JP2006131602A - Fine granule agent containing acetolactate synthesis inhibitor - Google Patents
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本発明は、生活環境に生育する不必要で有害な雑草類を効率的に防除する技術に関する。 The present invention relates to a technique for efficiently controlling unnecessary and harmful weeds that grow in a living environment.
農耕地、非農耕地を問わず雑草類の繁茂は、農業生産性の低下や生活環境の悪化をもたらし、その対策として除草剤や生育抑制剤が広く利用されている。この中でアセトラクテート合成阻害剤（以下ＡＬＳＩ剤と称する）は、高い選択性を有し特定の草種のみに極微量で非常に高い除草活性を有することから、水田、畑の他、シバ等緑化作物や鉄道、宅地、運動場、道路、駐車場等の管理地に広く使用されている。ＡＬＳＩ剤の性質として、主に茎葉から吸収されて効果を発現する、水溶液中で不安定である、有機溶媒溶解性が悪い等が挙げられる。そのため、水を媒体として使用できる水田において粒径の大きい粒剤が使われている以外は、茎葉に散布するための水和剤が殆どであり、極一部に乳剤が使用されているだけである。 Regardless of farmland or non-agricultural land, weeds overgrow, leading to a decline in agricultural productivity and a worsening living environment, and herbicides and growth inhibitors are widely used as countermeasures. Among them, an acetolactate synthesis inhibitor (hereinafter referred to as an ALSI agent) has high selectivity and has extremely high herbicidal activity only in a specific grass species. Widely used in management areas such as greening crops, railways, residential land, playgrounds, roads, parking lots, etc. The properties of the ALSI agent include those that are mainly absorbed from the foliage and exhibit an effect, unstable in an aqueous solution, and poor solubility in organic solvents. For this reason, except for the use of granules with a large particle size in paddy fields where water can be used as a medium, most of the wettable powder is sprayed on the foliage, and only an emulsion is used in a very small part. is there.
農薬の剤型のひとつに、粒剤よりも粒径の小さい粒径０．１〜０．３ｍｍの微粒剤があり、水で希釈して用いる乳剤や水和剤に比べて使用が簡便で、かつ飛散を防止する目的から使用されている。例えば茎葉及び根のいずれからも吸収されて効果を発現する脂肪酸系除草剤、植物ホルモン系除草剤で用いられている他、光合成阻害系除草剤であるジウロン（ＩＳＯ名ｄｉｕｒｏｎ）が３％微粒剤（商品名 ダイロン微粒剤）として、また脂肪酸系除草剤と植物ホルモン系除草剤の混合微粒剤（商品名 ミカロック微粒剤）が販売されている。さらに茎葉からの吸収によって効果を発現する薬剤を微粒剤として使用することも公知の事実である。例えば、グルホシネート（ＩＳＯ名ｇｌｕｆｏｓｉｎａｔｅ−ａｍｍｏｎｉｕｍ）をアタパルジャイト等に添加し、微粒剤として用いる方法が示されている（特許文献１参照）。また、グルホシネートもしくはグリホサート（ＩＳＯ名ｇｌｙｐｈｏｓａｔｅ）と土壌処理活性を有する除草剤を混合して使用することによって気象変動に強い微粒剤を調製する方法が示されている（特許文献２、特許文献３参照）。
環境に投下する薬剤量を少なくし、雑草を速やか且つ有効に、また簡便に防除することは大きな課題である。一般的にＡＬＳＩ剤は、非常に低薬量でアミノ酸の生合成系を阻害することにより植物を枯死に至らせる。従って、一般的に効果の発現と完成は遅い。また、殺草スペクトラムが狭い、土壌処理効果が低い、化合物として水中での安定性が低い、有機溶媒溶解性が低いといった物理化学的な性質から、水田で粒剤が用いられる外は、水和剤と極一部乳剤があるだけでその他の剤型がない等の欠点が認知されている。 It is a big problem to reduce the amount of chemicals dropped into the environment and to control weeds quickly, effectively and simply. In general, ALSI agents cause plants to die by inhibiting the biosynthesis system of amino acids at a very low dose. Therefore, the onset and completion of effects are generally slow. In addition, because of its physicochemical properties such as a narrow herbicidal spectrum, low soil treatment effect, low stability in water as a compound, and low solubility in organic solvents, it is hydrated except that granules are used in paddy fields. Disadvantages such as the absence of other dosage forms, with only agents and very partial emulsions, are recognized.
現在、商品化されている農薬の剤型にはいくつかの欠点がある。例えば、粒剤は粒径が大きいことから茎葉部には付着せず、生育期の雑草に対しては根部から吸収されてのみ効果を示すため、処理後の降雨、土壌水分といった環境要因によって除草効果が左右され、多大な薬剤量と効果完成までの日数を必要とする。また、水に懸濁して用いる剤型は薬液を調合する手間と、専用の散布器具を必要とし、加えて薬剤の飛散が大きい。更に、水利の悪い場所では使用することができない。 There are several drawbacks to the currently commercialized agrochemical dosage forms. For example, the granule does not adhere to the foliage due to its large particle size, and is effective only when it is absorbed from the root to weeds in the growing season, so weeding by environmental factors such as rainfall after treatment and soil moisture The effect depends on the amount of drug and the number of days until the effect is completed. In addition, the dosage form used by suspending in water requires troublesome preparation of a chemical solution and a special spraying device, and in addition, the scattering of the drug is large. Furthermore, it cannot be used in places with poor water use.
その他、選択的な除草剤を利用して、双子葉植物に比べ根系の発達が優れる単子葉植物主体の植相に転換させることによる土壌流亡の防止や雑草の草丈を抑制することも検討されている。 In addition, the use of selective herbicides to prevent soil runoff and to suppress weed plant height by switching to a monocotyledonous vegetation that has superior root system development compared to dicotyledonous plants is being studied. Yes.
本発明者らは従来使用されることのなかったＡＬＳＩ剤の微粒剤化について検討を重ね、０．１〜０．３ｍｍの微粒な鉱物に結合剤を用いて付着、もしくは給油能の高い鉱物に吸収させることによって茎葉部からの吸収を確保しながら、薬液を調合せず、使用が簡便かつ安全で飛散のない薬剤を完成させた。更にその他の茎葉部及び根部から吸収されて効果を現す薬剤を混合させることによって、殺草スペクトラムを拡大させ、効果発現速度を高め、残効性の向上を図りうることを見出した。 The inventors of the present invention have repeatedly studied on the atomization of an ALSI agent that has not been used in the past, and adhered to a fine mineral of 0.1 to 0.3 mm using a binder, or a mineral with a high oil supply ability. While ensuring absorption from the foliage by absorption, a chemical was not prepared, and a simple, safe and non-scattering drug was completed. Furthermore, the present inventors have found that by mixing a drug that is absorbed from other foliage and roots and exhibits an effect, the herbicidal spectrum can be expanded, the effect expression rate can be increased, and the residual effect can be improved.
本発明に関わるアセトラクテート合成阻害剤（ＡＬＳＩ剤）としては、イオドスルフロンメチルナトリウム塩（ＩＳＯ名ｉｏｄｏｓｕｌｆｕｒｏｎ−ｍｅｔｈｙｌ−ｓｏｄｉｕｍ）、シクロスルファムロン（ＩＳＯ名ｃｙｃｌｏｓｕｌｆａｍｕｒｏｎ）、トリフロキシスルフロンナトリウム塩（ＩＳＯ名ｔｒｉｆｌｏｘｙｓｕｌｆｕｒｏｎ−ｓｏｄｉｕｍ）、メトスルフロンメチル（ＩＳＯ名ｍｅｔｓｕｌｆｕｒｏｎ−ｍｅｔｈｙｌ）が挙げられる。薬剤の含有量は、イオドスルフロンメチルナトリウム塩、トリフロキシスルフロンナトリウム塩、メトスルフロンメチルの場合は０．００３〜０．０３重量％が適切であり、シクロスルファムロンの場合は０．０３〜０．３重量％が適切である。 Examples of the acetolactate synthesis inhibitor (ALIS agent) according to the present invention include iodosulfuron methyl sodium salt (ISO name iodosulfuron-methyl-sodium), cyclosulfamuron (ISO name cyclosulfamuron), trifloxysulfuron sodium salt (ISO Name trifloxysulfuron-sodium) and metsulfuron methyl (ISO name metsulfuron-methyl). The appropriate drug content is 0.003-0.03% by weight for iodosulfuron methyl sodium salt, trifloxysulfuron sodium salt, and metsulfuron methyl, and 0.03% for cyclosulfamuron. ~ 0.3% by weight is suitable.
本発明に係る微粒剤を調製するためには、結合剤とＡＬＳＩ剤の粉末、もしくは溶液、もしくは懸濁液を攪拌している鉱物担体中に投入する、もしくは噴霧させることによって容易に製造できる。 In order to prepare the fine granule according to the present invention, it can be easily produced by putting or spraying a powder or solution or suspension of a binder and an ALSI agent into a stirring mineral carrier.
