JP2021066712A - Agrochemical granule - Google Patents

Agrochemical granule Download PDF

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JP2021066712A
JP2021066712A JP2019195003A JP2019195003A JP2021066712A JP 2021066712 A JP2021066712 A JP 2021066712A JP 2019195003 A JP2019195003 A JP 2019195003A JP 2019195003 A JP2019195003 A JP 2019195003A JP 2021066712 A JP2021066712 A JP 2021066712A
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weight
pesticide
granules
oxazosulfyl
clay
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JP7388125B2 (en
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三慶 山根
Mitsuyoshi Yamane
三慶 山根
崇 柴山
Takashi Shibayama
崇 柴山
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Sumitomo Chemical Co Ltd
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Abstract

To provide an oxazosulfyl-containing agrochemical granule that controls the elution of oxazosulfyl contained therein and suppresses changes in physical chemical properties with time.SOLUTION: An agrochemical granule contains oxazosulfyl 0.5-5 wt.%, α-starch 4-7 wt.%, a nonionic surfactant 0.1-5 wt.%, calcium carbonate 3-10 wt.%, and clay 50-92 wt.%.SELECTED DRAWING: None

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(例えば、特許文献1参照)。 In the cultivation of paddy rice, by applying a pesticide preparation to the seedling raising box, when the seedlings grown in the seedling raising box are transplanted to the paddy field, the pesticide active compound contained in the pesticide preparation is also applied to the paddy field, and the pesticide activity is applied. As long as the efficacy of the compound lasts, no new application of the pesticide active compound to the paddy field is required. Therefore, many pesticide preparations suitable for such application forms have been developed (see, for example, Patent Document 1).

一方、殺虫活性化合物としてオキサゾスルフィルが知られている(例えば、特許文献2及び特許文献3参照)。 On the other hand, oxazosulfyl is known as an insecticidal active compound (see, for example, Patent Document 2 and Patent Document 3).

特開2016−166149号公報Japanese Unexamined Patent Publication No. 2016-166149 特開2017−131236号公報Japanese Unexamined Patent Publication No. 2017-131236 国際公開第2017/104592号International Publication No. 2017/10459

本発明は、含有されるオキサゾスルフィルの溶出が制御され、且つ物理化学的性状の経時変化が抑制された、オキサゾスルフィル含有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 oxazosulfyl-containing pesticide granule in which the elution of the contained oxazosulfyl is controlled and the change in physicochemical properties with time is suppressed.

本発明者等は、このような農薬粒剤を見出すべく検討の結果、オキサゾスルフィル、アルファ澱粉、ノニオン性界面活性剤、炭酸カルシウム及びクレーをそれぞれ特定量含有する農薬粒剤とすることにより、該粒剤に含有されるオキサゾスルフィルの溶出が制御され、また、該粒剤の物理化学的性状の経時変化が抑制されることを見出した。
すなわち本発明は、以下の〔1〕〜〔5〕の通りである。
〔1〕 オキサゾスルフィル0.5〜5重量%、
アルファ澱粉4〜7重量%、
ノニオン性界面活性剤0.1〜5重量%、
炭酸カルシウム3〜10重量%、及び
クレー50〜92重量%
を含有する農薬粒剤。
〔2〕 前記ノニオン性界面活性剤が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種のノニオン性界面活性剤である〔1〕に記載の農薬粒剤。
〔3〕 前記ノニオン性界面活性剤がポリオキシエチレントリスチリルフェニルエーテルである〔1〕に記載の農薬粒剤。
〔4〕 前記クレーがロウ石である〔1〕〜〔3〕のいずれかに記載の農薬粒剤。
〔5〕 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9.4以上である〔1〕〜〔4〕のいずれかに記載の農薬粒剤。
As a result of studies to find such pesticide granules, the present inventors have made pesticide granules containing oxazosulfyl, alpha starch, nonionic surfactant, calcium carbonate and clay in specific amounts. It has been found that the elution of oxazosulfyl contained in the granules is controlled, and the change over time in the physicochemical properties of the granules is suppressed.
That is, the present invention is as follows [1] to [5].
[1] Oxadiazolefil 0.5 to 5% by weight,
Alpha starch 4-7% by weight,
Nonionic surfactant 0.1 to 5% by weight,
Calcium carbonate 3-10% by weight, and clay 50-92% by weight
Pesticide granules containing.
[2] The pesticide granule according to [1], wherein the nonionic surfactant is at least one nonionic surfactant selected from the group consisting of polyoxyethylene alkyl ether and polyoxyethylene alkyl aryl ether.
[3] The pesticide granule according to [1], wherein the nonionic surfactant is polyoxyethylene tristyrylphenyl ether.
[4] The pesticide granule according to any one of [1] to [3], wherein the clay is pyrophyllite.
[5] The pesticide granule according to any one of [1] to [4], wherein the pH at 20 ° C. when 10 g of the pesticide granule and 90 g of ion-exchanged water are mixed is 9.4 or more.

