JP5016773B2 - Coated pesticide composition - Google Patents

Description

(7) 次に、660gのビオン／アクタラ コア GR(3.3+3.3)をオニオンパン（ハタ鉄工所社製）に装填し、該パンをしかる後に約20rpmの速度で絶えず回転させた。
【００５０】
(8) 次いで、5gのモレスコ ホワイト P−70を添加した。
【００５１】
(9) 続いて82gのSH−502を添加し、続いて5〜15分間25℃で乾燥した空気を0.6m³／分の空気吹込みで乾燥する。
【００５２】
(10) 工程(9)を8回反復した。
【００５３】
(11) 次いで5gのタルカムTAを添加した。
【００５４】
(12) 最後に、かくして得られる8回被覆したビオン／アクタラ コア GR(3.3+3.3)に、入口の空気温度60℃且つ出口の空気温度50℃以上の条件下に後乾燥を施した。
【００５５】
かくして次の組成を有する対応の徐放性の被覆した固体農薬の混合物を製造した；

(13) 前記で製造した速放性の被覆した農薬の混合物と徐放性の被覆した農薬の混合物とを１：１の重量比で混合し、これによって2種の有効成分を有する本発明の組成物を得た。
【００５６】
実施例 2 （製造例）
速放性の被覆した農薬の混合物と徐放性の被覆した農薬の混合物とを６：４の重量比で混合する以外は実施例1と同じ要領で組成物を製造した。
【００５７】
実施例 3 （製造例）
速放性の被覆した農薬の混合物と徐放性の被覆した農薬の混合物とを４：６の重量比で混合する以外は実施例1と同じ要領で組成物を製造した。
【００５８】
実施例 4 （製造例）
(1) 890gのピロキロン／アクタラ コア GR(2.4+2.4)をオニオンパン（ハタ鉄工所社製）に装填し、該パンをしかる後に約20rpmの速度で絶えず回転させる。
【００５９】
(2) 次いで、5gのモレスコ ホワイト P−70を添加した。
【００６０】
(3) 続いて、67gのSH−502を添加し、続いて5〜15分間25℃で乾燥した空気を0.6m³／分の空気吹込みで乾燥させた。
【００６１】
(4) 工程(3)を3回反復した。
【００６２】
(5) 次いで5gのタルカムTAを添加した。
【００６３】
(6) 最後に、かくして得られる三重被覆したピロキロン／アクタラ コア GR(2.4+2.4)に、入口の空気温度60℃且つ出口の空気温度50℃以上の条件下で後乾燥を施した。
【００６４】
かくして、次の組成を有する速放性の被覆した農薬の混合物を製造した；

(7) 次に、640gのピロキロン／アクタラ コア GR(36.5+3.3)をオニオンパンに装填し、該パンをしかる後に約20rpmの速度で絶えず回転させた。
【００６５】
(8) 次いで、5gのモレスコ ホワイトを添加した。
【００６６】
(9) 続いて、140gのSH−502を添加し、続いて5〜15分間25℃で乾燥した空気を0.6m³／分の空気吹込みで乾燥させた。
【００６７】
(10) 次いで、70gのSH−502を添加し、続いて5〜15分間25℃の乾燥した空気を0.6m³／分の空気吹込みで乾燥させた。
【００６８】
(11) 工程(10)を4回反復した。
【００６９】
(12) 次いで、2.5gのタルクを添加した。
【００７０】
(13) かくして得られる5回被覆したピロキロン／アクタラ コア GR (36.5+3.3)に、入口の空気温度60℃且つ出口の空気温度50℃以上の条件下に後乾燥を施した。
【００７１】
(14) 前記の5回被覆したピロキロン／アクタラ コア GR(36.5+3.3)を、約20rpmの速度で絶えず回転しているオニオンパンに再び装填した。
【００７２】
(15) 続いて、70gのSH−502を添加し、続いて5〜15分間25℃で乾燥した空気を0.6m²／分の空気吹込みで乾燥させた。
【００７３】
(16) 工程(15)を4回反復した。
【００７４】
(17) 次いで2.5gのタルクを添加した。
【００７５】
(18) かくして得られる9回被覆したピロキロン／アクタラ コア GR(36.5+3.3)に、入口の空気温度60℃且つ出口の空気温度50℃以上の条件下で後乾燥を施した。
【００７６】
かくして次の組成を有する対応の徐放性の被覆した農薬の混合物を製造した；

(18) 前記で製造した速放性の被覆した農薬の混合物と徐放性の被覆した農薬の混合物とを１：１の重量比で混合し、これによって2種の有効成分を有する本発明の組成物を得た。
【００７７】
実施例 5 （製造例）
(1) 890gのピロキロン／アクタラ コア GR(4.7+2.4)をオニオンパン（ハタ鉄工所社製）に装填し、該パンをその後約20rpmの速度で絶えず回転させた。
【００７８】
(2) 次いで、5gのモレスコ ホワイト P−70を添加した。
【００７９】