使用する鉱物担体には、アタパルジャイト、珪石、焼成珪藻土、ゼオライト、セピオライト、炭酸カルシウム、モンモリロナイト等を用いうる。粒剤の粒径は微細なほど葉面への付着効率を高めることができるが、風が強い場合、微細な粒子は飛散して周辺の植物に薬害を起こす場合がある。一方、粗い場合は葉面への付着が低下して十分な効果を得ることが難しい。従って、我が国で微粒剤に分類される０．１〜０．３ｍｍの粒径が好ましい。 As the mineral carrier to be used, attapulgite, quartzite, calcined diatomaceous earth, zeolite, sepiolite, calcium carbonate, montmorillonite and the like can be used. The finer the particle size of the granule, the higher the adhesion efficiency to the leaf surface. However, when the wind is strong, the fine particles may scatter and cause phytotoxicity to surrounding plants. On the other hand, when it is rough, adhesion to the leaf surface is lowered and it is difficult to obtain a sufficient effect. Accordingly, a particle size of 0.1 to 0.3 mm, which is classified as a fine granule in Japan, is preferable.
有効成分を鉱物担体に付着させるためには結合剤を用いることが重要である。結合剤としては、エチレングリコール、高級アルコール、高級脂肪酸エステル、鉱物油、ジメチルスルホキシド、植物油、プロピレングリコール、ポリエチレングリコール、ポリプロピレングリコール、プロピレングリコールモノメチルエーテル、１−メチルピロリドン等の高沸点高粘度の溶剤類、カルボキシメチルセルロース、デキストラン、ポリビニールアルコール、ポリビニールピロリドン等の糊料、及び各種の界面活性剤が使用できる。特に界面活性剤は、高粘度による光合成阻害系除草剤の担体鉱物への付着を助けるのみならず、散布された有効成分の植物体上での広がりや植物体内への速やかな浸透を促し、効果を安定させる機能を有している。 In order to attach the active ingredient to the mineral carrier, it is important to use a binder. Binders include high-boiling and high-viscosity solvents such as ethylene glycol, higher alcohol, higher fatty acid ester, mineral oil, dimethyl sulfoxide, vegetable oil, propylene glycol, polyethylene glycol, polypropylene glycol, propylene glycol monomethyl ether, and 1-methylpyrrolidone. , Pastes such as carboxymethyl cellulose, dextran, polyvinyl alcohol, polyvinyl pyrrolidone, and various surfactants can be used. In particular, surfactants not only help adhere the photosynthesis-inhibiting herbicide to the carrier mineral due to high viscosity, but also promote the spread of the sprayed active ingredients on the plant body and prompt penetration into the plant body. It has the function to stabilize.
多くの界面活性剤があるが、例えば、陰イオン界面活性剤としては、アルキルベンゼンスルホン酸塩、アルキルナフタレンスルホン酸塩、ジアルキルスルホサクシネート、ジアルキルリン酸塩、脂肪酸塩、ポリアクリル酸塩、ポリカルボン酸塩、モノアルキルリン酸塩、リグニンスルホン酸塩等があげられる。陽イオン界面活性剤としては、アルキルジメチルベンザルコニウムクロライド、アルキルトリメチルアンモニウムクロライド、アルキルペンタメチルプロピレンジアミンジクロライド、アルキル−Ｎ−メチルピリジニウムブロマイド、ベンゼトニウムクロライド、ポリオキシエチレンアルキルアミン、メチルポリオキシエチレンアルキルアンモニウムクロライド等があげられる。また、非イオン界面活性剤としては、ソルビタン脂肪酸エステル、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フェニールエーテル、ポリオキシエチレンアルキルフェニールエーテルホルマリン縮合物、ポリオキシアルキレンベンジルフェニルエーテル、ポリオキシエチレン脂肪酸エステル、ポリオキシエチレンソルビタン脂肪酸エステル等があげられる。両性イオン界面活性剤としては、アルキルベタイン等があげられる。界面活性剤を含む水溶性高沸点有機物質は単独もしくは混合して用いられ、その使用量は、製剤品全重量に対して０．１〜５．０重量％である。 There are many surfactants. For example, anionic surfactants include alkylbenzene sulfonate, alkylnaphthalene sulfonate, dialkyl sulfosuccinate, dialkyl phosphate, fatty acid salt, polyacrylate, polycarboxylate. Acid salts, monoalkyl phosphates, lignin sulfonates and the like. Cationic surfactants include alkyldimethylbenzalkonium chloride, alkyltrimethylammonium chloride, alkylpentamethylpropylenediamine dichloride, alkyl-N-methylpyridinium bromide, benzethonium chloride, polyoxyethylene alkylamine, methyl polyoxyethylene alkylammonium And chloride. Nonionic surfactants include sorbitan fatty acid ester, polyoxyethylene alkyl ether, polyoxyethylene alkyl phenyl ether, polyoxyethylene alkyl phenyl ether formalin condensate, polyoxyalkylene benzyl phenyl ether, polyoxyethylene fatty acid ester, And polyoxyethylene sorbitan fatty acid ester. Examples of zwitterionic surfactants include alkylbetaines. The water-soluble high-boiling organic substance containing a surfactant is used alone or as a mixture, and the amount used is 0.1 to 5.0% by weight with respect to the total weight of the preparation.
高粘度の結合剤を用いることによって粒剤が固結しやすくなる場合は、多孔質珪酸等の微粉を０．５〜５．０重量％添加することによって防止することができる。 If the granule is easily consolidated by using a high-viscosity binder, it can be prevented by adding 0.5 to 5.0% by weight of fine powder such as porous silicic acid.
また、気象条件によって葉面への付着が制限され除草効果が低下する場合や、後次に発生する雑草を防除するため土壌処理効果を有する除草剤を混合して製剤することも可能である。例えば、グリホサート（ＩＳＯ名ｇｌｙｐｈｏｓａｔｅ）もしくはグルホシネート（ＩＳＯ名ｇｌｕｆｏｓｉｎａｔｅ−ａｍｍｏｎｉｕｍ）等のアミノ酸系除草剤、イソウロン（ＩＳＯ名ｉｓｏｕｒｏｎ）、カルブチレート（ＩＳＯ名ｋａｒｂｕｔｉｌａｔｅ）、シアナジン（ＩＳＯ名ｃｙａｎａｚｉｎｅ）、ジウロン（ＩＳＯ名ｄｉｕｒｏｎ）、ターバシル（ＩＳＯ名ｔｅｒｂａｃｉｌ）、テブチウロン（ＩＳＯ名ｔｅｂｕｔｈｉｕｒｏｎ）、ブロマシル（ＩＳＯ名ｂｒｏｍａｃｉｌ）、メトリブジン（ＩＳＯ名ｍｅｔｒｉｂｕｚｉｎ）等の光合成阻害剤。アラクロール（ＩＳＯ名ａｌａｃｈｌｏｒ）、ジメテナミド（ＩＳＯ名ｄｉｍｅｔｈｅｎａｍｉｄ）、テニルクロール（ＩＳＯ名ｔｈｅｎｙｌｃｈｌｏｒ）、ブタクロール（ＩＳＯ名ｂｕｔａｃｈｌｏｒ）、プレチラクロール（ＩＳＯ名ｐｒｅｔｉｌａｃｈｌｏｒ）、メトラクロール（ＩＳＯ名ｍｅｔｏｌａｃｈｌｏｒ）等のハロゲノアセトアミド系除草剤。ペンディメタリン（ＩＳＯ名ｐｅｎｄｉｍｅｔｈａｌｉｎ）トリフルラリン（ＩＳＯ名ｔｒｉｆｌｕｒａｌｉｎ）、プロジアミン（ＩＳＯ名ｐｒｏｄｉａｍｉｎｅ）、ベンフラリン（ＩＳＯ名ｂｅｎｆｌｕｒａｌｉｎ）等のジニトロアニリン系除草剤、オキサジアルギル（ＩＳＯ名ｏｘａｄｉａｒｇｙｌ）、ピラフルフェンエチル（ＩＳＯ名ｐｙｒａｆｌｕｆｅｎ−ｅｔｈｙｌ）等のプロトポルフィリノーゲンオキシダーゼ阻害剤の他、シンメチリン（ＩＳＯ名ｃｉｎｍｅｔｈｙｌｉｎ）、アシュラム（ＩＳＯ名ａｓｕｌａｍ）、フルプロパネートナトリウム塩（ＩＳＯ名ｆｌｕｐｒｏｐａｎａｔｅ−ｓｏｄｉｕｍ）等が挙げられる。
これら機能の異なる除草剤を混合することによって、一般に使用される薬量以下での使用を可能にする。これらの薬剤含有量は薬剤によって異なるが、０．００５〜３．０重量％である。In addition, it is possible to prepare a mixture of herbicides having a soil treatment effect in order to control weeds that occur afterwards when adhesion to the leaf surface is limited due to weather conditions or to control weeds that are generated next. For example, amino acid herbicides such as glyphosate (ISO name glyphosate) or glufosinate (ISO name glufosinate-ammonium), isouron (ISO name isouron), carbbutyrate (ISO name karbutilate), cyanazine (ISO name cyanazine), diuron (ISO name) ), Terbacil (ISO name terbacil), tebuthiuron (ISO name tebuthiuron), bromacil (ISO name bromacil), photosynthesis inhibitors such as metribuzin (ISO name metricibuzin). Alachlor (ISO name alachlor), dimethenamide (ISO name dimethylenamide), tenyl chlor (ISO name tenchllor), butachlor (ISO name butachlor), pretilachlor (ISO name pretilachlor), metolachlor (ISO name metohalochol amide) . Dinitroaniline herbicides such as pendimethalin (ISO name pendimethalin) trifluralin (ISO name trifluralin), prodiamine (ISO name prodamine), benfuralin (ISO name befluralin), oxadialgyl (ISO name oxadiargyl), SO4 In addition to protoporphyrinogen oxidase inhibitors such as name pyraflufen-ethyl), synmethylin (ISO name cinmethyl), ashram (ISO name asuram), flupropanate sodium salt (ISO name flupropanate-sodium) and the like.