本発明の農薬粒剤は、オキサゾスルフィル、アルファ澱粉、ノニオン性界面活性剤、炭酸カルシウム及びクレーをそれぞれ特定量用いることにより、含有されるオキサゾスルフィルの溶出を抑制することができ、また、物理化学的性状の経時変化、特に硬度が経時的に低下することを抑制することができる。 The pesticide granules of the present invention can suppress the elution of oxazosulfyl contained in the pesticide granules by using specific amounts of oxazosulfyl, alpha starch, nonionic surfactant, calcium carbonate and clay, respectively. In addition, it is possible to suppress changes in physicochemical properties over time, particularly a decrease in hardness over time.

本発明の農薬粒剤(以下、本粒剤と記す)はオキサゾスルフィル(oxazosulfyl)を含有する。なお、オキサゾスルフィルは下記式(1)

Figure 2021066712
で示される化合物である。本粒剤におけるオキサゾスルフィルの含有量は、通常0.5〜5重量%、好ましくは1〜3重量%の範囲である。 The pesticide granules of the present invention (hereinafter referred to as the present granules) contain oxazosulfyl. Oxadiazole fil is given by the following formula (1).
Figure 2021066712
It is a compound indicated by. The content of oxazosulfyl in the granules is usually in the range of 0.5 to 5% by weight, preferably 1 to 3% by weight.

本粒剤はアルファ澱粉を含有する。本粒剤におけるアルファ澱粉の含有量は、4〜7重量%の範囲である。 This granule contains alpha starch. The content of alpha starch in the granules is in the range of 4-7% by weight.

本粒剤はノニオン性界面活性剤を含有する。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種のノニオン性界面活性剤が好ましく、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。
本粒剤におけるノニオン性界面活性剤の含有量は、通常0.1〜5重量%、好ましくは0.5〜2重量%の範囲である。
This granule contains a nonionic surfactant. Examples of such nonionic surfactants include polyoxyethylene alkyl ether, polyoxyethylene alkyl aryl ether, polyoxyethylene lanolin alcohol, polyoxyethylene alkylphenol formalin condensate, polyoxyethylene sorbitan fatty acid ester, and polyoxyethylene glyceryl monofatty 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 Examples thereof include polymers, polyoxyethylene fatty acid amides, alkylolamides, polyoxyethylene alkylamines, and at least one nonionic surfactant selected from the group consisting of polyoxyethylene alkyl ethers and polyoxyethylene alkyl aryl ethers. Preferably, polyoxyethylene tristyrylphenyl ether is even more preferred.
The content of the nonionic surfactant in the granules is usually in the range of 0.1 to 5% by weight, preferably 0.5 to 2% by weight.

本粒剤は炭酸カルシウムを含有する。本粒剤における炭酸カルシウムの含有量は、3〜10重量%の範囲である。 This granule contains calcium carbonate. The content of calcium carbonate in the granules is in the range of 3 to 10% by weight.