(3) 続いて、67gのSH−502を添加し、続いて5〜15分間25℃の乾燥した空気を0.6m³／分の空気吹込みで乾燥させた。
【００８０】
(4) 工程(3)を3回反復した。
【００８１】
(5) 次いで5gのタルカムTAを添加した。
【００８２】
(6) 最後に、かくして得られる三重被覆したピロキロン／アクタラ コア GR(4.7+2.4)に、入口の空気温度60℃且つ出口の空気温度50℃以上の条件下で後乾燥を施した。
【００８３】
かくして次の組成を有する速放性の被覆した農薬の混合物を製造した；

(7) 640gのピロキロン／アクタラ コア GR(32.2+3.3)をオニオンパンに装填し、該パンをしかる後に約20rpmの速度で回転させた。
【００８４】
(8) 次いで、5gのモレスコ ホワイトを添加した。
【００８５】
(9) 続いて、140gのSH−502を添加し、続いて5〜15分間25℃の乾燥した空気を0.6m³／分の空気吹込みで乾燥させた。
【００８６】
(10) 次いで70gのSH−502を添加し、続いて5〜15分間25℃の乾燥した空気を0.6m³／分の空気吹込みで乾燥させた。
【００８７】
(11) 工程(10)を4回反復した。
【００８８】
(12) 次いで、2.5gのタルクを添加した。
【００８９】
(13) かくして得られる5回被覆したピロキロン／アクタラ コア GR (32.2+3.3)に、入口の空気温度60℃且つ出口の空気温度50℃以上の条件下に後乾燥を施した。
【００９０】
(14) 前記の乾燥した、5回被覆したピロキロン／アクタラ コア GR(32.2+3.3)を、約20rpmの速度で絶えず回転するオニオンパンに再び装填した。
【００９１】
(15) 続いて、70gのSH−502を添加し、続いて5〜15分間25℃の乾燥した空気を0.6m³／分の空気吹込みで乾燥させた。
【００９２】
(16) 工程(15)を4回反復した。
【００９３】
(17) 次いで2.5gのタルクを添加した。
【００９４】
(18) かくして得られた9回被覆したピロキロン／アクタラ コア GR(32.2+3.3)に、入口の空気温度60℃且つ出口の空気温度50℃以上の条件下で後乾燥を施した。
【００９５】
かくして次の組成を有する徐放性の被覆した農薬の混合物を製造した；

(18) 前記で製造した速放性の被覆した農薬の混合物と徐放性の被覆した農薬の混合物とを１：１の重量比で混合し、これによって2種の有効成分を有する本発明の組成物を得た。
【００９６】
実施例 6 （製造例）
(1) 890gのピロキロン／アクタラ コア GR(9.4+2.4)をオニオンパン（ハタ鉄工所社製）に装填し、該パンをしかる後に約20rpmの速度で絶えず回転させた。
【００９７】
(2) 次いで、5gのモレスコ ホワイト P−70を添加した。
【００９８】
(3) 続いて、67gのSH−502を添加し、続いて5〜15分間25℃で乾燥した空気を0.6m³／分の空気吹込みで乾燥させた。
【００９９】
(4) 工程(3)を3回反復した。
【０１００】
(5) 次いで5gのタルカムTAを添加した。
【０１０１】
(6) 最後に、かくして得られる三重被覆したピロキロン／アクタラ コア GR(9.4+2.4)に、入口の空気温度60℃且つ出口の空気温度50℃以上の条件下に後乾燥を施した。
【０１０２】
かくして次の組成を有する速放性の被覆した農薬の混合物を製造した；

(7) 640gのピロキロン／アクタラ コア GR(26.3+3.3)をオニオンパンに装填し、該パンをその後約20rpmの速度で一定回転させた。
【０１０３】
(8) 次いで、5gのモレスコ ホワイトを添加した。
【０１０４】
(9) 続いて、140gのSH−502を添加し、続いて5〜15分間25℃の乾燥した空気を0.6m³／分の空気吹込みで乾燥させた。
【０１０５】
(10) 次いで70gのSH−502を添加し、続いて5〜15分間25℃の乾燥した空気を0.6m³／分の空気吹込みで乾燥させた。
【０１０６】
(11) 工程(10)を4回反復した。
【０１０７】
(12) 次いで、2.5gのタルクを添加した。
【０１０８】
(13) かくして得られる5回被覆したピロキロン／アクタラ コア GR (26.3+3.3)に、入口の空気温度60℃且つ出口の空気温度50℃以上の条件下で後乾燥を施した。
【０１０９】
(14) 前記の乾燥した、5回被覆したピロキロン／アクタラ コア GR(26.3+3.3)GRを、約20rpmの速度で一定回転するオニオンパンに再び装填した。
【０１１０】
(15) 続いて、70gのSH−502を添加し、続いて5〜15分間25℃の乾燥した空気を0.6m³／分の空気吹込みで乾燥させた。
【０１１１】
(16) 工程(15)を4回反復した。
【０１１２】
(17) 次いで2.5gのタルクを添加した。