By mixing herbicides having different functions, it is possible to use them at a dose below the commonly used dose. The content of these drugs varies depending on the drug, but is 0.005 to 3.0% by weight.
水和剤として使用していたＡＬＳＩ剤を微粒剤にすることによって、従来の剤型よりも速効性を向上させつつ効果を安定させ、同時に飛散なく簡便な使用を可能にする。また、ＡＬＳＩ剤に茎葉処理剤もしくは土壌処理剤を混合することにより、速効性及び後次発生抑制等の付与をも可能にする。更に、薬剤の組み合わせによっては投下薬量を減少することにより、雑草の草丈を抑制することも可能にする。 By making the ALSI agent used as a wettable powder into a fine granule, the effect is stabilized while improving the quick-acting property as compared with the conventional dosage form, and at the same time, a simple use without scattering is enabled. In addition, by adding a foliar treatment agent or a soil treatment agent to the ALSI agent, it is possible to impart quick action and suppression of subsequent generation. Furthermore, depending on the combination of the drugs, it is also possible to reduce the weed plant height by reducing the amount of dropped drug.
発明の実施の形態を製剤例に基づき説明する。
（製剤例１）メトスルフロンメチル０．００８％微粒剤の調製
メカノミル（造粒コーティング機、岡田精工株式会社製品）の攪拌槽に微粒の珪石（珪砂Ｖ７号、三河珪石株式会社商品）４８５．５ｇとメトスルフロンメチル６０％水和剤（サーベルＤＦ水和剤、デュポン株式会社商品）を２％水溶液として２．０ｇを仕込み、３５０ｒｐｍで回転させながら１分間混合した。次にネオスコア２３３９（ポリオキシアルキレンモノアルキルエーテル、東邦化学工業株式会社商品）７．５ｇを４００ｒｐｍで回転させながらゆっくり添加した。続いて多孔質珪酸（カープレックスＸＲ、塩野義製薬株式会社商品）５．０ｇを加えて１分間攪拌後取り出し、風乾して０．１〜０．３ｍｍの粒子を篩い分けして求める微粒剤４９２ｇを得た。Embodiments of the invention will be described based on formulation examples.
Formulation Example 1 Preparation of Methosulfuron Methyl 0.008% Fine Granules In a stirring tank of Mechano Mill (granulation coating machine, Okada Seiko Co., Ltd.), 485.5 g of fine silica stone (Silica Sand V7, Mikawa Silica Co., Ltd.) And metsulfuron methyl 60% wettable powder (Saber DF wettable powder, DuPont Co., Ltd.) as a 2% aqueous solution was charged with 2.0 g and mixed for 1 minute while rotating at 350 rpm. Next, 7.5 g of Neoscore 2339 (polyoxyalkylene monoalkyl ether, product of Toho Chemical Co., Ltd.) was slowly added while rotating at 400 rpm. Subsequently, 492 g of a fine particle agent obtained by adding 5.0 g of porous silicic acid (Carplex XR, Shionogi & Co., Ltd. product), taking out after stirring for 1 minute, air drying and sieving 0.1 to 0.3 mm particles. Got.
（製剤例２）シクロスルファムロン０．１％微粒剤の調製
メカノミルの攪拌槽に微粒の珪石４８２．５ｇとシクロスルファムロン１０％水和剤（ダブルアップ水和剤、ＢＡＳＦアグロ株式会社商品）５．０ｇを仕込み、３５０ｒｐｍで回転させながら１分間混合した。次に６５％ジオクチルスルホサクシネート（ジェラポンＤＯＳ／ＰＣ−６５、ローディア日華株式会社商品）７．５ｇを４００ｒｐｍで回転させながらゆっくり添加した。続いて多孔質珪酸５．０ｇを加えて１分間攪拌後取り出し、風乾して０．１〜０．３ｍｍの粒子を篩い分けして求める微粒剤４９３ｇを得た。(Formulation example 2) Preparation of cyclosulfamuron 0.1% fine powder 482.5g of fine silica stone and 10% cyclosulfamuron wettable powder (double up wettable powder, BASF Agro Co., Ltd. ) 5.0 g was charged and mixed for 1 minute while rotating at 350 rpm. Next, 7.5 g of 65% dioctylsulfosuccinate (Jerapon DOS / PC-65, Rhodia Nikka Co., Ltd.) was slowly added while rotating at 400 rpm. Subsequently, 5.0 g of porous silicic acid was added, taken out after stirring for 1 minute, air-dried, and 493 g of a fine granule obtained by sieving 0.1 to 0.3 mm particles was obtained.
（製剤例３）イオドスルフロンメチルナトリウム塩０．０１％微粒剤の調製
メカノミルの攪拌槽に微粒の珪石４８５．０ｇとイオドスルフロンメチルナトリウム塩５％顆粒水和剤（Ｈｕｓｓａｒ顆粒水和剤、バイエルクロップサイエンス株式会社商品）を２％懸濁液として２．５ｇを仕込み、３５０ｒｐｍで回転させながら１分間混合した。次に６５％ジオクチルスルホサクシネート７．５ｇを４００ｒｐｍで回転させながらゆっくり添加した。続いて多孔質珪酸５．０ｇを加えて１分間攪拌後取り出し、風乾して０．１〜０．３ｍｍの粒子を篩い分けして求める微粒剤４９２ｇを得た。(Formulation example 3) Preparation of iodosulfuron methyl sodium salt 0.01% fine granule 485.0 g of fine silica stone and 5% iodosulfuron methyl sodium salt granule wettable powder (Hussar granule wettable powder, Bayer CropScience Co., Ltd.) as a 2% suspension was charged with 2.5 g and mixed for 1 minute while rotating at 350 rpm. Next, 7.5 g of 65% dioctylsulfosuccinate was slowly added while rotating at 400 rpm. Subsequently, 5.0 g of porous silicic acid was added, taken out after stirring for 1 minute, taken out and air-dried to obtain 492 g of a fine granule obtained by sieving 0.1 to 0.3 mm particles.
（製剤例４）トリフロキシスルフロンナトリウム塩０．０１％微粒剤の調製
メカノミルの攪拌槽に微粒の珪石４８４．９ｇとトリフロキシスルフロンナトリウム塩７２％水和剤（モニュメント顆粒水和剤、シンジェンタ株式会社商品）を２％水溶液として２．６ｇを仕込み、３５０ｒｐｍで回転させながら１分間混合した。次に６５％ジオクチルスルホサクシネート７．５ｇを４００ｒｐｍで回転させながらゆっくり添加した。続いて多孔質珪酸５．０ｇを加えて１分間攪拌後取り出し、風乾して０．１〜０．３ｍｍの粒子を篩い分けして求める微粒剤４９２ｇを得た。(Formulation Example 4) Preparation of Trifloxysulfuron Sodium Salt 0.01% Fine Granules 484.9 g of fine silica stone and 72% trifloxysulfuron sodium salt wettable powder (monument granule wettable powder, Syngenta) 2.6 g as a 2% aqueous solution was added and mixed for 1 minute while rotating at 350 rpm. Next, 7.5 g of 65% dioctylsulfosuccinate was slowly added while rotating at 400 rpm. Subsequently, 5.0 g of porous silicic acid was added, taken out after stirring for 1 minute, taken out and air-dried to obtain 492 g of a fine granule obtained by sieving 0.1 to 0.3 mm particles.
（製剤例５）チフェンスルフロンメチル０．０４％微粒剤の調製
メカノミルの攪拌槽に微粒の珪石４８８．０ｇとチフェンスルフロンメチル（ＩＳＯ名ｔｈｉｆｅｎｓｕｌｆｕｒｏｎ−ｍｅｔｈｙｌ）７５％水和剤（ハーモニー７５ＤＦ水和剤、デュポン株式会社商品）を１０％懸濁液として２．０ｇを仕込み、３５０ｒｐｍで回転させながら１分間混合した。次に５．０ｇのネオスコア２３３９を４００ｒｐｍで回転させながらゆっくり添加した。続いて多孔質珪酸５．０ｇを加えて１分間攪拌後取り出し、風乾して０．１〜０．３ｍｍの粒子を篩い分けして求める微粒剤４９６ｇを得た。(Formulation Example 5) Preparation of Thifensulfuron Methyl 0.04% Fine Granules 488.0 g of fine silicalite and ISOF thifensulfuron methyl (ISO name thifensulfuron-methyl) 75% wettable powder (Harmony 75DF Hydration) 2.0 g as a 10% suspension was added and mixed for 1 minute while rotating at 350 rpm. Next, 5.0 g of Neoscore 2339 was added slowly while rotating at 400 rpm. Subsequently, 5.0 g of porous silicic acid was added, taken out after stirring for 1 minute, taken out and air-dried to obtain 496 g of a fine granule obtained by sieving 0.1 to 0.3 mm particles.
