JP2003252702A - Improved method for producing agrochemical granule - Google Patents
Improved method for producing agrochemical granuleInfo
- Publication number
- JP2003252702A JP2003252702A JP2002055187A JP2002055187A JP2003252702A JP 2003252702 A JP2003252702 A JP 2003252702A JP 2002055187 A JP2002055187 A JP 2002055187A JP 2002055187 A JP2002055187 A JP 2002055187A JP 2003252702 A JP2003252702 A JP 2003252702A
- Authority
- JP
- Japan
- Prior art keywords
- pesticide
- producing
- active ingredient
- thermoplastic material
- agrochemical
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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Abstract
Description
【0001】[0001]
【発明の属する技術分野】本発明は土壌に施用する徐放
性農薬粒剤の製造方法に関する。更に詳しくは、該農薬
粒剤の生産効率を高めた製造方法に関する。TECHNICAL FIELD The present invention relates to a method for producing a sustained-release agricultural chemical granule applied to soil. More specifically, it relates to a production method in which the production efficiency of the agricultural chemical granules is enhanced.
【0002】[0002]
【従来の技術】近年の農業分野においては、低コスト
化、省力化を指向して急速にその栽培規模、栽培方法が
変革されてきている。それに対応するように農薬の散布
方法に関する技術革新が進み、各種省力型製剤及び散布
方法が検討されるようになり、これまでは不可能と思わ
れてきた農薬製剤が開発されている。その一例として、
農薬製剤からの農薬活性成分の放出を長期間持続する徐
放化製剤の開発が挙げられる。この製剤は、その徐放化
機構により、これまで環境中に流亡するなどして有効に
植物体へ吸収されなかった農薬活性成分を効率よく植物
体へ吸収させることができるため、長期間の植物体内濃
度の維持が可能となり、ひいては長期間の病害虫防除を
達成することができる。そのため長期にわたって農薬活
性成分の効力を持続させる徐放化製剤は理想的な製剤で
ある。2. Description of the Related Art In recent years, in the agricultural field, the cultivation scale and cultivation method have been rapidly changed in order to reduce costs and save labor. Correspondingly, technological innovations related to pesticide application methods have advanced, various labor-saving formulations and application methods have been studied, and pesticide formulations that have been considered impossible until now have been developed. As an example,
The development of sustained-release preparations that sustain the release of pesticide active ingredients from pesticide preparations for a long period of time is mentioned. Due to its sustained release mechanism, this formulation can efficiently absorb into the plant a pesticidal active ingredient that has not been effectively absorbed into the plant until now because it has been washed away into the environment. The concentration in the body can be maintained, and thus pest control can be achieved for a long period of time. Therefore, a sustained-release preparation that maintains the efficacy of pesticide active ingredients for a long period of time is an ideal preparation.
【0003】このような農薬活性成分の放出を制御した
農薬製剤の製造方法として、WO95/09532号に
は農薬活性成分、融点50℃以上の疎水性物質及び吸油
能を有する物質を含有する農薬組成物を、該疎水性物質
の融点以上の加熱条件下で押し出し造粒する方法が、W
O95/28835号には融点などの物性が異なる複数
のワックス及び農薬活性成分を必須成分として多軸型エ
クストルーダーにより、使用するワックスのうち、最も
高い融点のワックスの融点以下に、エクストルーダーの
バレル及びダイスの温度を設定して、混練、押し出し造
粒を一括して行う、農薬含有ワックスマトリックスの製
法が開示されている。この方法では、エクストルーダー
のバレル及びダイスの設定温度を、使用するワックスの
うち最も高い融点のワックスの融点より5〜30℃程度
低い温度に設定することが望ましいことも開示してい
る。また、特開2000−26206号公報には農薬活
性成分、融点が60℃以上で農薬活性成分の融点未満で
かつ酸価が一定範囲内のエステル系疎水性物質、及び無
機系希釈担体を加熱しながら混合し、造粒する方法が開
示されている。As a method for producing an agrochemical formulation in which the release of such an agrochemical active ingredient is controlled, WO95 / 09532 discloses an agrochemical composition containing an agrochemical active ingredient, a hydrophobic substance having a melting point of 50 ° C. or higher and a substance having an oil absorbing ability. The method of extruding and granulating a product under heating conditions above the melting point of the hydrophobic substance is W
O95 / 28835 uses a multi-screw extruder with a plurality of waxes having different physical properties such as melting points and agrochemical active ingredients as essential components, and among the waxes used, below the melting point of the highest melting wax, the extruder barrel Also disclosed is a method for producing a pesticide-containing wax matrix, in which the temperature of a die is set, and kneading and extrusion granulation are collectively performed. This method also discloses that it is desirable to set the set temperature of the barrel and die of the extruder to a temperature about 5 to 30 ° C. lower than the melting point of the highest melting wax among the waxes used. In JP-A-2000-26206, a pesticide active ingredient, an ester-based hydrophobic substance having a melting point of 60 ° C. or higher and lower than the pesticide active ingredient and an acid value within a certain range, and an inorganic diluent carrier are heated. While mixing, the method of granulating is disclosed.