本粒剤はクレーを含有する。本明細書において、クレーはケイ酸塩鉱物を主成分とするものを意味し、一般に粘土と称される天然物であり、その粉砕物が農薬粒剤を調製する際に増量剤として使用されている。かかるクレーとしては、サポナイト、ヘクトライト、ソーコナイト、スチーブンサイト、ノントロナイト、モンモリロナイト、バイデライト等のスメクタイト鉱物、カオリナイト、ディッカナイト、ナクライト、ハロサイト等のカオリン鉱物、クリソタイル、リザータイト、アンチコライト、アメサイト等の蛇紋石、パイロフィライト、タルク、ロウ石、白雲母、フェンジャイト、セリサイト、イライト等の雲母、アタパルジャイト、セピオライト等の含水ケイ酸マグネシウム、ゼオライト、バーミキュライト等が挙げられ、ロウ石が好ましい。
本粒剤におけるクレーの含有量は、通常50〜92重量%、好ましくは70〜90重量%の範囲である。
This granule contains clay. In the present specification, clay means a substance containing a silicate mineral as a main component, and is a natural product generally called clay, and the pulverized product is used as a bulking agent in preparing pesticide granules. There is. Such clay includes smectite minerals such as saponite, hectrite, saconite, stephensite, nontronite, montmorillonite, and biderite, kaolin minerals such as kaolinite, diccanite, nacrite, and halosite, chrysotile, lizardite, anticholite, and candy. Serpentine stones such as sites, pyrophyllite, talc, wax stones, muscovite, fengyite, cericite, illite and other mica, hydrous magnesium silicate such as attapargit, sepiolite, zeolite, vermiculite, etc. preferable.
The content of clay in this granule is usually in the range of 50 to 92% by weight, preferably 70 to 90% by weight.

本粒剤は、オキサゾスルフィルに加えて、その他の農薬活性化合物を含有していてもよい。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種の病害抵抗性誘導活性化合物が好ましく、これらの中でもイソチアニルが好ましい。
本粒剤が他の農薬活性化合物を含有する場合、その含有量は、通常0.1〜50重量%、好ましくは0.5〜10重量%の範囲である。
The granules may contain other pesticide active compounds in addition to oxazosulfyl. Examples of such other pesticide active compounds include insecticidal active compounds, bactericidal 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 a disease resistance inducer. Disease resistance inducers are agents that control diseases by developing disease resistance of plants rather than acting directly on pathogens, and are mainly used for controlling blast. In the present invention, as the disease resistance-inducing active compound, at least one selected from the group consisting of thiadinil, isotianil, probenazole and acibenzolar-S-methyl. Disease resistance-inducing active compounds are preferable, and among these, isothienyl is preferable.
When the granules contain other pesticide active compounds, the content is usually in the range of 0.1 to 50% by weight, preferably 0.5 to 10% by weight.

また、本粒剤は、製剤用補助剤を含有していてもよい。かかる製剤用補助剤としては、例えば、浸透剤、湿潤剤、結合剤、防腐剤、酸化防止剤、固着剤、消泡剤、防錆剤、及び色素・顔料が挙げられる。 In addition, the granules may contain an auxiliary agent for preparation. Examples of such pharmaceutical auxiliary agents include penetrants, wetting agents, binders, preservatives, antioxidants, fixing agents, antifoaming agents, rust inhibitors, and pigments / pigments.

本粒剤は、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(以下、粒剤のpHと記す)が9.4以上であるか、9.4〜10.4の範囲であることが好ましい。粒剤のpHの値は、農薬粒剤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。農薬粒剤の粉砕は、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。粒剤のpHが9.4より低い場合には、粒剤のpHが9.4以上、または9.4〜10.4の範囲になるように、炭酸カルシウムの含有量を上述した範囲内で高くするか、アルカリ性のクレーを含有させるか、粒剤のpHをアルカリ性にするための添加剤(pH調整剤等)を適量含有させればよい。 This granule has a pH of 9.4 or more (hereinafter referred to as the pH of the granule) at 20 ° C. when 10 g of the pesticide granule and 90 g of ion-exchanged water are mixed, or 9.4 to 10.4. It is preferably in the range of. For the pH value of the granules, 10 g of pesticide granules was crushed using a crusher, the obtained pulverized product was placed in a container such as a screw tube having a capacity of 100 mL, and 90 g of ion-exchanged water whose temperature was adjusted to 20 ° C. was added. 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 pesticide granules can be crushed by using a crusher such as a coffee mill (Mini Blender MB-2, manufactured by Melita) for about 1 minute. When the pH of the granules is lower than 9.4, the calcium carbonate content should be within the above range so that the pH of the granules is 9.4 or higher, or 9.4 to 10.4. It may be increased, an alkaline clay may be contained, or an appropriate amount of an additive (pH adjuster or the like) for making the pH of the granules alkaline may be contained.