【０１１３】
(18) かくして得られる9回被覆したピロキロン／アクタラ コア GR (26.3+3.3)に、入口の空気温度60℃且つ出口の空気温度50℃以上の条件下に、後乾燥を施した。
【０１１４】
かくして、次の組成を有する徐放性の被覆した農薬の混合物を製造した；

(19) 前記で製造した速放性の被覆した農薬の混合物と徐放性の被覆した農薬の混合物とを１：１の重量比で混合し、これによって2種の有効成分を有する本発明の組成物を得た。
【０１１５】
実施例 7 （製造例）
(1) 890gのピロキロン／アクタラ コア GR(3.8+3.8)をオニオンパン（ハタ鉄工所社製）に装填し、該パンをその後に約20rpmの速度で一定回転させる。
【０１１６】
(2) 次いで、20gのモレスコ ホワイト P−70を添加した。
【０１１７】
(3) 続いて、107gのSH−502を添加し、続いて5〜15分間25℃の乾燥した空気を0.6m³／分の空気吹込みで乾燥させた。
【０１１８】
(4) 工程(3)を2回反復した。
【０１１９】
(5) 次いで5gのタルカムTAを添加した。
【０１２０】
(6) 最後に、かくして得られる2回被覆したピロキロン／アクタラ コア GR(3.8+3.8)に、入口の空気温度60℃且つ出口の空気温度50℃以上の条件下に後乾燥を施した。
【０１２１】
かくして次の組成を有する速放性の被覆した農薬の混合物を製造した；

(7) 640gのピロキロン コア GR 63.1をオニオンパンに装填し、該パンをその後約20rpmの速度で一定回転させた。
【０１２２】
(8) 次いで、22gのモレスコ ホワイトを添加した。
【０１２３】
(9) 続いて、94gのSH−502を添加し、続いて5〜15分間25℃の乾燥した空気を0.6m³／分の空気吹込みで乾燥させた。
【０１２４】
(10) 工程(9)を4回反復した。
【０１２５】
(11) 次いで、2gのタルクを添加した。
【０１２６】
(12) かくして得られる4回被覆したピロキロン コア GR 63.1に、入口の空気温度60℃且つ出口の空気温度50℃以上の条件下に、後乾燥を施した。
【０１２７】
(13) 前記の乾燥した、4回被覆したピロキロン コア GR 63.1を約20rpmの速度で一定回転するオニオンパンに再び装填した。
【０１２８】
(14) 続いて、94gのSH−502を添加し、続いて5〜15分間25℃の乾燥した空気を0.6m³／分の空気吹込みで乾燥させた。
【０１２９】
(15) 工程(14)を3回反復した。
【０１３０】
(16) 次いで2gのタルクを添加した。
【０１３１】
(17) かくして得られる7回被覆したピロキロン コア GR 63.1に、入口の空気温度60℃且つ出口の空気温度50℃以上の条件下で後乾燥を施した。
【０１３２】
(18) 前記の乾燥した、7回被覆したピロキロン コア GR 63.1を約20rpmの速度で一定回転するオニオンパンに再び装填した。
【０１３３】
(19) 続いて、94gのSH−502を添加し、続いて5〜15分間25℃の乾燥した空気を0.6m³／分の空気吹込みで乾燥させた。
【０１３４】
(20) 工程(19)を3回反復した。
【０１３５】
(21) 次いで1gのタルクを添加した。
【０１３６】
(22) かくして得られる10回被覆したピロキロン コア GR 63.1に、入口の空気温度60℃且つ出口の空気温度50℃以上の条件下に後乾燥を施した。
【０１３７】
かくして、次の組成を有する徐放性の被覆した農薬を製造した；

(23) 640gのチアメトキサム コア GR 5.1をオニオンパンに装填し、該パンをその後約20rpmの速度で一定回転させた。
【０１３８】
(24) 次いで、20gのモレスコ ホワイトを添加した。
【０１３９】
(25) 続いて、73gのSH−502を添加し、続いて5〜15分間25℃の乾燥した空気を0.6m³／分の空気吹込みで乾燥させた。
【０１４０】
(26) 工程(25)を3回反復した。
【０１４１】
(27) 次いで2gのタルクを添加した。
【０１４２】
(28) 前記の乾燥した、3回被覆したチメトキサム コア GR 5.1を、約20rpmの速度で一定回転するオニオンパンに再び装填した。
【０１４３】
(29) 続いて、73gのSH−502を添加し、続いて5〜15分間25℃の乾燥した空気を0.6m³／分の空気吹込みで乾燥させた。
【０１４４】
(30) 工程(29)を3回反復した。
【０１４５】
(31) 次いで2gのタルクを添加した。
【０１４６】
(32) かくして得られる6回被覆したチメトキサム コア GR 5.1に、入口の空気温度60℃及び出口の空気温度50℃以上の条件下に後乾燥を施した。
【０１４７】
(33) 前記の乾燥した、6回被覆したチメトキサム コア GR 5.1を約20rpmの速度で一定回転するオニオンパンに再び装填した。