【0004】WO95/09532号記載の方法では、
該疎水性物質の融点以上で押し出し造粒を行うため、押
し出し直後の造粒物の表面は溶融した疎水性物質が付着
しており、そのため、造粒物がベトついており、ダンゴ
状の造粒物生成量が多く、低い生産効率に難点があっ
た。In the method described in WO95 / 09532,
Since extrusion granulation is performed at a temperature above the melting point of the hydrophobic substance, the surface of the granulated product immediately after extrusion is adhered with the molten hydrophobic substance, and therefore, the granulated product is sticky and has a dango-like granulation. There is a problem in that the production amount is large and the production efficiency is low.
【0005】WO95/28835号には、エクストル
ーダーのバレル及びダイの設定温度しか開示していな
く、本発明者が本方法を実施しても、粉体が多い規格外
品が多く、生産効率は悪かった。[0005] WO95 / 28835 discloses only the set temperature of the barrel and die of the extruder. Even if the present inventor carries out the present method, there are many nonstandard products containing a large amount of powder, and the production efficiency is high. It was bad.
【0006】特開2000−26206号公報において
も、造粒時の温度条件の具体的な開示はされていない。[0006] Japanese Patent Application Laid-Open No. 2000-26206 also does not disclose a specific temperature condition during granulation.
【0007】つまり、農薬活性成分、熱可塑性材料、及
び無機系希釈担体からなる農薬粒剤の製造方法におい
て、農薬活性成分の徐放性を保持したままで、高い生産
効率を得ることができる製造方法として、押し出し造粒
時の好適な温度条件は知られていない。That is, in a method for producing an agricultural chemical granule comprising an agricultural chemical active ingredient, a thermoplastic material, and an inorganic diluent carrier, high production efficiency can be obtained while maintaining sustained release of the agricultural chemical active ingredient. As a method, suitable temperature conditions for extrusion granulation are not known.
【0008】[0008]
【発明が解決しようとする課題】本発明の目的は、農薬
活性成分、1種類の熱可塑性材料、及び無機系希釈担体
からなる農薬粒剤において、均質な徐放性を維持すると
ともに安定、且つ高い生産性を達成し得る製造方法を提
供することにある。SUMMARY OF THE INVENTION An object of the present invention is to provide a pesticide granule comprising a pesticide active ingredient, one kind of thermoplastic material, and an inorganic diluent carrier, while maintaining a uniform sustained release property and stable, and It is to provide a manufacturing method capable of achieving high productivity.
【0009】[0009]
【課題を解決するための手段】本発明者らは、これらの
課題を解決すべく、(i)混合工程、(ii)混練工
程、(iii)押し出し工程を通して製造される農薬粒
剤の製造条件について鋭意検討した結果、農薬活性成
分、1種類の熱可塑性材料、及び無機系希釈担体からな
る農薬組成物を押し出し造粒する際、熱可塑性材料の凝
固点以上、融点未満の温度で、押し出し造粒を行うこと
により、製造により生じる不良品が減少し、高い生産性
が確保できることを見い出し、本発明を完成させた。Means for Solving the Problems In order to solve these problems, the present inventors have prepared (a) a mixing step, (ii) a kneading step, and (iii) an extrusion step for producing pesticide granules. As a result of diligent study, when extruding and granulating an agrochemical composition comprising an agrochemical active ingredient, one kind of thermoplastic material, and an inorganic diluent carrier, extrusion granulation at a temperature not lower than the freezing point of the thermoplastic material and lower than the melting point. By carrying out the above, it was found that defective products caused by manufacturing can be reduced and high productivity can be secured, and the present invention was completed.
【0010】すなわち、本発明は以下のとおりである。
[1] 農薬活性成分、1種類の熱可塑性材料、及び無
機系希釈担体からなる農薬粒剤を、(i)混合工程、
(ii)混練工程、(iii)押し出し工程を通して製
造する方法において、該熱可塑性材料の凝固点以上、融
点未満の温度で、押し出し造粒を行うことを特徴とする
農薬粒剤の製造方法。
[2] 農薬活性成分が水溶解度60ppm以上の物質
であることを特徴とする[1]記載の農薬粒剤の製造方
法。
[3]農薬活性成分がニテンピラム、イミダクロプリ
ド、アセタミプリド、3-(2-クロロチアゾール-5-イルメ
チル)-5-メチル-1,3,5-オキサジアジナン-4-イリデン-N
-(ニトロ)アミン(一般名チアメトキサム)、(E)-1-
(2-クロロ-1,3-チアゾール-5-イルメチル)-3-メチル-2-
ニトログアニジン(一般名クロチアニジン)、N-[3-(6-
クロロピリジン-3-イルメチル)チアゾリジン-2-イリデ
ン]シアナミド(一般名チアクロプリド)、(RS)-1-メチ
ル-2-ニトロ-3-[(3-テトラヒドロフリル)メチル]グア
ニジン(一般名ジノテフラン)から選ばれる一種以上の
化合物であることを特徴とする[2]記載の農薬粒剤の
製造方法。
[4] 熱可塑性材料が疎水性物質であることを特徴と
する[1]〜[3]の何れか一項に記載の農薬粒剤の製
造方法。
[5] 疎水性物質がモンタン酸エステルワックスであ
ることを特徴とする[4]記載の農薬粒剤の製造方法。
[6] 農薬活性成分、1種類の熱可塑性材料、及び無
機系希釈担体からなる農薬組成物を押し出し造粒するに
おいて、使用する押し出し機がスクリュー式の押し出し
機であることを特徴とする[1]〜[5]の何れか一項