本粒剤は、オキサゾスルフィル、アルファ澱粉、ノニオン性界面活性剤、炭酸カルシウム及びクレー、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混練機としては、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。 The granules are prepared by adding water to a mixture containing oxazosulfyl, alpha starch, nonionic surfactants, calcium carbonate and clay, and optionally formulation aids and / or other pesticide active compounds. The kneaded product obtained by kneading is granulated, and then the obtained granulated product is dried and, if necessary, crushed, sieved, sized and the like can be produced. The amount of water added during kneading is usually 3 to 50 parts by weight with respect to 100 parts by weight of the mixture. Examples of the kneading machine used for kneading include a kneader, a nouter mixer, a ladyge 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押出造粒される。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。乾燥後、必要に応じて解砕、篩分、整粒等を行うことにより得られる最終製品としての本粒剤の粒長は、通常0.5〜6.0mm、好ましくは0.7〜4.0mmである。本明細書において粒長は、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 the kneaded product is extruded and granulated, it is usually extruded and granulated using a screen having a size 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. After drying, the grain length of this granule as a final product obtained by crushing, sieving, sizing, etc. as necessary is usually 0.5 to 6.0 mm, preferably 0.7 to 4 It is 0.0 mm. In the present specification, the grain length means the maximum length that a grain can take. Examples of the extrusion granulators include a screw type extrusion granulator, a roll type extrusion granulator, a disc pelleter type extrusion granulator, a pellet mill type extrusion granulator, a basket type extrusion granulator, and a blade type extrusion granulator. Machines, oscillating type extrusion granulators, gear type extrusion granulators, ring die type extrusion granulators and the like can be mentioned.

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 paddy rice seedling box processing. The paddy rice seedling box has a size of 30 cm × 60 cm (inner diameter: 28 cm × 58 cm) and is a seedling box for raising rice seedlings until rice planting (generally 20 to 40 days). Paddy rice seedling box treatment is a simple control method in which granules are sprayed on the seedling raising box in order to control pests 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, test examples and the like, but the present invention is not limited to these examples.

参考製造例1 粉状農薬組成物1の調製
70.0重量部のオキサゾスルフィル及び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5.9μm(MALVERN製MASTERSIZER2000により測定)のオキサゾスルフィ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 Powdered Agricultural Chemical Composition 1 70.0 parts by weight of oxazosulfyl and 30.0 parts by weight of pyrophyllite (Katsumitsuyama Clay S, manufactured by Katsukoyama Mining Co., Ltd.) are uniformly mixed and centrifuged. A powdery pesticide composition (hereinafter referred to as powdery pesticide composition 1) containing oxazosulfyl having a volume median diameter of 5.9 μm (measured by MASTERSIZER 2000 manufactured by MALVERN) is crushed by a crusher. Obtained.

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6.0μm(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 Agricultural Chemical Composition 2 70.0 parts by weight of isothianyl and 30.0 parts by weight of pyrophyllite (Katsumitsuyama Clay S, manufactured by Katsukoyama Mining Co., Ltd.) are uniformly mixed and put into a centrifugal crusher. The whole amount was pulverized to obtain a powdery pesticide composition (hereinafter referred to as powdery pesticide composition 2) containing isothianyl having a volume median diameter of 6.0 μm (measured by MASTERSIZER 2000 manufactured by MALVERN).