【０１４８】
(34) 続いて、73gのSH−502を添加し、続いて5〜15分間25℃の乾燥した空気を0.6m³／分の空気吹込みで乾燥させた。
【０１４９】
(35) 工程(34)を3回反復した。
【０１５０】
(36) 次いで1gのタルクを添加した。
【０１５１】
(37) かくして得られる、9回被覆したチメトキサム コア GR 5.1に、入口の空気温度60℃及び出口の空気温度50℃以上の条件下に後乾燥を施した。
【０１５２】
かくして次の組成を有する徐放性の被覆した農薬を製造した；

前記で製造した速放性の被覆した農薬の混合物と2種の徐放性の被覆した農薬のそれぞれ単独とを１：１：１の重量比で混合して、これによって2種の有効成分を有する本発明の組成物を得た。
【０１５３】
実施例 8 （放出試験）
3度のドイツ硬度を有する水1000mlを1000mlの栓付きフラスコに装入し、これに実施例1の工程(6)又は(12)で製造した農薬250mgあるいは実施例4の工程(6)又は(17)で製造した農薬250mgを添加した。前記水の温度を25+−2℃に保持した。若干の顆粒が水の表面に浮遊しているならば、これらをフラスコの底部に沈降させた。
【０１５４】
(2) 前記の試験系を製造してから3日後に、これから10mlのホールピペットを用いて10mlの液体をピペットで取出し、次いで栓付きの遠心管に移送した。液体をピペットで取出す時には、ホールピペットの先端を液体表面とフラスコの底部との間の中間点に定置させた。液体をピペットで取出した後に、3度のドイツ硬度を有する水10mlを試験系に添加した。若干の顆粒が遠心管に移送した液体中で浮遊するか又は凝集しているならば、これを遠心分離して顆粒を沈降させた。
【０１５５】
(3) 次いで遠心管に移送した液体にHPLC及び／又はGLC分析を施して液体中の農薬有効成分濃度を測定した。この測定は各々の有効成分について行なった。
【０１５６】
(4) 試験系を製造してから、1、3、7、14、21、28、36、42、50、56、63、71、77、80、101及び133日後に工程(2)〜(3)を反復した。
【０１５７】
結果を表1に示す。
【０１５８】
実施例 9 （放出試験）
実験は実施例8と同じ要領で行なうが、但し実施例1の工程(13)の組成物の250mgを、実施例1の工程(6)又は(12)で製造した農薬あるいは実施例4の工程(6)又は(17)で製造した農薬の代りに用いるものとし、放出試験は25℃及び15℃で行なうものとし、実施例7の工程(2)〜(3)は試験系を製造してから1、3、7、14、28、42、56、71、80及び101日後に反復するものとし、チアメトキサムの濃度のみを測定するものとする。
【０１５９】
結果を表2に示す。
【０１６０】
表1 放出試験の結果

表2 放出試験の結果

実施例8から得られた表1の結果から見られる通り、本発明は上昇温度条件下で1種又はそれ以上の有効成分の一定の放出を達成することは明らかである。例えば、実施例4の速放性農薬（10％の被覆層）は25℃で14日でピロキロンの放出を完了するが、然るに同じ実施例の徐放性農薬（35％の被覆層）は25℃で14日で25％のピロキロンを放出するに過ぎない。温度が14日で25℃よりも高い温度に上昇するならば、速放性の農薬は温度が前記温度に到達する前に14日よりも短かい期間内にピロキロンの放出を完了することが予期される。然しながら、速放性農薬がピロキロンの放出を完了する期間中に徐放性農薬からのピロキロンの放出は速放性農薬の放出と比較すると実際上無視しうる程小さいことが予期され、しかも徐放性農薬からのピロキロンの放出速度は速放性農薬からの放出の完了後に上昇した温度で増大することが予期される。それ故、本発明は上昇する温度条件下でさえ1種又はそれ以上の有効成分の一定の放出を達成することが明らかである。同じことは、アシベンゾラー−S−メチル及びチアメトキサムの放出挙動の結果からも予期され得る。
【０１６１】
実施例9は実施例1の組成物を用いて前記の予想を証明するために行なうものであり、該組成物は有効成分がアシベンゾラー−S−メチル及びチアメトキサムである速放性農薬と徐放性農薬とからなる。表2が示す様に、25℃でチアメトキサムの放出速度は15℃での放出速度よりも約2倍程大きい。然しながら、最初の2週間の間の放出速度は15℃及び25℃の両方での第3週乃至第4週の間の放出速度より約2倍程大きい。それ故、実施例1の組成物の施用後に最初の2週間は温度が15℃のままであり、次いで突然に25℃まで昇温するならば、放出速度は第1週については8％であり、第2週については7％であり、第3週については12％であり、第4週及び第5週については10％であり、第6週及び第7週については8.5％であり、第8週及び第9週については8％である。これらの結果は、本発明の組成物が、上昇する温度条件下で有効成分の放出を十分に加減し得ることを明らかに証明するものである。