（製剤例６）トリフロキシスルフロンナトリウム塩０．００８％メトスルフロンメチル０．００８％微粒剤の調製
メカノミルの攪拌槽に微粒の珪石４８３．５ｇとトリフロキシスルフロンナトリウム塩２％溶液２．０ｇ及びメトスルフロンメチル２％溶液２．０ｇを仕込み、３５０ｒｐｍで回転させながら１分間混合した。次に６５％ジオクチルスルホサクシネート７．５ｇを４００ｒｐｍで回転させながらゆっくり添加した。続いて多孔質珪酸５．０ｇを加えて１分間攪拌後取り出し、風乾して０．１〜０．３ｍｍの粒子を篩い分けして求める微粒剤４９２ｇを得た。(Formulation Example 6) Preparation of Trifloxysulfuron Sodium Salt 0.008% Metosulfuron Methyl 0.008% Fine Granules 483.5 g of fine silica stone and 2.0 g of 2% trifloxysulfuron sodium salt solution in a stirring tank of Mechanomyl Then, 2.0 g of a 2% solution of metsulfuron methyl was charged and mixed for 1 minute while rotating at 350 rpm. Next, 7.5 g of 65% dioctylsulfosuccinate was slowly added while rotating at 400 rpm. Subsequently, 5.0 g of porous silicic acid was added, taken out after stirring for 1 minute, taken out and air-dried to obtain 492 g of a fine granule obtained by sieving 0.1 to 0.3 mm particles.
（製剤例７）メトスルフロンメチル０．００８％グリホサート２．０％ゼオライト微粒剤の調製
メカノミルの攪拌槽に微粒のゼオライト（ゼオグリーン微粒８号、日本ゼオライト株式会社商品）４４８．７ｇとグリホサートイソプロピルアミン４１％液剤（ラウンドアップ液剤、日本モンサント株式会社商品）２４．３ｇ及びメトスルフロンメチル２％溶液２．０ｇを仕込み、３５０ｒｐｍで回転させながら１分間混合した。次に６５％ジオクチルスルホサクシネート２０．０ｇを４００ｒｐｍで回転させながらゆっくり添加した。続いて多孔質珪酸５．０ｇを加えて１分間攪拌後取り出し、風乾して０．１〜０．３ｍｍの粒子を篩い分けして求める微粒剤４９２ｇを得た。(Formulation Example 7) Preparation of methosulfuron methyl 0.008% glyphosate 2.0% zeolite fine granules 448.7 g of fine zeolite (Zeogreen Fine Granule No. 8, product of Nippon Zeolite Co., Ltd.) and glyphosate isopropylamine in a stirring tank of Mechanomyl 24.3 g of 41% solution (Round-up solution, Nippon Monsanto Co., Ltd.) and 2.0 g of metsulfuron methyl 2% solution were charged and mixed for 1 minute while rotating at 350 rpm. Next, 20.0 g of 65% dioctyl sulfosuccinate was slowly added while rotating at 400 rpm. Subsequently, 5.0 g of porous silicic acid was added, taken out after stirring for 1 minute, taken out and air-dried to obtain 492 g of a fine granule obtained by sieving 0.1 to 0.3 mm particles.
（製剤例８）メトスルフロンメチル０．００８％ブロマシル１．０％微粒剤の調製
メカノミルの攪拌槽に微粒の珪石４７９．２ｇとブロマシル８０％水和剤（ハイバーＸ水和剤、デュポン株式会社商品）６．３ｇを仕込み、３５０ｒｐｍで回転させながら１分間混合した。次にメトスルフロンメチル２％溶液２．０ｇをゆっくりと滴下し、さらに１分間混合した。次に７．５ｇのネオスコア２３３９を４００ｒｐｍで回転させながらゆっくり添加した。続いて多孔質珪酸５．０ｇを加えて１分間攪拌後取り出し、風乾して０．１〜０．３ｍｍの粒子を篩い分けして求める微粒剤４９６ｇを得た。(Formulation Example 8) Preparation of Methosulfuronmethyl 0.008% Bromacil 1.0% Fine Granules 479.2g of fine silica stone and 80% bromacil wettable powder (Hiber X wettable powder, DuPont product) ) 6.3 g was charged and mixed for 1 minute while rotating at 350 rpm. Next, 2.0 g of metsulfuron methyl 2% solution was slowly added dropwise and mixed for another 1 minute. Next, 7.5 g of Neoscore 2339 was added slowly while rotating at 400 rpm. Subsequently, 5.0 g of porous silicic acid was added, taken out after stirring for 1 minute, taken out and air-dried to obtain 496 g of a fine granule obtained by sieving 0.1 to 0.3 mm particles.
（製剤例９）メトスルフロンメチル０．００８％ジウロン２．０％微粒剤の調製
メカノミルの攪拌槽に微粒の珪石４７５．３ｇとジウロン７８．５％水和剤（カーメックスＤ水和剤、ナガセグリフィン株式会社商品）１２．７ｇを仕込み、３５０ｒｐｍで回転させながら１分間混合した。次にメトスルフロンメチル２％溶液２．０ｇをゆっくりと滴下し、さらに１分間混合した。次に５．０ｇのネオスコア２３３９を４００ｒｐｍで回転させながらゆっくり添加した。続いて多孔質珪酸５．０ｇを加えて１分間攪拌後取り出し、風乾して０．１〜０．３ｍｍの粒子を篩い分けして求める微粒剤４９５ｇを得た。Formulation Example 9 Preparation of Methosulfuron Methyl 0.008% Diuron 2.0% Fine Granules 475.3 g of fine silica and 78.5% diuron wettable powder (Carmex D wettable powder, Nagase Griffin Co., Ltd. product) 12.7 g was charged and mixed for 1 minute while rotating at 350 rpm. Next, 2.0 g of metsulfuron methyl 2% solution was slowly added dropwise and mixed for another 1 minute. Next, 5.0 g of Neoscore 2339 was added slowly while rotating at 400 rpm. Subsequently, 5.0 g of porous silicic acid was added, taken out after stirring for 1 minute, air-dried, and 495 g of fine particles obtained by sieving 0.1 to 0.3 mm particles were obtained.
（製剤例１０）メトスルフロンメチル０．００８％アシュラム１．５％微粒剤の調製
メカノミルの攪拌槽に微粒のゼオライト４７１．７ｇとアシュラム８０％水溶剤（アージラン水溶剤、アベンティスクロップサイエンス株式会社商品）９．８ｇを仕込み、３５０ｒｐｍで回転させながら１分間混合した。次にメトスルフロンメチル２％溶液２．０ｇをゆっくりと滴下し、さらに１分間混合した。次に７８％ポリオキシエチレンドデシルエーテル（サーファクタントＷＫ、花王株式会社商品）１１．５ｇを４００ｒｐｍで回転させながらゆっくり添加した。続いて多孔質珪酸５．０ｇを加えて１分間攪拌後取り出し、風乾して０．１〜０．３ｍｍの粒子を篩い分けして求める微粒剤４９４ｇを得た。(Formulation Example 10) Preparation of metsulfuron methyl 0.008% ashram 1.5% fine granule 471.7 g of fine zeolite in mechano-mill stirring tank and ashram 80% water solvent (Ajlan Water Solvent, Aventy Scrop Science Co., Ltd.) 9.8 g was charged and mixed for 1 minute while rotating at 350 rpm. Next, 2.0 g of metsulfuron methyl 2% solution was slowly added dropwise and mixed for another 1 minute. Next, 11.5 g of 78% polyoxyethylene dodecyl ether (Surfactant WK, product of Kao Corporation) was slowly added while rotating at 400 rpm. Subsequently, 5.0 g of porous silicic acid was added, taken out after stirring for 1 minute, and air-dried to obtain 494 g of fine particles obtained by sieving 0.1 to 0.3 mm particles.
（製剤例１１）メトスルフロンメチル０．００８％シンメチリン０．７％微粒剤の調製
メカノミルの攪拌槽に微粒の珪石４８３．１ｇとシンメチリン７２％乳剤（アゴールド乳剤、ＢＡＳＦアグロ株式会社商品）４．９ｇ及びメトスルフロンメチル２％溶液２．０ｇを仕込み、３５０ｒｐｍで回転させながら１分間混合した。次に５．０ｇのネオスコア２３３９を４００ｒｐｍで回転させながらゆっくり添加した。続いて多孔質珪酸５．０ｇを加えて１分間攪拌後取り出し、風乾して０．１〜０．３ｍｍの粒子を篩い分けして求める微粒剤４９６ｇを得た。(Formulation Example 11) Preparation of Methosulfuron Methyl 0.008% Cinmethylin 0.7% Fine Granules 483.1 g of fine silicalite and 72% cinmethylin emulsion (Agold emulsion, product of BASF Agro Co., Ltd.) 9 g and 2.0 g of metsulfuron methyl 2% solution were charged and mixed for 1 minute while rotating at 350 rpm. Next, 5.0 g of Neoscore 2339 was added slowly while rotating at 400 rpm. Subsequently, 5.0 g of porous silicic acid was added, taken out after stirring for 1 minute, taken out and air-dried to obtain 496 g of a fine granule obtained by sieving 0.1 to 0.3 mm particles.
