカーに３度硬水９００ｍＬ及び撹拌子を入れ、該ビーカーを該水槽内に設置した。このとき、該撹拌子が回転する位置に該ビーカーを設置した。該スターラーを作動させて該ビーカー内の水を撹拌すると共に、該装置を作動させて該ビーカー内のの水温を２５℃に調整した。農薬粒剤２７ｍｇを該ビーカー内に投入し、投入２１日後に、水中のシアントラニリプロール濃度を、ＨＰＬＣを用いて測定した。そして、下記式（１）により、水中溶出率を求めた。
式（１） 水中溶出率（％）＝２１日後の水中のシアントラニリプロール濃度（ｐｐｍ）／シアントラニリプロールの最大溶出濃度（ｐｐｍ）×１００
ただし、上記式（１）において、シアントラニリプロールの最大溶出濃度とは、農薬粒剤に含有されるシアントラニリプロールが全量水中に溶出したときの濃度である。
結果を表２に示す。
Test example 1
A water bath installed on a stirrer was equipped with a water-immersion type thermostat, and tap water was poured into the water bath. 900 mL of hard water three times and a stirrer were placed in a glass beaker having a capacity of 1 L, and the beaker was set in the water tank. At this time, the beaker was set at a position where the stirrer rotated. The stirrer was operated to stir the water in the beaker, and the device was operated to adjust the temperature of the water in the beaker to 25 ° C. 27 mg of pesticide granules were charged into the beaker, and 21 days after the introduction, the concentration of cyantraniliprole in water was measured using HPLC. Then, the dissolution rate in water was determined by the following equation (1).
Formula (1) Dissolution rate in water (%) = concentration of cyantraniliprole in water after 21 days (ppm) / maximum dissolution concentration of cyantraniliprole (ppm) × 100
However, in the above formula (1), the maximum elution concentration of cyantraniliprole is the concentration of cyantraniliprole contained in the pesticide granules when the total amount elutes into water.
Table 2 shows the results.
試験例２
農薬粒剤５０ｇをアルミ内装クラフト袋に入れ、５４℃の恒温器中で２週間保存した。保存後の農薬粒剤中のシアントラニリプロール含有量をＨＰＬＣを用いて定量し、下記式（２）により、分解率を求めた。
式（２） 分解率（％）＝１００−（保存後の農薬粒剤中のシアントラニリプロール含有量／保存前の農薬粒剤中のシアントラニリプロール含有量×１００）
結果を表３に示す。
Test example 2
A pesticide granule (50 g) was placed in an aluminum interior kraft bag and stored in a 54 ° C. thermostat for 2 weeks. The content of cyantraniliprole in the pesticide granules after storage was quantified using HPLC, and the decomposition rate was determined by the following formula (2).
Formula (2) Decomposition rate (%) = 100− (cyantraniliprole content in pesticide granule after storage / cyantraniliprole content in pesticide granule before storage × 100)
Table 3 shows the results.
Claims (3)
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Free format text: JAPANESE INTERMEDIATE CODE: R313531 |
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| R350 | Written notification of registration of transfer |
Free format text: JAPANESE INTERMEDIATE CODE: R350 |