に記載の農薬粒剤の製造方法。That is, the present invention is as follows. [1] A pesticide granule comprising an agrochemical active ingredient, one kind of thermoplastic material, and an inorganic diluent carrier, (i) mixing step,
A method for producing an agrochemical granule, which comprises performing extrusion granulation at a temperature not lower than the freezing point and lower than the melting point of the thermoplastic material in the method of producing through the (ii) kneading step and (iii) extrusion step. [2] The method for producing a pesticide granule according to [1], wherein the pesticide active ingredient is a substance having a water solubility of 60 ppm or more. [3] Agrochemical active ingredients are nitenpyram, imidacloprid, acetamiprid, 3- (2-chlorothiazol-5-ylmethyl) -5-methyl-1,3,5-oxadiazinane-4-ylidene-N
-(Nitro) amine (generic name thiamethoxam), (E) -1-
(2-chloro-1,3-thiazol-5-ylmethyl) -3-methyl-2-
Nitroguanidine (generic name clothianidin), N- [3- (6-
From (chloropyridin-3-ylmethyl) thiazolidin-2-ylidene] cyanamide (generic name thiacloprid), (RS) -1-methyl-2-nitro-3-[(3-tetrahydrofuryl) methyl] guanidine (generic name dinotefuran) The method for producing an agricultural chemical granule according to [2], which is one or more compounds selected. [4] The method for producing an agricultural chemical granule according to any one of [1] to [3], wherein the thermoplastic material is a hydrophobic substance. [5] The method for producing an agricultural chemical granule according to [4], wherein the hydrophobic substance is montanic acid ester wax. [6] In extrusion granulation of an agricultural chemical composition comprising an agricultural chemical active ingredient, one kind of thermoplastic material, and an inorganic diluent carrier, the extruder used is a screw type extruder [1] ] The manufacturing method of the agricultural chemical granule as described in any one of [5].
【0011】[0011]
【発明の実施の形態】本発明に用いられる農薬活性成分
は特に限定されないが、水溶解度は60ppm以上のも
のが好ましい。60ppm以下の場合は、土壌に施用し
た場合、降雨量が多くても農薬活性成分が土中であまり
移動しないため、放出を制御する必要がないためであ
る。本発明に使用できる農薬活性成分として、次に示す
ものが挙げられる。BEST MODE FOR CARRYING OUT THE INVENTION The agrochemical active ingredient used in the present invention is not particularly limited, but it is preferable that the water solubility is 60 ppm or more. This is because when the amount is 60 ppm or less, when applied to the soil, the pesticide active ingredient does not move much in the soil even if the amount of rainfall is large, and it is not necessary to control the release. Examples of the agricultural chemical active ingredient that can be used in the present invention include the following.
【0012】除草剤では、モリネート、プロパニル、ア
ラクロール、メトラクロール、ベンスルフロンメチル、
イマゾスルフロン、シメトリン、シアナジン、ベンフレ
セートなどが挙げられる。Herbicides include molinate, propanil, alachlor, metolachlor, bensulfuron-methyl,
Imazosulfuron, cimetrin, cyanazine, benfresate and the like can be mentioned.
【0013】殺虫剤では、MPP、アセフェート、バミ
ドチオン、DMTP、ピラクロホス、ジメチルビンホ
ス、CVP、BPMC、エチオフェンカルブ、シクロプ
ロトリン、トラロメトリン、カルタップ、チオシクラ
ム、イミダクロプリド、ホスチアゼート、アセタミプリ
ド、NAC、ピメトロジン、ニテンピラム、3-(2-クロ
ロチアゾール-5-イルメチル)-5-メチル-1,3,5-オキサジ
アジナン-4-イリデン-N-(ニトロ)アミン(一般名チア
メトキサム)、(E)-1-(2-クロロ-1,3-チアゾール-5-イ
ルメチル)-3-メチル-2-ニトログアニジン(一般名クロ
チアニジン)、及びN-[3-(6-クロロピリジン-3-イルメ
チル)チアゾリジン-2-イリデン]シアナミド(一般名チ
アクロプリド)、または(RS)-1-メチル-2-ニトロ-3-[(3
-テトラヒドロフリル)メチル]グアニジン(一般名ジノ
テフラン)などが挙げられる。Examples of insecticides include MPP, acephate, bamidothion, DMTP, pyraclofos, dimethylvinphos, CVP, BPMC, ethiophencarb, cycloprotoline, tralomethrin, cartap, thiocyclam, imidacloprid, fosthiazate, acetamiprid, NAC, pymetrozine, nitenpyram3. -(2-chlorothiazol-5-ylmethyl) -5-methyl-1,3,5-oxadiazinane-4-ylidene-N- (nitro) amine (generic name thiamethoxam), (E) -1- (2-chloro -1,3-thiazol-5-ylmethyl) -3-methyl-2-nitroguanidine (generic name clothianidin), and N- [3- (6-chloropyridin-3-ylmethyl) thiazolidine-2-ylidene] cyanamide ( Generic name thiacloprid), or (RS) -1-methyl-2-nitro-3-[(3
-Tetrahydrofuryl) methyl] guanidine (generic name dinotefuran) and the like.