（製剤例１２）メトスルフロンメチル０．００８％ピラフルフェンエチル％微粒剤の調製
メカノミルの攪拌槽に微粒の珪石４８３．０ｇとメトスルフロンメチル２％溶液２．０ｇ及びピラフルフェンエチル２％水和剤（エコパートフロアブル、日本農薬株式会社商品）２．５ｇを仕込み、３５０ｒｐｍで回転させながら１分間混合した。次に７．５ｇのネオスコア２３３９を４００ｒｐｍで回転させながらゆっくり添加した。続いて多孔質珪酸５．０ｇを加えて１分間攪拌後取り出し、風乾して０．１〜０．３ｍｍの粒子を篩い分けして求める微粒剤４９３ｇを得た。(Formulation example 12) Preparation of metsulfuron methyl 0.008% pyraflufenethyl% fine granule 483.0 g of fine silicalite, 2.0 g of metsulfuronmethyl 2% solution and pyraflufenethyl 2% water in a stirring tank of Mechanomyl 2.5 g of a preservative (Eco Part Floorable, Nippon Pesticide Co., Ltd.) was charged and mixed for 1 minute while rotating at 350 rpm. Next, 7.5 g of Neoscore 2339 was added slowly while rotating at 400 rpm. Subsequently, 5.0 g of porous silicic acid was added, taken out after stirring for 1 minute, air-dried, and 493 g of a fine granule obtained by sieving 0.1 to 0.3 mm particles was obtained.
（製剤例１３）メトスルフロンメチル０．０１％フルプロパネートナトリウム塩４．０％微粒剤の調製
メカノミルの攪拌槽に微粒のゼオライト４００．５ｇとフルプロパネートナトリウム塩３０％液剤（フレノック液剤、株式会社三共緑化商品）６７．０ｇ及びメトスルフロンメチル０．６％溶液８．３ｇを仕込み、３５０ｒｐｍで回転させながら１分間混合した。次に７８％ポリオキシエチレンドデシルエーテル１９．２ｇを４００ｒｐｍで回転させながらゆっくり添加した。続いて多孔質珪酸５．０ｇを加えて１分間攪拌後取り出し、風乾して０．１〜０．３ｍｍの粒子を篩い分けして求める微粒剤４９６ｇを得た。(Formulation Example 13) Preparation of Methosulfuronmethyl 0.01% Flupropanate Sodium Salt 4.0% Fine Granules 400.5 g of fine zeolite in mechanomil stirring tank and 30% flupropanate sodium salt liquid (Frenoc liquid, stock Company Sankyo Greening Products) 67.0 g and methosulfuron methyl 0.6% solution 8.3 g were charged and mixed for 1 minute while rotating at 350 rpm. Next, 19.2 g of 78% polyoxyethylene dodecyl ether was slowly added while rotating at 400 rpm. Subsequently, 5.0 g of porous silicic acid was added, taken out after stirring for 1 minute, taken out and air-dried to obtain 496 g of a fine granule obtained by sieving 0.1 to 0.3 mm particles.
（製剤例１４）シクロスルファムロン０．１％シンメチリン０．７％微粒剤の調製
メカノミルの攪拌槽に微粒の珪石４７７．６ｇとシンメチリン７２％乳剤４．９ｇ及びシクロスルファムロン１０％溶液５．０ｇを仕込み、３５０ｒｐｍで回転させながら１分間混合した。次に６５％ジオクチルスルホサクシネート７．５ｇを４００ｒｐｍで回転させながらゆっくり添加した。続いて多孔質珪酸５．０ｇを加えて１分間攪拌後取り出し、風乾して０．１〜０．３ｍｍの粒子を篩い分けして求める微粒剤４９６ｇを得た。(Formulation Example 14) Preparation of 0.1% cymethyrin 0.7% fine granule with cyclosulfamuron 477.6 g of fine silica and 4.9 g of symethyline 72% emulsion and cyclosulfamuron 10% solution 5 in a stirring tank of Mechanomyl 0.0 g was charged and mixed for 1 minute while rotating at 350 rpm. Next, 7.5 g of 65% dioctylsulfosuccinate was slowly added while rotating at 400 rpm. Subsequently, 5.0 g of porous silicic acid was added, taken out after stirring for 1 minute, taken out and air-dried to obtain 496 g of a fine granule obtained by sieving 0.1 to 0.3 mm particles.
（製剤例１５）チフェンスルフロンメチル０．０４％シンメチリン０．７％微粒剤の調製
メカノミルの攪拌槽に微粒の珪石４８３．１ｇとシンメチリン７２％乳剤４．９ｇ及びチフェンスルフロンメチル７５％水和剤を１０％懸濁液として２．０ｇを仕込み、３５０ｒｐｍで回転させながら１分間混合した。次に５．０ｇのネオスコア２３３９を４００ｒｐｍで回転させながらゆっくり添加した。続いて多孔質珪酸５．０ｇを加えて１分間攪拌後取り出し、風乾して０．１〜０．３ｍｍの粒子を篩い分けして求める微粒剤４９６ｇを得た。Formulation Example 15 Preparation of Thifensulfuron Methyl 0.04% Cinmethyline 0.7% Fine Granules 483.1 g of fine silicalite and 4.9 g of cinmethyrin 72% emulsion and 75% thifensulfuron methyl hydrated in a stirring tank of Mechanomyl As a 10% suspension of the agent, 2.0 g was charged and mixed for 1 minute while rotating at 350 rpm. Next, 5.0 g of Neoscore 2339 was added slowly while rotating at 400 rpm. Subsequently, 5.0 g of porous silicic acid was added, taken out after stirring for 1 minute, taken out and air-dried to obtain 496 g of a fine granule obtained by sieving 0.1 to 0.3 mm particles.
（製剤例１６）メトスルフロンメチル０．００８％グリホサート１．０％ブロマシル１．０％微粒剤（Ａ）の調製
メカノミルの攪拌槽に微粒のゼオライト４５９．５ｇとブロマシル８０％水和剤６．３ｇを仕込み、３５０ｒｐｍで回転させながら１分間混合した。次にグリホサートイソプロピルアミン４１％液剤１２．２ｇ及びメトスルフロンメチル２％溶液２．０ｇをゆっくりと滴下し、さらに１分間混合した。次に１５．０ｇのネオスコア２３３９を４００ｒｐｍで回転させながらゆっくり添加した。続いて多孔質珪酸５．０ｇを加えて１分間攪拌後取り出し、風乾して０．１〜０．３ｍｍの粒子を篩い分けして求める微粒剤４９２ｇを得た。(Formulation Example 16) Preparation of Methosulfuron Methyl 0.008% Glyphosate 1.0% Bromasil 1.0% Fine Granule (A) 459.5 g of fine zeolite and 6.3 g of bromacil 80% wettable powder in a mechanomill stirring tank Was mixed for 1 minute while rotating at 350 rpm. Next, 12.2 g of a 41% solution of glyphosate isopropylamine and 2.0 g of a 2% solution of metsulfuron methyl were slowly added dropwise and further mixed for 1 minute. Next, 15.0 g of Neoscore 2339 was added slowly while rotating at 400 rpm. Subsequently, 5.0 g of porous silicic acid was added, taken out after stirring for 1 minute, taken out and air-dried to obtain 492 g of a fine granule obtained by sieving 0.1 to 0.3 mm particles.
（製剤例１７）メトスルフロンメチル０．００８％グリホサート１．０％ブロマシル１．０％微粒剤（Ｂ）の調製
メカノミルの攪拌槽に微粒の珪石４６９．５ｇとブロマシル８０％水和剤６．３ｇを仕込み、３５０ｒｐｍで回転させながら１分間混合した。次にグリホサートイソプロピルアミン４１％液剤１２．２ｇ及びメトスルフロンメチル２％溶液２．０ｇをゆっくりと滴下し、さらに１分間混合した。次に５．０ｇのネオスコア２３３９を４００ｒｐｍで回転させながらゆっくり添加した。続いて多孔質珪酸５．０ｇを加えて１分間攪拌後取り出し、風乾して０．１〜０．３ｍｍの粒子を篩い分けして求める微粒剤４９４ｇを得た。(Formulation Example 17) Preparation of Methosulfuron Methyl 0.008% Glyphosate 1.0% Bromasil 1.0% Fine Granule (B) 469.5 g of fine silica stone and 6.3 g of Bromasil 80% wettable powder in a mechano-mill stirring tank Was mixed for 1 minute while rotating at 350 rpm. Next, 12.2 g of a 41% solution of glyphosate isopropylamine and 2.0 g of a 2% solution of metsulfuron methyl were slowly added dropwise and further mixed for 1 minute. Next, 5.0 g of Neoscore 2339 was added slowly while rotating at 400 rpm. Subsequently, 5.0 g of porous silicic acid was added, taken out after stirring for 1 minute, and air-dried to obtain 494 g of fine particles obtained by sieving 0.1 to 0.3 mm particles.