【０１６２】
更には、表１のピロキロンからの結果が示す通り、本発明の組成物は、1種又はそれ以上の有効成分の放出速度が初期の段階では高いことが必要とされるがその後は低くしかも長期持続性であることが必要とされる用途にも適している。前記した如く、その優れた放出制御性に因り、本発明の組成物は、農夫の労働力の更なる低減が要求される現在及び将来の農園芸用に欠くことのできない農薬組成物である。[0001]
The present invention relates to a composition comprising a sustained or slow release coated pesticide and an immediate release coated pesticide (hereinafter simply referred to as an agrochemical).
[0002]
Coated solid pesticides are well known in the art and are commonly applied to control the release of their active ingredients as described, for example, in PCT application WO 99/01243. However, conventional coated pesticides do not exhibit satisfactory release characteristics after their application, especially if the temperature changes due to the temperature dependence of the release rate of the active ingredient.
[0003]
  Surprisingly according to the recently found process, the following ingredients:
  (1) A pesticidal active ingredient is formulated together with an inert carrier and a surfactant to form granules or powder, and the granules or powder is coated with an emulsifying thermoplastic polymer with water. Releasable coated solid pesticides and
  (2) The same active ingredient as that of the agrochemical (1) is formulated together with an inert carrier and a surfactant to form granules or powder, and the granules or powder is coated with an emulsifying thermoplastic polymer with water. A solid release pesticide with an immediate release
A pesticidal composition comprising a sustained release property and a rapid release property only by adjusting the content of the thermoplastic polymer, only by adjusting the content of the active ingredient, or the above. The agrochemical composition, which is adjusted by adjusting the content of the thermoplastic polymer and the content of the active ingredient, unexpectedly achieves the desired release characteristics under changing and particularly rising temperature conditions. The temperature is found to be at least 15 ° C. after application of the compositionFrom25 ℃InIt will rise.