製造例1 本粒剤1の調製
粉状農薬組成物1 2.9重量部、アルファ澱粉(モールド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)5.0重量部及びロウ石(勝光山クレーS、勝光山鉱業所製)86.1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、本粒剤1を得た。
Production Example 1 Preparation of Granule 1 Powdered pesticide composition 1 2.9 parts by weight, alpha starch (mold No. 1A, manufactured by Nippon Corn Starch) 5.0 parts by weight, calcium carbonate (SS # 80, Nitto Flour Chemical Industry) (Manufactured by) 5.0 parts by weight and brazing stone (Katsumitsuyama Clay S, manufactured by Katsukoyama Mining Co., Ltd.) 86.1 parts by weight of a nonionic surfactant (polyoxyethylene tristyrylphenyl ether, Sopol T-20, (Manufactured by Toho Kagaku Kogyo) About 20 parts by weight of water containing 1.0 part by weight was added and kneaded. Approximately 1.0 kg of the obtained kneaded product was put into a basket-type extrusion granulator with a 1.2 mmφ screen (HU-G type field granulator, manufactured by Hata Iron Works Co., Ltd.) for 10 seconds. The grain machine was operated. After removing the granulated product obtained in 10 seconds, the operation of the granulating machine was restarted, and the granulated product obtained in 30 seconds was dried at 70 ° C. for 30 minutes to obtain this granule 1. ..

製造例2 本粒剤2の調製
粉状農薬組成物2 2.9重量部を加え、ロウ石(勝光山クレーS、勝光山鉱業所製)86.1重量部を83.2重量部とした以外は製造例1と同様の操作を行い、本粒剤2を得た。
Production Example 2 Preparation of Granule 2 22.9 parts by weight of powdered pesticide composition was added to make 86.1 parts by weight of pyrophyllite (Katsumitsuyama Clay S, manufactured by Katsukoyama Mining Co., Ltd.) 83.2 parts by weight. The same operation as in Production Example 1 was carried out except for this, to obtain this granule 2.

比較製造例1 比較農薬粒剤1の調製
粉状農薬組成物1 2.9重量部、合成含水酸化珪素微粉末(トクシールGU−N、トクヤマ製)1.0重量部、リグニンスルホン酸塩(Polyfon H、Ingevity製)2.0重量部、ベントナイト(ベントナイト穂高、ホージュン製)20.0重量部、及びカオリンクレー(Caolin B−10、INDUSTRIAS FINOR, S. L.社製)74.1重量部の混合物に水 約27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、比較農薬粒剤1を得た。
Comparative Production Example 1 Preparation of Comparative Agricultural Chemical Granules 1 2.9 parts by weight of powdered agricultural chemical composition, 1.0 part by weight of synthetic silicon hydroxide-containing fine powder (Tokuseal GU-N, manufactured by Tokuyama Corporation), lignin sulfonate (Polyphon) H, manufactured by Ingeverity) 2.0 parts by weight, bentonite (manufactured by Bentonite Hotaka, manufactured by Hojun) 20.0 parts by weight, and kaolin clay (manufactured by Caolin B-10, INDUSTRIAS FINOR, manufactured by SL) 74.1 parts by weight About 27 parts by weight of water was added to the mixture and kneaded. Approximately 1.0 kg of the obtained kneaded product was put into a basket-type extrusion granulator with a 1.2 mmφ screen (HU-G type field granulator, manufactured by Hata Iron Works Co., Ltd.) for 10 seconds. The grain machine was operated. After removing the granulated product obtained in 10 seconds, the operation of the granulating machine was restarted, and the granulated product obtained in 30 seconds was dried at 70 ° C. for 30 minutes to obtain Comparative Agricultural Chemical Granule 1 It was.

比較製造例2 比較農薬粒剤2の調製
粉状農薬組成物2 2.9重量部を加え、カオリンクレー(Caolin B−10、INDUSTRIAS FINOR, S. L.社製)74.1重量部を71.2重量部とした以外は比較製造例1と同様の操作を行い、比較農薬粒剤2を得た。
Comparative Production Example 2 Preparation of Comparative Agricultural Chemical Granules 2 Add 2.9 parts by weight of powdered pesticide composition 2 to 71 parts by weight of 74.1 parts by weight of Kaolin B-10, INDUSTRIAS FINOR, SL. A comparative pesticide granule 2 was obtained by performing the same operation as in Comparative Production Example 1 except that the weight was 2 parts by weight.