（製剤例１８）メトスルフロンメチル０．００８％グルホシネート０．８％ブロマシル１．０％微粒剤の調製
メカノミルの攪拌槽に微粒のゼオライト４５４．７ｇとブロマシル８０％水和剤６．３ｇを仕込み、３５０ｒｐｍで回転させながら１分間混合した。次にグルホシネート１８．５％液剤（バスタ液剤、バイエルクロップサイエンス株式会社商品）２２．０ｇ及びメトスルフロンメチル２％溶液２．０ｇをゆっくりと滴下し、さらに１分間混合した。次に１０．０ｇのネオスコア２３３９を４００ｒｐｍで回転させながらゆっくり添加した。続いて多孔質珪酸５．０ｇを加えて１分間攪拌後取り出し、風乾して０．１〜０．３ｍｍの粒子を篩い分けして求める微粒剤４９３ｇを得た。(Formulation example 18) Preparation of metsulfuron methyl 0.008% glufosinate 0.8% bromacil 1.0% fine granule 454.7 g of fine zeolite and 6.3 g of bromacil 80% wettable powder were charged in a stirring tank of mechanomyl. The mixture was mixed for 1 minute while rotating at 350 rpm. Next, 22.0 g of glufosinate 18.5% solution (Buster solution, product of Bayer Crop Science Co., Ltd.) and 2.0 g of metsulfuron methyl 2% solution were slowly added dropwise and further mixed for 1 minute. Next, 10.0 g of Neoscore 2339 was added slowly while rotating at 400 rpm. Subsequently, 5.0 g of porous silicic acid was added, taken out after stirring for 1 minute, air-dried, and 493 g of a fine granule obtained by sieving 0.1 to 0.3 mm particles was obtained.
（製剤例１９）メトスルフロンメチル０．００８％グリホサート１．０％ジウロン２．０％微粒剤の調製
メカノミルの攪拌槽に微粒のゼオライト４５３．１ｇとジウロン７８．５％水和剤１２．７ｇを仕込み、３５０ｒｐｍで回転させながら１分間混合した。次にグリホサートイソプロピルアミン４１％液剤１２．２ｇ及びメトスルフロンメチル２％溶液２．０ｇをゆっくりと滴下し、さらに１分間混合した。次に１５．０ｇのネオスコア２３３９を４００ｒｐｍで回転させながらゆっくり添加した。続いて多孔質珪酸５．０ｇを加えて１分間攪拌後取り出し、風乾して０．１〜０．３ｍｍの粒子を篩い分けして求める微粒剤４９２ｇを得た。(Formulation Example 19) Preparation of metsulfuron methyl 0.008% glyphosate 1.0% diuron 2.0% fine granule 453.1 g of fine zeolite and 12.7 g of diuron 78.5% wettable powder were added to the stirring tank of Mechanomyl. The mixture was charged and mixed for 1 minute while rotating at 350 rpm. Next, 12.2 g of a 41% solution of glyphosate isopropylamine and 2.0 g of a 2% solution of metsulfuron methyl were slowly added dropwise and further mixed for 1 minute. Next, 15.0 g of Neoscore 2339 was added slowly while rotating at 400 rpm. Subsequently, 5.0 g of porous silicic acid was added, taken out after stirring for 1 minute, taken out and air-dried to obtain 492 g of a fine granule obtained by sieving 0.1 to 0.3 mm particles.
（製剤例２０）メトスルフロンメチル０．００８％グリホサート１．０％シンメチリン０．７％微粒剤の調製
メカノミルの攪拌槽に微粒の珪石４７０．９ｇとシンメチリン７２％水和剤４．９ｇを仕込み、３５０ｒｐｍで回転させながら１分間混合した。次にグリホサートイソプロピルアミン４１％液剤１２．２ｇ及びメトスルフロンメチル２％溶液２．０ｇをゆっくりと滴下し、さらに１分間混合した。次に６５％ジオクチルスルホサクシネート５．０ｇを４００ｒｐｍで回転させながらゆっくり添加した。続いて多孔質珪酸５．０ｇを加えて１分間攪拌後取り出し、風乾して０．１〜０．３ｍｍの粒子を篩い分けして求める微粒剤４９２ｇを得た。(Preparation Example 20) Preparation of metsulfuron methyl 0.008% glyphosate 1.0% cymethyline 0.7% fine granule 470.9 g of fine silicalite and 4.9 g of symethyline 72% wettable powder were charged in a stirring tank of Mechanomyl. The mixture was mixed for 1 minute while rotating at 350 rpm. Next, 12.2 g of a 41% solution of glyphosate isopropylamine and 2.0 g of a 2% solution of metsulfuron methyl were slowly added dropwise and further mixed for 1 minute. Next, 5.0 g of 65% dioctylsulfosuccinate was slowly added while rotating at 400 rpm. Subsequently, 5.0 g of porous silicic acid was added, taken out after stirring for 1 minute, taken out and air-dried to obtain 492 g of a fine granule obtained by sieving 0.1 to 0.3 mm particles.
（製剤例２１）メトスルフロンメチル０．００８％グリホサート２．０％ペンディメタリン１．２％微粒剤の調製
メカノミルの攪拌槽に微粒のゼオライト４４０．４ｇとペンディメタリン４５％水和剤（ウェイアップフロアブル、ＢＡＳＦアグロ株式会社商品）１３．３ｇ及びグリホサートイソプロピルアミン４１％液剤２４．３ｇ及びメトスルフロンメチル２％溶液２．０ｇを仕込み、３５０ｒｐｍで回転させながら１分間混合した。次に１５．０ｇのネオスコア２３３９を４００ｒｐｍで回転させながらゆっくり添加した。続いて多孔質珪酸５．０ｇを加えて１分間攪拌後取り出し、風乾して０．１〜０．３ｍｍの粒子を篩い分けして求める微粒剤４９２ｇを得た。(Formulation Example 21) Preparation of metsulfuron methyl 0.008% glyphosate 2.0% pendimethalin 1.2% fine granules 440.4 g of fine zeolite and 45% pendimethalin wettable powder (way) Upflowable, product of BASF Agro Co., Ltd.) 13.3 g, glyphosate isopropylamine 41% solution 24.3 g and metsulfuron methyl 2% solution 2.0 g were charged and mixed for 1 minute while rotating at 350 rpm. Next, 15.0 g of Neoscore 2339 was added slowly while rotating at 400 rpm. Subsequently, 5.0 g of porous silicic acid was added, taken out after stirring for 1 minute, taken out and air-dried to obtain 492 g of a fine granule obtained by sieving 0.1 to 0.3 mm particles.
（製剤例２２）メトスルフロンメチル０．００８％ブロマシル１．０％ピラフルフェンエチル０．０１％微粒剤の調製
メカノミルの攪拌槽に微粒の珪石４７６．７ｇとブロマシル８０％水和剤６．３ｇを仕込み、３５０ｒｐｍで回転させながら１分間混合した。次にメトスルフロンメチル２％溶液２．０ｇ及びピラフルフェンエチル２％水和剤２．５ｇをゆっくりと滴下し、さらに１分間混合した。次に７．５ｇのネオスコア２３３９を４００ｒｐｍで回転させながらゆっくり添加した。続いて多孔質珪酸５．０ｇを加えて１分間攪拌後取り出し、風乾して０．１〜０．３ｍｍの粒子を篩い分けして求める微粒剤４９２ｇを得た。(Formulation Example 22) Preparation of metsulfuron methyl 0.008% bromacil 1.0% pyraflufenethyl 0.01% fine granule 476.7 g of fine silica stone and 6.3 g of bromacil 80% wettable powder in a stirring tank of Mechanomyl Was mixed for 1 minute while rotating at 350 rpm. Next, 2.0 g of metsulfuron methyl 2% solution and 2.5 g of pyraflufenethyl 2% wettable powder were slowly added dropwise and further mixed for 1 minute. Next, 7.5 g of Neoscore 2339 was added slowly while rotating at 400 rpm. Subsequently, 5.0 g of porous silicic acid was added, taken out after stirring for 1 minute, taken out and air-dried to obtain 492 g of a fine granule obtained by sieving 0.1 to 0.3 mm particles.
（製剤例２３）メトスルフロンメチル０．００５％ジウロン１．５％シンメチリン０．５％微粒剤の調製
メカノミルの攪拌槽に微粒の珪石４７５．６ｇとジウロン７８．５％水和剤９．６ｇ及びシンメチリン７２％水和剤３．５ｇを仕込み、３５０ｒｐｍで回転させながら１分間混合した。次にメトスルフロンメチル２％溶液１．３ｇをゆっくりと滴下し、さらに１分間混合した。次にネオスコア２３３９ ５．０ｇを４００ｒｐｍで回転させながらゆっくり添加した。続いて多孔質珪酸５．０ｇを加えて１分間攪拌後取り出し、風乾して０．１〜０．３ｍｍの粒子を篩い分けして求める微粒剤４９２ｇを得た。(Formulation example 23) Preparation of metsulfuron methyl 0.005% diuron 1.5% cymethyline 0.5% fine granule In a stirring tank of Mechanomyl, 475.6 g of fine silica and 9.6 g of diuron 78.5% wettable powder and Cinmethylin 72% wettable powder 3.5 g was charged and mixed for 1 minute while rotating at 350 rpm. Next, 1.3 g of metsulfuron methyl 2% solution was slowly added dropwise and mixed for another 1 minute. Next, 5.0 g of Neoscore 2339 was slowly added while rotating at 400 rpm. Subsequently, 5.0 g of porous silicic acid was added, taken out after stirring for 1 minute, taken out and air-dried to obtain 492 g of a fine granule obtained by sieving 0.1 to 0.3 mm particles.