[0004]
  The sustained-release coated pesticides (1) usually show long-term pest killing effects in water at high temperatures, whereas the fast-release coated pesticides (2) are lowWarmWith long-term pest killing effect in water. Therefore, by appropriately combining these two types of pesticides (1) and (2), which have the same pesticide-killing active ingredient, release of the active ingredient during periods of low temperature at the beginning and high at the end Can be held substantially constant. The composition of the present invention as described above achieves such controlled release even when applied only once in the initial stages of sowing / cultivation.
[0005]
Pesticide killing active ingredients to be used in the present invention include herbicides, fungicides and insecticides as well as plant growth regulators and inhibitors and plant activators. Examples of herbicides include pretilachlor, clomeprop, bifenox, pyrazoxifene, pyrazolinate, sinosulfurone, dimethylpiperate, bensulfuron-methyl, pyrazosulfuron-ethyl, naproanilide, bromobutide, mefenacet, imazosulfuron, dimron, bentazone, benzomethazone, benzomethatoe Turol, azimusulfuron, pyriminobac-methyl, benzophenap, pyributicarb, tenyl chlor, MCPB, benferate, butamifos, cyclosulfamuron, dimetametrine, eprocarb, fentolazamide, indanophane, inprothiolane, molinate, oxadichrome horn, Paclobutrazol, pentoxazone, prohexa There are dione-Ca, pyrazogyl, simetreen, thiobencarb and uniconazole. Examples of fungicides include acibenzolar-S-methyl, isoprothiolane, ipconazole, iprodione, oxophosphate, kasugamycin, capramide, captan, thiabendazole, thiram, thiophenate-methyl, organocopper, tricyclazole, triflumizole, paridamycin, azo Xistulobin, pyroxylone, fludioxonil, prochloraz, probenazole, benomyl, metasulfocarb, TPN, BJL-002, BJL-003, chlorothalonil, copper, diclocimets, dichromedine, edifenphos, phenoxanyl, ferrimzone, flutolanil, furamepizil, promexazole, promexazole There are metminosulobin, pefrazoate, pencyclon, teclophthalam and tifluzamide. Insecticides include isoprothiolane, imidacloprid, etofenprox, cartap, thiamethoxam, thiocyclam, bensultap, bendiocarb, monocrotophos, alprocarb, pimetruzine, benfuracarb, buprofezin, carbosulfan, cycloprotorin, fenitrothion, fiprofento, isoxathione, , Silafluorene, triazophos, trichlorphone, methoxyphenozide and clothianidin.
[0006]
Among these pesticidal active ingredients, Acibenzolar-S-methyl, fludioxonil and pyroxylone as fungicides, thiamethoxam, thiocyclam and pimetrudin as insecticides, and pretilachlor as herbicide Sinosulfuron is particularly preferred, and all of these ingredients are those produced by Novartis Crop protection AG.
[0007]
Suitable solid carriers for use are usually natural inorganic fillers such as zeolite, calcite, talc, kaolin, montmorillonite, attapulgite or another inorganic carrier. In order to improve the physical properties, highly dispersible silicic acid or highly dispersible absorbent polymers can be added. Suitable granulated adsorbent carriers are porous carriers such as pumice, crushed bricks, sepiolite or bentonite and suitable non-absorbable carriers are eg calcite or sand. Furthermore, a large number of pre-granulated materials of inorganic or organic species can be used, for example dolomite or powdered plant residues.
[0008]
Suitable surfactants and dispersants are nonionic, cationic and / or anionic agents with good emulsifying, dispersing and wetting properties.
[0009]
Suitable anionic dispersants / surfactants are for example the following components:
Salts of polystyrene sulfonic acid, especially alkali metal salts, alkaline earth metal salts and ammonium salts;
Salts of polyvinylsulfonic acid, in particular alkali metal salts, alkaline earth metal salts and ammonium salts;
Naphthalenesulfonic acid, preferably a salt of a condensate of naphthalene-2-sulfonic acid and formaldehyde, in particular alkali metal salts, alkaline earth metal salts and ammonium salts;
Salts of condensates of naphthalenesulfonic acid with phenolsulfonic acid and formaldehyde, in particular alkali metal salts, alkaline earth metal salts and ammonium salts;
Salts of lignin sulfonic acid, especially sodium, potassium, magnesium, calcium or ammonium salts;
Naphthalenesulfonic acid salts, especially alkali metal salts, alkaline earth metal salts and ammonium salts.