試験例1
本粒剤1及び2、並びに比較農薬粒剤1及び2のそれぞれについて以下の操作を行った。農薬粒剤100g(Ag)を秤量し、陶器製のボール(重量35±3.0g/個、直径30±2.0mm)が3個入った陶器製円筒ボールミルポット(直径125mm、高さ125mm)に入れて蓋を閉め、ローラーにボールミルポットを乗せて75回転/分の速度で15分間回転させた。その後農薬粒剤をボールミルポットから取り出し、目開き500μmの篩で篩分け、500μmの篩上に残った農薬粒剤の重量(Bg)を測定し、下記式により崩壊率を求めた。
崩壊率[%]=(A−B)/A×100
その結果を表1に示した。いずれの農薬粒剤も崩壊率は低く、硬度は良好であった。
Test Example 1
The following operations were performed for each of the present granules 1 and 2 and the comparative pesticide granules 1 and 2, respectively. Weighing 100 g (Ag) of pesticide granules, a pottery cylindrical ball mill pot (diameter 125 mm, height 125 mm) containing three pottery balls (weight 35 ± 3.0 g / piece, diameter 30 ± 2.0 mm) The ball mill pot was placed on a roller and rotated at a speed of 75 rpm for 15 minutes. Then, the pesticide granules were taken out from the ball mill pot, sieved with a sieve having a mesh size of 500 μm, the weight (Bg) of the pesticide granules remaining on the sieve having a mesh size of 500 μm was measured, and the disintegration rate was calculated by the following formula.
Collapse rate [%] = (AB) / A × 100
The results are shown in Table 1. All the pesticide granules had a low disintegration rate and good hardness.

Figure 2021066712
Figure 2021066712

試験例2
本粒剤1及び2、並びに比較農薬粒剤1及び2をそれぞれアルミ内装クラフト袋に入れ、40℃、相対湿度90%で2週間保存した後、試験例1と同様の手順でそれぞれの農薬粒剤の崩壊率を測定した。その結果を表2に示した。本粒剤1及び2の崩壊率はほとんど変化せず、比較農薬粒剤1及び2の崩壊率は上昇した。
Test Example 2
The granules 1 and 2 and the comparative pesticide granules 1 and 2 are placed in an aluminum interior kraft bag, respectively, and stored at 40 ° C. and a relative humidity of 90% for 2 weeks. The disintegration rate of the agent was measured. The results are shown in Table 2. The disintegration rates of the present granules 1 and 2 hardly changed, and the disintegration rates of the comparative pesticide granules 1 and 2 increased.

Figure 2021066712
Figure 2021066712

試験例3
蓋付きガラス製容器(φ11cm×高さ15cm)に900mLの3度硬水を入れ、水温が25±1.0℃になるように調整した。本粒剤1、比較農薬粒剤1及び2のいずれかを所定量該容器中に入れ、該容器内の液温が25±1.0℃になるように温度管理しながら該容器を放置した。農薬粒剤を入れてから3日後に、容器の中央部から溶液約2mLをポリスポイドを用いてサンプリングした。サンプリングされた溶液を所定の条件のもとで高速液体クロマトグラフィーを用いて分析を行い、サンプリングされた溶液中のオキサゾスルフィル濃度を定量して以下の式を用いてオキサゾスルフィルの溶出率を算出した。
オキサゾスルフィルの溶出率(%)=(サンプリングした溶液中のオキサゾスルフィル濃度[ppm]/水中溶出試験に供試した農薬粒剤の最大溶出濃度[ppm])×100
その結果を表3に示す。ただし、供試された農薬粒剤の量は、農薬粒剤中に含まれるオキサゾスルフィルの全てが水に溶解した時の濃度(最大溶出濃度[ppm])が0.601ppmになる量とした。
Test Example 3
900 mL of 3 degree hard water was placed in a glass container with a lid (φ11 cm × height 15 cm), and the water temperature was adjusted to 25 ± 1.0 ° C. A predetermined amount of either the main granule 1 or the comparative pesticide granules 1 and 2 was placed in the container, and the container was left to stand while controlling the temperature so that the liquid temperature in the container was 25 ± 1.0 ° C. .. Three days after the pesticide granules were added, about 2 mL of the solution was sampled from the center of the container using a polyspoid. The sampled solution is analyzed by high performance liquid chromatography under predetermined conditions, the concentration of oxazosulfyl in the sampled solution is quantified, and the elution of oxazosulfyl is performed using the following formula. The rate was calculated.
Elution rate of oxazosulfyl (%) = (Oxazosulfyl concentration in sampled solution [ppm] / Maximum elution concentration of pesticide granules tested in water dissolution test [ppm]) x 100
The results are shown in Table 3. However, the amount of pesticide granules tested was such that the concentration (maximum elution concentration [ppm]) when all of the oxazosulfyl contained in the pesticide granules was dissolved in water was 0.601 ppm. did.