上記製剤例１〜２３、及び対照薬剤の植物に対する除草効果をポット及び圃場で比較検討した。 The herbicidal effects of the above Formulation Examples 1 to 23 and the control drug on plants were compared in pots and fields.
（除草効果試験例１）ポット試験
２００ｃｍ２のポットに養生した草丈１０ｃｍ程度のオナモミとヒエ、ツルマメに対し、微粒剤を散布した。対照薬剤として用いたグリホサート２．０％微粒剤は製剤実施例１６に準じて調製した。除草効果は処理３日後、１週間後、２週間後、３週間後に薬剤に対する反応の度合いによって評価した。試験は各剤２反復として２００４年４月２３日に実施した。その結果の平均値を表１に示す。(Herbicidal Effect Test Example 1) Pot Test A fine granule was sprayed on onomami, millet, and beans with a height of about 10 cm, which were cured in a 200 cm 2 pot. A glyphosate 2.0% fine granule used as a control drug was prepared according to Formulation Example 16. The herbicidal effect was evaluated by the degree of response to the drug after 3 days, 1 week, 2 weeks and 3 weeks after treatment. The test was conducted on April 23, 2004 as two repeats of each agent. The average value of the results is shown in Table 1.
表１からも明らかな通り、本発明に係る微粒剤は、オナモミ、ヒエ、ツルマメに対して従来の微粒剤よりも迅速且つ長期間に亘って効果を上げることができる。 As is clear from Table 1, the fine granule according to the present invention can increase the effect on onamomi, mackerel, and swine beans more quickly and over a long period of time than the conventional fine granule.
（除草効果試験例２）圃場試験
草丈１０〜４０ｃｍのシロザ、ハコベ、メヒシバ、タデ、イヌビエ等が発生している茨城県つくば市下別府地区の圃場を１区１．０ｍ×１．５ｍに区切り、微粒剤及び市販対照薬剤を散布した。市販対照薬剤、草退治粒剤（シアナジン１．０％、ジウロン３．０％、ジクロベニル（ＩＳＯ名ｄｉｃｈｌｏｂｅｎｉｌ）１．５％混合粒剤、住化タケダ園芸株式会社商品）の薬量は登録範囲内とした。除草効果は処理３日後、１週間後、２週間後、４週間後、６週間後に薬剤に対する反応の度合いによって評価した。試験は各剤２反復として２００４年５月２８日に実施した。その結果の平均値を表２に示す。(Weeding effect test example 2) Field test The field in Shimobeppu district, Tsukuba City, Ibaraki Prefecture, where 10-40 cm tall Shiroza, leafhopper, Japanese bark, Japanese beetle, etc. are generated is divided into 1.0 mx 1.5 m in 1 ward. Sprayed with fine granules and commercially available control drug. The doses of commercially available control drugs, herbal extermination granules (cyanazine 1.0%, diuron 3.0%, diclobenil 1.5% mixed granule, Sumika Takeda Horticultural Co., Ltd. products) are within the registration range It was. The herbicidal effect was evaluated by the degree of reaction to the drug after 3 days, 1 week, 2 weeks, 4 weeks, and 6 weeks after treatment. The test was conducted on May 28, 2004 as 2 repetitions of each agent. The average value of the results is shown in Table 2.
（除草効果試験例３）圃場試験
草丈５〜２０ｃｍのシロザ、オランダミミナグサ、ナズナ、ハコベ、メヒシバ、イヌビエ等が発生している茨城県つくば市下別府地区の圃場を１区１．０ｍ×１．５ｍに区切り、微粒剤及び市販対照薬剤、草退治粒剤を散布した。市販対照薬剤の薬量は登録範囲内とした。除草効果は処理３日後、１週間後、２週間後、４週間後、６週間後に薬剤に対する反応の度合いによって評価した。試験は各剤２反復として２００４年５月１２日に実施した。
その結果の平均値を表３に示す。(Weeding effect test example 3) Field test A field in Shimobeppu district, Tsukuba City, Ibaraki Prefecture, where 5-20 cm tall Shiroza, Dutch white primrose, Japanese tuna, Japanese chickweed, Japanese barnyard beetle, Inbiebi, etc. are generated is 1.0m x 1.5m And was sprayed with fine granules, commercially available control drugs, and herbicide granules. The dosage of the marketed control drug was within the registration range. The herbicidal effect was evaluated by the degree of reaction to the drug after 3 days, 1 week, 2 weeks, 4 weeks, and 6 weeks after treatment. The test was conducted on May 12, 2004 as 2 repeats of each agent.
The average value of the results is shown in Table 3.
表３の通り、本発明に係る製剤８、１７、１８、２２、即ち、微粒剤はシロザ、オランダミミナグサ、ナズナ、ハコベ、メヒシバ、イヌビエ等に対しても従来の草退治粒剤等よりも有効であることは明らかである。 As shown in Table 3, the preparations 8, 17, 18, and 22 according to the present invention, that is, the fine granules are more effective than white herbicide granules, etc. It is clear that there is.
（除草効果試験例４）圃場試験
草丈５〜２０ｃｍ程度のシロザ、オランダミミナグサ、ナズナ、ハコベ、スズメノテッポウ、ノミノフスマ等が発生している茨城県つくば市下別府地区の圃揚を１区１．０ｍ×１．５ｍに区切り、微粒剤と比較対照粒剤及び市販対照薬剤、カソロン粒剤２．５（ジクロベニル２．５％粒剤、北興化学株式会社商品）、ザイトロン微粒剤（トリクロピル（ＩＳＯ名ｔｒｉｃｈｏｐｙｒ）３．０％微粒剤、保土谷アグロス株式会社商品）を散布した。比較対照粒剤は担体を粒子径０．６〜１．７ｍｍの珪砂（珪砂Ｖ３号、三河珪石株式会社商品）を用い製剤例１１に準じて調製した。市販対照薬剤の薬量は登録範囲内とした。除草効果は処理３日後、１週間後、２週間後、４週間後、６週間後に薬剤に対する反応の度合いによって評価した。試験は各剤２反復として２００４年４月２３日に実施した。その結果の平均値を表４に示す。(Herbicidal effect test example 4) Field test Farming in Shimo-Beppu district, Tsukuba city, Ibaraki prefecture, where Shiroza, Dutch Mimosa, Nazuna, Jacobe, Suzumenoteppo, Nominofusuma, etc., with a plant height of about 5-20 cm, is generated. .5 m, fine granules, comparative control granules and commercially available control drugs, catolone granules 2.5 (dicrobenyl 2.5% granules, Hokuko Chemical Co., Ltd.), zytron granules (Triclopyr (ISO name trichopyr) 3 0.0% fine granule, Hodogaya Agros Co., Ltd. product) was sprayed. The comparative granule was prepared according to Formulation Example 11 using silica sand (silica sand V3, product of Mikawa Silica Co., Ltd.) having a particle size of 0.6 to 1.7 mm. The dosage of the marketed control drug was within the registration range. The herbicidal effect was evaluated by the degree of reaction to the drug after 3 days, 1 week, 2 weeks, 4 weeks, and 6 weeks after treatment. The test was conducted on April 23, 2004 as two repeats of each agent. The average value of the results is shown in Table 4.
表４の通り、本発明に係る製剤例１０、１１、１９、２０、２１は従来の粒剤、微粒剤に比較して有効であることは明らかである。 As shown in Table 4, it is clear that Formulation Examples 10, 11, 19, 20, and 21 according to the present invention are more effective than conventional granules and fine granules.
（除草効果試験例５）圃場試験
草丈５ｃｍ程度のイネ科雑草スズメノテッポウ、３ｃｍ程度の広葉雑草ノミノフスマ、タネツケバナが発生している佐賀県神埼郡地区の麦畑を１区２．０ｍ×２．５ｍに区切り、微粒剤及び市販対照薬剤を散布した。市販対照薬剤、ハーモニー７５ＤＦ水和剤（チフェンスルフロンメチル７５％顆粒水和剤、デュポン株式会社商品）ハーモニー細粒剤Ｆ（チフェンスルフロンメチル０．１５％粉粒剤、丸和バイオケミカル株式会社商品）、クリアターン細粒剤Ｆ（チオベンカーブ（ＩＳＯ名ｔｈｉｏｂｅｎｃａｒｂ）８．０％、ペンディメタリン０．８％、リニュロン（ＩＳＯ名ｌｉｎｕｒｏｎ）１．２％混合粉粒剤、クミアイ化学株式会社商品）の薬量は登録範囲内とした。除草効果は処理２４日後、５３日後に薬剤に対する反応の度合いによって評価した。試験は各剤２反復として２００３年１２月２７日に実施した。その結果の平均値を表５に示す。(Weeding effect test example 5) Field test A grass field in the Kanzaki district of Saga Prefecture, where the weeds of the grass weeds, about 3 cm wide, and the broad-leaved weeds Nominofusuma, about 3 cm wide, are divide into 2.0 mx 2.5 m. Sprayed with fine granules and commercially available control drug. Market control drug, Harmony 75DF wettable powder (Thifensulfuron methyl 75% granule wettable powder, DuPont Co., Ltd. product) Harmony fine granule F (Tifensulfuron methyl 0.15% powder, Maruwa Biochemical Co., Ltd. product) ), Clear Turn Fine Granule F (thioben curve (ISO name thiobencarb) 8.0%, pendimethalin 0.8%, linuron (ISO name linuron) 1.2% mixed granule, product of Kumiai Chemical Co., Ltd.) The dose was within the registration range. The herbicidal effect was evaluated by the degree of response to the drug 24 days after treatment and 53 days later. The test was conducted on December 27, 2003 as 2 repeats of each agent. The average value of the results is shown in Table 5.