【0014】殺菌剤としては、ピロキロン、ブラストサ
イジンS、カスガマイシン、プロベナゾール、フェリム
ゾン、トリシクラゾール、メトミノストロビン、フラメ
トピル、バリダマイシンなどが挙げられる。Examples of the fungicides include pyroquilon, blasticidin S, kasugamycin, probenazole, ferrimzone, tricyclazole, metaminostrobin, flametopyr, validamycin and the like.
【0015】農薬活性成分は通常、1種に限定されるこ
とはなく、これらの中の同種、あるいは異種を組み合せ
て使用してもよい。本発明では農薬活性成分は農薬組成
物に対して0.01〜50重量%、好ましくは0.01
〜20重量%となるように使用する。The pesticidal active ingredient is not usually limited to one type, and the same type or different types among these may be used in combination. In the present invention, the agrochemical active ingredient is 0.01 to 50% by weight, preferably 0.01 to the agrochemical composition.
It is used so as to be about 20% by weight.
【0016】本発明では1種類の熱可塑性材料を使用す
る。熱可塑性材料は取り扱い易さの点から、融点が50
℃〜120℃であるものが好ましく、融点が50℃〜1
00℃のものが更に好ましい。熱可塑性材料は親水性ま
たは疎水性に区別なく使用することができるが、比較的
水溶解度の高い農薬活性成分の徐放化を達成するために
は疎水性のものが好適である。熱可塑性材料の使用量
は、本発明の農薬粒剤全重量に対して通常5重量%以
上、好ましくは10重量%以上であり、添加される農薬
活性成分の量、希釈担体の物性によって決めることがで
きる。経済的な面から熱可塑性材料の使用量の上限は3
0重量%である。The present invention uses one type of thermoplastic material. Thermoplastic materials have a melting point of 50 from the viewpoint of easy handling.
C. to 120.degree. C. is preferable, and melting point is 50.degree. C. to 1
It is more preferably at 00 ° C. The thermoplastic material can be used regardless of whether it is hydrophilic or hydrophobic, but a hydrophobic material is suitable for achieving sustained release of the agricultural chemical active ingredient having a relatively high water solubility. The amount of the thermoplastic material used is usually 5% by weight or more, preferably 10% by weight or more, based on the total weight of the pesticide granules of the present invention, and is determined depending on the amount of the pesticide active ingredient added and the physical properties of the diluent carrier. You can From the economical aspect, the upper limit of the amount of thermoplastic material used is 3
It is 0% by weight.
【0017】本発明で使用する熱可塑性材料を例示する
と、疎水性熱可塑性材料としてはキャンデリラワック
ス、カルナウバワックス、シュガーケンワックス、ライ
スワックス等の植物系ワックス、モンタン酸エステルワ
ックス、オゾケライト、セレシン等の鉱物系ワックス、
パラフィンワックス、マイクロクリスタリンワックス、
ペトロラタム等の石油系ワックス、フィッシャートロプ
シュワックス等の合成炭化水素、パラフィンワックス誘
導体、マイクロクリスタリンワックス誘導体等の変性ワ
ックス、ステアリン酸、ベヘニン酸などの脂肪酸、硬化
ヒマシ油、硬化ヒマシ油誘導体の水素化ワックス、ステ
アリルアルコールなどの高級アルコール、ステアリン酸
ステアリルなどの脂肪酸と高級アルコールとの脂肪酸エ
ステル、12−ヒドロキシステアリン酸、ステアリン酸
アミド、無水フタル酸イミド、塩素化炭化水素等の脂肪
酸、酸アミド、エステル、ケトン等が挙げられる。ま
た、親水性熱可塑性材料としては、ポリエチレングリコ
ール20000、ポリオキシエチレンポリオキシプロピ
レングリコール、ポリオキシエチレン、などのほか、エ
チレングリコールジステアレートやソルビタンジステア
レート、ショ糖脂肪酸エステルなどの界面活性剤も挙げ
られる。これらのうち、モンタン酸エステルワックスが
農薬活性成分の徐放化に好適である。Illustrative of the thermoplastic material used in the present invention, the hydrophobic thermoplastic material includes plant waxes such as candelilla wax, carnauba wax, sugarken wax, rice wax, montanic acid ester wax, ozokerite and ceresin. Mineral wax such as
Paraffin wax, microcrystalline wax,
Petroleum wax such as petrolatum, synthetic hydrocarbon such as Fischer-Tropsch wax, paraffin wax derivative, modified wax such as microcrystalline wax derivative, fatty acid such as stearic acid and behenic acid, hydrogenated castor oil, hydrogenated wax of hydrogenated castor oil derivative , Higher alcohols such as stearyl alcohol, fatty acid esters of fatty acids and higher alcohols such as stearyl stearate, 12-hydroxystearic acid, stearic acid amide, phthalic anhydride, fatty acids such as chlorinated hydrocarbons, acid amides, esters, Examples include ketones. Examples of hydrophilic thermoplastic materials include polyethylene glycol 20000, polyoxyethylene polyoxypropylene glycol, polyoxyethylene, and the like, and surfactants such as ethylene glycol distearate, sorbitan distearate, and sucrose fatty acid ester. Can also be mentioned. Among these, montanic acid ester wax is suitable for sustained release of the agricultural chemical active ingredient.