Figure 2021066712
Figure 2021066712

Claims (5)

オキサゾスルフィル0.5〜5重量%、
アルファ澱粉4〜7重量%、
ノニオン性界面活性剤0.1〜5重量%、
炭酸カルシウム3〜10重量%、及び
クレー50〜92重量%
を含有する農薬粒剤。
Oxadiazolefil 0.5-5% by weight,
Alpha starch 4-7% by weight,
Nonionic surfactant 0.1 to 5% by weight,
Calcium carbonate 3-10% by weight, and clay 50-92% by weight
Pesticide granules containing.
前記ノニオン性界面活性剤が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種のノニオン性界面活性剤である請求項1に記載の農薬粒剤。 The pesticide granule according to claim 1, wherein the nonionic surfactant is at least one nonionic surfactant selected from the group consisting of polyoxyethylene alkyl ether and polyoxyethylene alkyl aryl ether. 前記ノニオン性界面活性剤がポリオキシエチレントリスチリルフェニルエーテルである請求項1に記載の農薬粒剤。 The pesticide granule according to claim 1, wherein the nonionic surfactant is polyoxyethylene tristyrylphenyl ether. 前記クレーがロウ石である請求項1〜3のいずれかに記載の農薬粒剤。 The pesticide granule according to any one of claims 1 to 3, wherein the clay is pyrophyllite. 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9.4以上である請求項1〜4のいずれかに記載の農薬粒剤。 The pesticide granule according to any one of claims 1 to 4, wherein the pH at 20 ° C. when 10 g of the pesticide granule and 90 g of ion-exchanged water are mixed is 9.4 or more.
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Citations (5)

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Publication number Priority date Publication date Assignee Title
WO2004089091A1 (en) * 2003-04-09 2004-10-21 Meiji Seika Kaisha, Ltd. Sustained release agrichemical granule
JP2009019034A (en) * 2007-06-14 2009-01-29 Sumitomo Chemical Co Ltd Agrochemical granule composition
JP2016166149A (en) * 2015-03-10 2016-09-15 住友化学株式会社 Agrochemical granule
WO2017104592A1 (en) * 2015-12-16 2017-06-22 住友化学株式会社 2-(3-e thanesulfonyl pyridine-2-yl)-5-(trifluoromethanesulfonyl) benzoxazole crystal
JP2019156836A (en) * 2018-03-09 2019-09-19 三井化学アグロ株式会社 Agricultural and horticultural granular composition and method for producing said composition

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2004089091A1 (en) * 2003-04-09 2004-10-21 Meiji Seika Kaisha, Ltd. Sustained release agrichemical granule
JP2009019034A (en) * 2007-06-14 2009-01-29 Sumitomo Chemical Co Ltd Agrochemical granule composition
JP2016166149A (en) * 2015-03-10 2016-09-15 住友化学株式会社 Agrochemical granule
WO2017104592A1 (en) * 2015-12-16 2017-06-22 住友化学株式会社 2-(3-e thanesulfonyl pyridine-2-yl)-5-(trifluoromethanesulfonyl) benzoxazole crystal
JP2019156836A (en) * 2018-03-09 2019-09-19 三井化学アグロ株式会社 Agricultural and horticultural granular composition and method for producing said composition

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