上記の試験で明らかのように、微粒剤にすることで粒剤よりも成分含有量を減らすことができ、更に速効的かつ安定した効果を確認することができた。 As is apparent from the above test, the content of the components can be reduced by using fine granules, and a more rapid and stable effect can be confirmed.
（除草効果試験例６）圃場試験
草丈１０ｃｍ程度のスギナ、メヒシバ、タデ、シロザが発生している茨城県つくば市下別府地区の圃場を１区１．０ｍ×１．５ｍに区切り、微粒剤及び市販対照薬剤を散布した。市販対照薬剤、クサノンＶ粒剤（ジウロン４．０％、ダラポン（一般名ｄａｌａｐｏｎ）１０．０％、メコプロップ（ＩＳＯ名ｍｅｃｏｐｒｏｐ）４．０％混合粒剤、住化タケダ園芸株式会社商品）、ネコソギエースＡ粒剤（イソウロン１．０％、ジウロン６．０％、ジクロベニル３．０％混合粒剤、レインボー薬品株式会社商品）の薬量は登録範囲内とした。除草効果は処理３日後、１週間後、２週間後、４週間後、６週間後に薬剤に対する反応の度合いによって評価した。試験は各剤２反復として２００４年７月１３日に実施した。その結果の平均値を表６に示す。(Weeding effect test example 6) Field test A field in Shimobeppu district, Tsukuba city, Ibaraki, where cedar, mosquito, tade, and shiroza with a plant height of about 10 cm are generated is divided into 1.0 mx 1.5 m in 1 ward, A commercial control drug was sprayed. Commercially available control drug, xanon V granule (diuron 4.0%, dalapon (generic name: dalapon) 10.0%, mecoprop (ISO name mecoprop) 4.0% mixed granule, Sumika Takeda Horticultural Co., Ltd.), cat sogi The dosage of Ace A granules (isouron 1.0%, diuron 6.0%, diclobenil 3.0% mixed granules, products of Rainbow Chemical Co., Ltd.) was within the registration range. The herbicidal effect was evaluated by the degree of reaction to the drug after 3 days, 1 week, 2 weeks, 4 weeks, and 6 weeks after treatment. The test was conducted on July 13, 2004 as 2 repeats for each agent. The average value of the results is shown in Table 6.
（除草効果試験例７）圃場試験
草丈１０〜２０ｃｍ程度のシロザ、ナズナ、ブタクサ等が発生している千葉県印旛郡酒々井町地区の圃場を１区１．０ｍ×１．５ｍに区切り、微粒剤及び市販対照薬剤を散布した。市販対照薬剤、ダイロン微粒剤（ジウロン３．０％微粒剤、住化タケダ園芸株式会社商品）、草退治粒剤の薬量は登録範囲内とした。除草効果は処理３日後、１週間後、２週間後、４週間後、６週間後に薬剤に対する反応の度合いによって評価した。試験は各剤２反復として２００３年６月３日に実施した。その結果の平均値を表７に示す。(Example 7 of herbicidal effect test) Field test The field in Shisui-cho, Inba-gun, Chiba Prefecture, where the plant is about 10-20cm in height, such as Shiroza, Nazuna, Ragweed, etc., is divided into 1.0m x 1.5m in 1 ward and divided into fine granules And a commercial control drug was sprayed. The doses of the commercially available control drug, Dyrone fine granules (Diuron 3.0% fine granules, Sumika Takeda Horticultural Co., Ltd.) and herbicide granules were within the registration range. The herbicidal effect was evaluated by the degree of reaction to the drug after 3 days, 1 week, 2 weeks, 4 weeks, and 6 weeks after treatment. The test was conducted on June 3, 2003 as two repeats for each agent. The average value of the results is shown in Table 7.
（除草効果試験例８）圃場試験
草丈５〜１０ｃｍ程度のササ、４０ｃｍ程度のススキ、１０〜２０ｃｍ程度のヘビイチゴ、ヨモギ、セイタカアワダチソウ、チヂミザサ等が発生している茨城県筑波郡伊奈町地区の松林を１区１．０ｍ×１．０ｍに区切り、微粒剤と比較対照の細粒剤及び市販対照薬剤、フレノック液剤（フルプロパネートナトリウム塩３０％液剤、株式会社三共緑化商品）を散布した。市販対照薬剤の薬量は登録範囲内とした。比較対照の細粒剤は、担体を粒子径０．３〜０．８５ｍｍの珪砂（珪砂Ｖ５号、三河珪石株式会社商品）を用い製剤例１３に準じて調製した。除草効果は処理１ヶ月後、４ヶ月後、６ヶ月後、８ヶ月後に薬剤に対する反応の度合いによって評価した。試験は各剤１反復として２００３年１０月２１日に実施した。その結果の平均値を表８に示す。(Weeding effect test example 8) Field test A pine forest in Ina-cho, Tsukuba-gun, Ibaraki Prefecture, where 5 to 10 cm tall Sasa, 40 cm Susuki, 10 to 20 cm snake strawberry, mugwort, black-tailed millet, swordfish, etc. are generated Were divided into 1.0 m × 1.0 m, and fine granules, comparative fine granules, commercially available control drugs, and Frenoc solution (flupropanate sodium salt 30% solution, Sankyo Greening Co., Ltd.) were sprayed. The dosage of the marketed control drug was within the registration range. A comparative fine granule was prepared according to Formulation Example 13 using silica sand (silica sand V5, product of Mikawa Silica Co., Ltd.) having a particle size of 0.3 to 0.85 mm as a carrier. The herbicidal effect was evaluated by the degree of reaction to the drug after 1 month, 4 months, 6 months, and 8 months after treatment. The test was conducted on October 21, 2003 as one repetition of each agent. The average value of the results is shown in Table 8.
（除草効果試験例９）圃場試験
草丈２０〜５０ｃｍ程度のメヒシバ、１０〜３０ｃｍ程度のシロザ、５〜２０ｃｍ程度のスギナ、スベリヒユ、ハコベ等が発生している茨城県つくば市下別府地区の圃場を１区１．０ｍ×１．０ｍに区切り、微粒剤及び市販対照薬剤、ハイバーＸ粒剤１．５（ブロマシル１．５％粒剤、丸和バイオケミカル株式会社商品）、ネコソギエース粒剤（イソウロン１．０％、ジウロン６．０％、クロルチアミド（一般名ｃｈｌｏｒｔｈｉａｍｉｄ）３．０％混合粒剤、保土谷化学工業株式会社商品）を散布した。市販対照薬剤の薬量は登録範囲内とした。除草効果は処理１週間後、２週間後、４週間後、６週間後に薬剤に対する反応の度合いによって評価した。試験は各剤２反復として２００３年８月４日に実施した。その結果の平均値を表９に示す。(Example 9 of herbicidal effect test) Field test A field in Shimo-Beppu district, Tsukuba city, Ibaraki prefecture, where vegetation 20 to 50 cm in height, Shiroza about 10 to 30 cm, Sugina 5 to 20 cm, Sugahiyu, Hakobe, etc. are generated. Divided into 1 section 1.0m x 1.0m, fine granules and commercially available control drugs, Hiber X granules 1.5 (Bromasil 1.5% granules, Maruwa Biochemical Co., Ltd. products), Nekosogiace granules (Isouron 1 0.0%, diuron 6.0%, chlorthiamid (generic name: chlorthiamid) 3.0% mixed granule, Hodogaya Chemical Co., Ltd. product) was sprayed. The dosage of the marketed control drug was within the registration range. The herbicidal effect was evaluated by the degree of response to the drug after 1 week, 2 weeks, 4 weeks and 6 weeks of treatment. The test was conducted on August 4, 2003 as 2 repeats for each agent. The average value of the results is shown in Table 9.
試験例９で明らかなように除草効果試験例１に比較して、処理薬量を減らすことにより、散布直後に植物上部の枯死を認めたが、その後長期間イネ科雑草の生育を抑制することが確認された。 As is clear from Test Example 9, compared to Herbicidal Effect Test Example 1, by reducing the amount of treatment, plant death was observed immediately after spraying, but thereafter the growth of grass weeds was suppressed for a long period of time. Was confirmed.
以上の試験例で明らかなように、アセトラクテート合成阻害剤（ＡＬＳＩ剤）を水溶性高沸点有機物質と共に微粒な鉱物に付着もしくは含浸させることによって、除草用もしくは生育抑制用微粒剤としての使用を可能にした。 As is clear from the above test examples, the acetolactate synthesis inhibitor (ALSI agent) is attached to or impregnated into fine minerals together with water-soluble high-boiling organic substances, so that it can be used as a fine granule for herbicidal or growth suppression. Made possible.
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