【0018】本発明で使用する無機系希釈担体は、特に
限定されるものではなく、例えば、クレー、珪石、タル
ク、ベントナイト、炭酸カルシウム、軽石、ケイソウ
土、バーミキュライト、パーライト、アタパルジャイト
および非晶質二酸化珪素、通称ホワイトカーボンなどが
挙げられる。通常、農薬粉剤や粒剤に利用される、いわ
ゆる増量剤や担体が1種または2種以上を併用すること
ができる。The inorganic diluent carrier used in the present invention is not particularly limited, and examples thereof include clay, silica stone, talc, bentonite, calcium carbonate, pumice stone, diatomaceous earth, vermiculite, perlite, attapulgite and amorphous dioxide. Silicon, commonly known as white carbon and the like can be mentioned. Usually, one kind or two or more kinds of so-called bulking agents and carriers, which are generally used for pesticide powders and granules, can be used in combination.
【0019】本発明の農薬粒剤は、本発明の目的と効果
を損なわない範囲で、界面活性剤、水溶性高分子を適
宜、含有させることができる。これらは農薬粒剤中に含
まれる農薬活性成分の徐放化速度を微調整するためや、
止水効果による農薬活性成分の効果安定化のために使用
される。The pesticide granules of the present invention can appropriately contain a surfactant and a water-soluble polymer within a range that does not impair the objects and effects of the present invention. These are for fine-tuning the sustained release rate of the pesticide active ingredient contained in the pesticide granules,
It is used for stabilizing the effect of pesticide active ingredients by the water-stopping effect.
【0020】また、本発明の農薬粒剤には、本発明の目
的と効果を損なわない範囲で、酸化防止剤や紫外線吸収
剤、帯電防止剤などの各種添加剤を用いて粒剤とするこ
ともできる。The pesticide granules of the present invention may be made into granules by using various additives such as antioxidants, ultraviolet absorbers, antistatic agents, etc. within the range that does not impair the objects and effects of the present invention. You can also
【0021】次に、本発明の農薬粒剤の製造方法につい
て説明する。本発明の農薬粒剤は(i)混合工程、(i
i)混練工程、(iii)押し出し工程を通して製造さ
れる。Next, the method for producing the agricultural chemical granules of the present invention will be described. The pesticide granules of the present invention include (i) a mixing step, (i)
It is manufactured through i) a kneading process and (iii) an extrusion process.
【0022】(i)混合工程:この工程では、農薬活性
成分、1種の熱可塑性材料、及び無機系希釈担体を含む
農薬組成物成分を加熱条件下に混合する。混合後の次工
程への移送など、混合物の取り扱いが容易であるために
は、混合後の状態は粉状や粉粒状が好ましい。従って、
混合工程は混合後の状態が粉状や粉粒状を維持できる温
度であれば、いずれの温度でもよく、場合によっては、
次工程の混練工程を本工程で行うこともできる。また、
この混合工程は次工程の混練工程で、混練と同時に行う
こともできる。(I) Mixing step: In this step, the agricultural chemical composition ingredients including the agricultural chemical active ingredient, one kind of thermoplastic material, and the inorganic diluent carrier are mixed under heating conditions. In order to easily handle the mixture such as transfer to the next step after mixing, the state after mixing is preferably powdery or granular. Therefore,
The mixing step may be any temperature as long as the state after mixing can maintain a powdery state or a powdery state, and in some cases,
The kneading step of the next step can also be performed in this step. Also,
This mixing step can be performed simultaneously with the kneading in the kneading step of the next step.
【0023】(ii)混練工程:混練工程では、混合工
程で得られた混合物を加熱条件下で混練して、熱可塑性
材料のマトリックスが形成される。本工程では熱可塑性
材料を部分的に、あるいは全体を溶融させて行うことが
必須である。そのため、混練時の温度は熱可塑性材料の
融点以上の温度条件で行うことが必要である。本工程で
使用される混練装置としては、圧縮、せん断、摩擦など
の外力が効率よく材料に加わる固定容器水平単軸型また
は固定容器水平複軸型のもの、具体的には、バンバリー
ミキサー、スクリュー式押し出し機などが好適である。
中でもスクリュー式押し出し機、特にニ軸型スクリュー
式押し出し機等の多軸型スクリュー式押し出し機は好適
である。混練操作にスクリュー式押し出し機を使用する
場合、混練工程と次工程の押し出し工程を同一機械で同
時に行うことができる。この場合、押し出し機の排出口
から混練物が排出されるが、排出口の開口部に所定の孔
径を有するダイスを設置して押し出すことで、農薬成型
物が得られる。(Ii) Kneading step: In the kneading step, the mixture obtained in the mixing step is kneaded under heating conditions to form a matrix of thermoplastic material. In this step, it is essential to melt the thermoplastic material partially or entirely. Therefore, it is necessary to carry out the kneading at a temperature not lower than the melting point of the thermoplastic material. As the kneading device used in this step, a fixed container horizontal single-axis type or a fixed container horizontal multi-axis type in which external forces such as compression, shear, and friction are efficiently applied to the material, specifically, a Banbury mixer, a screw A type extruder or the like is suitable.