[0010]
Suitable nonionic dispersants / surfactants are, for example, polyvinyl alcohol, polyvinyl methyl ether, polyvinyl pyrrolidone, alkylated polyvinyl pyrrolidone, hydroxyethyl cellulose, hydroxypropyl cellulose, methyl cellulose (degree of substitution; 1.5-2), hydroxyethyl methyl cellulose. Hydroxypropylmethylcellulose, poly (2-hydroxyethyl) methacrylate, poly [2- (2-hydroxyethoxy) ethyl] methacrylate, polyethylene oxide (polyoxyethylene) and polyallyl alcohol (polyglycidol);
Products obtained by the reaction of ethylene oxide or a combination of ethylene oxide and propylene oxide with fatty alcohols, alkylphenols, styrenephenols, fatty acids, fatty acid esters of polyhydroxy compounds, castor oil, fatty acid amides and fatty amines (but ethylene oxide units) And the number of propylene oxide units can vary within a wide range). In general, the number of ethylene oxide units or ethylene oxide units and propylene oxide units is 1 to 200, preferably 5 to 100, and most preferably 8 to 40.
[0011]
Suitable cationic dispersants / surfactants are, for example, at least one C as N-substituent.₈~ C_{twenty two}It is a quaternary ammonium salt containing an alkyl group and an unsaturated or halogenated lower alkyl group, benzyl group or hydroxy-lower alkyl group as another substituent.
[0012]
Granules or powders of the pesticides (1) and (2) can be produced by any known method, for example by mixing the active ingredient with a carrier material, a dispersant / surfactant and an auxiliary agent, followed by a fluid bed grinder Alternatively, it can be produced by granulating by means of extrusion, compression, or agglomeration with a stirring type crusher; mechanically pulverized by, for example, a hammer mill or wet pulverized by, for example, a bead mill; and tableted by a roller compressor. The content of active ingredient can be varied within a wide range, for example from 1 to 50% by weight, based on the total weight of the granule or powder. Examples of such granules or powders are Bion core GR 2.5 / 2.7 / 2.8 / 3.3, granules containing acibenzolar-S-methyl in amounts of 2.5, 2.7, 2.8 and 3.3% by weight, respectively 2.4, Actara core GR 2.4 / 2.5 / 3.3, granules containing thiamethoxam in amounts of 2.5 and 3.3% by weight and granules containing pyroxylone in amounts of 2.4, 4.7, 9.4, 26.3, 32.2 and 36.6% by weight, respectively Pirokilone Core GR 2.4 / 4.7 / 9.4 / 26.3 / 32.2 / 36.6, all of which are commercial products of Novartis Agro.
[0013]
Prior to coating with a water-emulsifiable thermoplastic polymer, the granules or powders are hydrophobic liquids such as olive oil, palm oil, soybean oil, liquid paraffin or the like, preferably liquid paraffin in whole or in part. Can be coated. The hydrophobic liquid is used in an amount of 0.01 to 10% by weight, preferably 0.05 to 5% by weight, most preferably 0.1 to 1% by weight, based on the total weight of the composition of the present invention.
[0014]
These granules or powders of pesticides (1) and (2) are coated with one or more layers of a water-emulsifiable thermoplastic polymer. According to the present invention, "water-emulsifiable thermoplastic polymer" means any polymer that is emulsifiable in water, thermoplastic, and film-forming. These polymers are well known in the art. Examples of such polymers include polyethylene, polypropylene and copolymers of ethylene and / or propylene and unsubstituted or substituted olefins as comonomers; polyvinyl alcohol and copolymers of vinyl alcohol and unsubstituted or substituted olefins as comonomers; Copolymers of polyacrylates and methacrylates and / or acrylates with unsubstituted or substituted olefins as comonomers, polymethacrylic acid, polyacrylic acid and polymaleic acid and methacrylic acid, acrylic acid and / or maleic acid and unsubstituted or substituted as comonomers Copolymers with olefins; copolymers of polymaleic acid esters and maleic acid with unsubstituted or substituted olefins as comonomers; polyvinyl acetate and vinyl Copolymers of tate and unsubstituted or substituted olefins as comonomers; polyacrylonitrile and copolymers of acrylonitrile and unsubstituted or substituted olefins as comonomers; polyacrylamides and polymethacrylamides and acrylamides, methacrylamides or both and non-comonomers Copolymers with substituted or substituted olefins; polyhydroxyalkyl- or polyaminoalkyl vinyl alcohols and copolymers of hydroxyalkyl vinyl ethers, aminoalkyl vinyl ethers or both with unsubstituted or substituted olefins as comonomers; polybutadiene, polyisoprene, polychloroprene and butadiene , Isoprene, chloroprene or two or three of these components and an unsubstituted or substituted monomer as a comonomer Copolymers with olefins; hydroxylated polybutadienes from butadiene, isoprene or chloroprene and copolymers of butadiene, isoprene, chloroprene or two or three of these monomers with unsubstituted or substituted olefins as comonomers; polystyrene and styrene with non Copolymers with substituted or substituted olefins; hydroxy- or aminopolystyrene, chloromethylpolystyrene and polystyrenesulfonic acid and hydroxystyrene, aminostyrene, chloromethylstyrene, polystyrene sulfonic acid or two or more of these monomers and non-comonomer Copolymers with substituted or substituted olefins; polyurethanes.