Among them, a screw type extruder, particularly a multi-screw type extruder such as a double screw type extruder is suitable. When a screw type extruder is used for the kneading operation, the kneading step and the subsequent extrusion step can be simultaneously performed on the same machine. In this case, the kneaded product is discharged from the discharge port of the extruder, and a pesticide molded product can be obtained by installing and extruding a die having a predetermined hole diameter at the opening of the discharge port.
【0024】(iii)押し出し工程:混練工程で得ら
れた農薬組成物を押し出し機で押し出し、農薬成型物を
得る工程である。スクリュー式押し出し機を使用した場
合、前工程の混練工程も同時に行うことができる。本発
明では、該熱可塑性材料の凝固点以上、融点未満の温度
条件で、押し出し造粒を行う。熱可塑性材料の融点以上
の温度で押し出した場合、成型物中の熱可塑性材料が粘
着性を示し、成型物どおしの付着・融着を起こし、つい
にはアメ状やダンゴ状となり、農薬粒剤の生産性は著し
く悪い。また、熱可塑性材料の凝固点未満の温度で押し
出した場合、得られた成型物は円柱状に成型されず、且
つ、粉状物の多い規格外品が多く、生産性が著しく悪
い。かくして、熱可塑性材料の凝固点以上、融点未満の
温度条件下で農薬組成物を押し出すことにより、きれい
な円柱状の農薬成型物が得られ、且つ、生産性も著しく
向上する。(Iii) Extrusion step: a step of extruding the pesticide composition obtained in the kneading step with an extruder to obtain a pesticide molding. When a screw type extruder is used, the kneading step of the previous step can be performed at the same time. In the present invention, extrusion granulation is carried out under a temperature condition that is equal to or higher than the freezing point of the thermoplastic material and lower than the melting point. If extruded at a temperature above the melting point of the thermoplastic material, the thermoplastic material in the molded product will show tackiness, causing adhesion and fusion of the molded product, eventually becoming a candy-like or dango-like, pesticide grain. The productivity of the agent is extremely poor. Further, when extruded at a temperature lower than the freezing point of the thermoplastic material, the obtained molded product is not molded into a columnar shape, and there are many nonstandard products with many powdery substances, resulting in extremely poor productivity. Thus, by extruding the agrochemical composition under a temperature condition of not less than the freezing point of the thermoplastic material and less than its melting point, a clean columnar pesticide molded article can be obtained and the productivity is remarkably improved.
【0025】押し出された農薬成型物は、その後の冷却
工程、整粒工程を経て農薬粒剤が得られる。The extruded pesticide molding product is subjected to the subsequent cooling step and sizing step to obtain pesticide granules.
【0026】かかる本発明の製造方法により、高い生産
性で農薬粒剤を得ることができる。また、得られた農薬
粒剤は農薬活性成分の均質な徐放性をも保持している。The pesticide granules can be obtained with high productivity by the production method of the present invention. Further, the obtained agricultural chemical granules also maintain a uniform sustained release property of the agricultural chemical active ingredient.
【0027】[0027]
【実施例】次に実施例により本発明をさらに詳細に説明
するが、実施例に記す農薬粒剤の製剤処方はこれらに限
定されるものではない。尚、ここで示す配合割合はすべ
て重量%とする。EXAMPLES The present invention will be described in more detail with reference to examples, but the formulation of the agricultural chemical granules described in the examples is not limited thereto. The mixing ratios shown here are all weight%.
【0028】実施例1 農薬活性成分としてジノテフラ
ンを2重量%、熱可塑性材料としてモンタン酸エステル
ワックス(BASF社製、商品名Luwax−E、融点;7
5〜85℃、凝固点;70〜75℃)20重量%、無機
系希釈担体としてホワイトカーボン5重量%、タルク1
0重量%、炭酸カルシウム63重量%をヘンシェルミキ
サーに投入して混合し、76℃で粉体の状態で排出し
た。この粉体を不二パウダル製スクリュー式押し出し造
粒機(EXR―130)に投入して、78℃で混練を行
った。73℃で目開き0.8mmのダイスを経て押し出
し造粒を行い、農薬成型物を得た。これを解砕機で粉砕
して、農薬粒剤を得た。(製品収率、94%)Example 1 2% by weight of dinotefuran as an agrochemical active ingredient and montanic acid ester wax as a thermoplastic material (manufactured by BASF, trade name Luwax-E, melting point; 7
5 to 85 ° C., freezing point: 70 to 75 ° C.) 20% by weight, white carbon 5% by weight as an inorganic diluent carrier, talc 1
0% by weight and 63% by weight of calcium carbonate were put into a Henschel mixer, mixed, and discharged in a powder state at 76 ° C. This powder was introduced into a Fuji Paudal screw-type extrusion granulator (EXR-130) and kneaded at 78 ° C. Extrusion and granulation were carried out at 73 ° C through a die having an opening of 0.8 mm to obtain a pesticide molded article. This was crushed with a crusher to obtain a pesticide granule. (Product yield, 94%)
【0029】実施例2 農薬活性成分としてジノテフ
ランを2重量%、熱可塑性材料としてモンタン酸エステ
ルワックス(BASF社製、商品名Luwax−E、融点;
75〜85℃、凝固点;70〜75℃)20重量%、無
機系希釈担体としてホワイトカーボン5重量%、タルク
10重量%、炭酸カルシウム63重量%をヘンシェルミ
キサーに投入して混合し、78℃で、粉体の状態で排出
した。この粉体を不二パウダル製スクリュー式押し出し
造粒機(EXR―130)に投入して、78℃で混練を
行った。73℃で目開き0.8mmのダイスを経て押し
出し造粒を行い、農薬成型物を得た。これを解砕機で粉
砕して、農薬粒剤を得た。(製品収率、93%)Example 2 2% by weight of dinotefuran as an agrochemical active ingredient and montanic acid ester wax as a thermoplastic material (manufactured by BASF, trade name Luwax-E, melting point;
75-85 ° C., freezing point; 70-75 ° C.) 20% by weight, 5% by weight of white carbon as an inorganic diluent, 10% by weight of talc, 63% by weight of calcium carbonate are put into a Henschel mixer and mixed at 78 ° C. , Was discharged in the form of powder. This powder was introduced into a Fuji Paudal screw-type extrusion granulator (EXR-130) and kneaded at 78 ° C. Extrusion and granulation were carried out at 73 ° C through a die having an opening of 0.8 mm to obtain a pesticide molded article. This was crushed with a crusher to obtain a pesticide granule. (Product yield, 93%)
【0030】実施例3 農薬活性成分としてジノテフラ
ンを2重量%、熱可塑性材料としてカルナウバワックス
(東亜化成社製、商品名Refined Granul
arCarnauba、融点;83℃、凝固点73〜74
℃)20重量%、無機系希釈担体としてホワイトカーボ
ン5重量%、タルク10重量%、炭酸カルシウム63重
量%をヘンシェルミキサーに投入して混合し、80℃で
粉粒の状態で排出した。この粉体を不二パウダル製スク
リュー式押し出し造粒機(EXR―130)に投入し
て、85℃で混練を行った。78℃で目開き0.8mm
のダイスを経て押し出し造粒を行い、農薬成型物を得
た。これを解砕機で粉砕して、農薬粒剤を得た。(製品
収率、92%)Example 3 2% by weight of dinotefuran as an agrochemical active ingredient and carnauba wax as a thermoplastic material (trade name: Refined Granul, manufactured by Toa Kasei Co., Ltd.)
arCarnauba, melting point; 83 ° C., freezing point 73-74
20% by weight, 5% by weight of white carbon as an inorganic diluent, 10% by weight of talc and 63% by weight of calcium carbonate were put into a Henschel mixer and mixed, and discharged at 80 ° C. in the form of powder particles. This powder was charged into a Fuji Paudal screw-type extrusion granulator (EXR-130) and kneaded at 85 ° C. 0.8 mm opening at 78 ° C
The mixture was extruded and granulated through the above die to obtain a pesticide molded product. This was crushed with a crusher to obtain a pesticide granule. (Product yield, 92%)
【0031】比較例1 押し出し造粒時の温度を78℃
で行った以外は実施例1と同様に行った。その結果、塊
状の農薬成型物を得た。これを解砕機で粉砕して、農薬
粒剤を得た。(製品収率、38%)Comparative Example 1 The temperature during extrusion granulation was 78 ° C.
The same procedure as in Example 1 was carried out except that the above procedure was performed. As a result, a block-shaped pesticide molded product was obtained. This was crushed with a crusher to obtain a pesticide granule. (Product yield, 38%)
【0032】比較例2 押し出し造粒時の温度を68℃
で行った以外は実施例1と同様に行った。その結果、粉
体の多い農薬成型物を得た。これを解砕機で粉砕して、
農薬粒剤を得た。(製品収率、41%)Comparative Example 2 The temperature during extrusion granulation was 68 ° C.
The same procedure as in Example 1 was carried out except that the above procedure was performed. As a result, a pesticide molded product containing a large amount of powder was obtained. Crush this with a crusher,
A pesticide granule was obtained. (Product yield, 41%)
【0033】試験例1(農薬粒剤の溶出試験)
実施例1〜3で得られた農薬粒剤を標準3度硬水25m
lを入れた50mlの密栓付きサンプル管に、農薬活性
成分として920ppm相当の量を投入して水中に沈
め、25℃下所定時間静置後、全量を濾別し、濾液中の
農薬活性成分量をHPLCにて測定した。測定より下記
式に基づき溶出率を計算した。溶出率=(濾液中の農薬
活性成分量/粒剤中の農薬活性成分量)×100結果を
表−1に示した。この結果から、均質な徐放性を維持し
ていた。Test Example 1 (Dissolution test of pesticide granules) The pesticide granules obtained in Examples 1 to 3 were treated with standard 3 degree hard water of 25 m.
Into a 50 ml sample tube with a sealed stopper containing 1 liter, an amount corresponding to 920 ppm as an agrochemical active ingredient was put and submerged in water, and after standing at 25 ° C. for a predetermined time, the whole amount was filtered off to obtain the amount of the agrochemical active ingredient in the filtrate. Was measured by HPLC. From the measurement, the dissolution rate was calculated based on the following formula. Dissolution rate = (amount of pesticide active ingredient in filtrate / amount of pesticide active ingredient in granule) × 100 The results are shown in Table 1. From this result, a uniform sustained release property was maintained.
【0034】[0034]
【表1】 [Table 1]
【0035】[0035]
【発明の効果】本発明の製造方法により、製造工程を通
して得られた農薬粒剤は農薬活性成分の徐放化を保持
し、且つ、高い製品収率で農薬粒剤を得ることができ
る。そのため、製造コストを低く抑えることができるメ
リットもある。Industrial Applicability According to the production method of the present invention, the agricultural chemical granules obtained through the manufacturing process can maintain the sustained release of the agricultural chemical active ingredient and can obtain the agricultural chemical granules with a high product yield. Therefore, there is an advantage that the manufacturing cost can be kept low.
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Claims (6)
及び無機系希釈担体からなる農薬粒剤を、(i)混合工
程、(ii)混練工程、(iii)押し出し工程を通し
て製造する方法において、該熱可塑性材料の凝固点以
上、融点未満の温度で、押し出し造粒を行うことを特徴
とする農薬粒剤の製造方法。1. An agrochemical active ingredient, one kind of thermoplastic material,
And a method for producing an agricultural chemical granule comprising an inorganic diluent carrier through (i) a mixing step, (ii) a kneading step, and (iii) an extrusion step, at a temperature not lower than the freezing point and lower than the melting point of the thermoplastic material A method for producing a pesticide granule, which comprises granulating.
の物質であることを特徴とする請求項1記載の農薬粒剤
の製造方法。2. The method for producing a pesticide granule according to claim 1, wherein the pesticide active ingredient is a substance having a water solubility of 60 ppm or more.
プリド、アセタミプリド、3-(2-クロロチアゾール-5-イ
ルメチル)-5-メチル-1,3,5-オキサジアジナン-4-イリデ
ン-N-(ニトロ)アミン(一般名チアメトキサム)、(E)
-1-(2-クロロ-1,3-チアゾール-5-イルメチル)-3-メチル
-2-ニトログアニジン(一般名クロチアニジン)、N-[3-
(6-クロロピリジン-3-イルメチル)チアゾリジン-2-イ
リデン]シアナミド(一般名チアクロプリド)、(RS)-1-
メチル-2-ニトロ-3-[(3-テトラヒドロフリル)メチル]
グアニジン(一般名ジノテフラン)から選ばれる一種以
上の化合物であることを特徴とする請求項2記載の農薬
粒剤の製造方法。3. The pesticide active ingredient is nitenpyram, imidacloprid, acetamiprid, 3- (2-chlorothiazol-5-ylmethyl) -5-methyl-1,3,5-oxadiazinane-4-ylidene-N- (nitro) amine. (Generic name thiamethoxam), (E)
-1- (2-chloro-1,3-thiazol-5-ylmethyl) -3-methyl
-2-Nitroguanidine (generic name clothianidin), N- [3-
(6-chloropyridin-3-ylmethyl) thiazolidin-2-ylidene] cyanamide (generic name thiacloprid), (RS) -1-
Methyl-2-nitro-3-[(3-tetrahydrofuryl) methyl]
The method for producing a pesticide granule according to claim 2, which is one or more compounds selected from guanidine (generic name dinotefuran).
特徴とする請求項1〜3記載の何れか一項に記載の農薬
粒剤の製造方法。4. The method for producing an agrochemical granule according to claim 1, wherein the thermoplastic material is a hydrophobic substance.
スであることを特徴とする請求項4記載の農薬粒剤の製
造方法。5. The method for producing an agricultural chemical granule according to claim 4, wherein the hydrophobic substance is montanic acid ester wax.
及び無機系希釈担体からなる農薬組成物を押し出し造粒
するにおいて、使用する押し出し機がスクリュー式の押
し出し機であることを特徴とする請求項1〜5の何れか
一項に記載の農薬粒剤の製造方法。6. A pesticide active ingredient, one kind of thermoplastic material,
In the case of extruding and granulating an agrochemical composition consisting of an inorganic diluent carrier, the extruder used is a screw type extruder, and the agrochemical granules according to any one of claims 1 to 5. Manufacturing method.
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---|---|---|---|
JP2002055187A JP4159789B2 (en) | 2002-03-01 | 2002-03-01 | Improved process for producing pesticide granules |
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Publication Number | Publication Date |
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JP2003252702A true JP2003252702A (en) | 2003-09-10 |
JP4159789B2 JP4159789B2 (en) | 2008-10-01 |
Family
ID=28666084
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