[0015]
Preferred polymers are, for example, polyethylene, polypropylene and copolymers of ethylene and / or propylene with unsubstituted or substituted olefins as comonomers; polymethacrylates, polyacrylates and methacrylates and / or copolymers of acrylates with unsubstituted or substituted olefins as comonomers; Polyvinyl acetate and copolymers of vinyl acetate and unsubstituted or substituted olefins as comonomers; Polyacrylonitrile and copolymers of acrylonitrile and unsubstituted or substituted olefins as comonomers; Acrylamide or methacrylamide and unsubstituted or substituted olefins as comonomers A copolymer of polybutadiene, polyisoprene, polychloroprene and butadiene, isoprene, chloroprene or Copolymers of two or more of these monomers with unsubstituted or substituted olefins as comonomers; polystyrene and copolymers of styrene with unsubstituted or substituted olefins; hydroxystyrene, aminostyrene, chloromethylstyrene or polystyrenesulfonic acid; Copolymers with unsubstituted or substituted olefins as comonomers; polyurethanes.
[0016]
Particularly preferred polymers are for example polyacrylates such as polymethyl acrylate and polyethyl acrylate; polymethacrylates such as polymethyl methacrylate and polyethyl methacrylate; polyvinyl acetate; polystyrene; styrene / acrylate copolymers such as styrene / methyl acrylate and styrene / ethyl acrylate; styrene / methacrylate Copolymers such as styrene / methyl methacrylate and styrene / ethyl methacrylate; vinyl acetate / acrylate copolymers such as vinyl acetate / methyl acrylate and vinyl acetyl / ethyl acrylate; vinyl acetate / methacrylate copolymers such as vinyl acetate / methyl methacrylate and vinyl acetate / ethyl methacrylate DOO; polyisoprene, ethylene / vinyl acetate copolymers, ethylene / vinyl acetate / acrylate terpolymers such as ethylene / vinyl acetate / methyl acrylate, ethylene / vinyl acetate / methacrylate terpolymers such as ethylene / vinyl acetate / methyl methacrylate; polybutadiene. Polyacrylate and polyvinyl acetate are particularly preferred. These polymers can be used alone or as a mixture.
[0017]
If one or more coating layers are formed on the granules or powders of pesticides (1) and (2), these layers need not necessarily be made of the same polymer (s). For example, the first layer can be made of polyvinyl acetate, the second layer can be formed from a polyethylene-polyvinyl acetate mixture, and the third layer can be formed from an ethylene / vinyl acetate / methyl methacrylate copolymer. If the layers consist of different polymers, an “interphase boundary” is formed between the layers, which can be observed by using, for example, an optical microscope or an electron microscope.
[0018]
If the control of release is to be achieved only by adjusting the polymer content, the polymer content is 15-50% by weight for the pesticide (1), preferably 20-40% by weight, based on the total weight of the pesticide (1). Yes, based on the total weight of the agrochemical (2), the agrochemical (2) is 1 to 20% by weight, preferably 2 to 15% by weight. The polymer content can be determined empirically for each of the pesticides (1) and (2) so that the desired release characteristics are obtained, and the release characteristics are effective in the granules or powder of the pesticides (1) and (2) It is strongly dependent on the type and content of the components and the natural conditions for applying the composition of the present invention. The number of polymer coating layers varies with the thickness of each layer, but is usually 1 to 20, preferably 1 to 15. The content of active ingredient can be selected within a wide range, for example 1 to 50% by weight, based on the total weight of the granule or powder.
[0019]
If the control of the release is to be achieved only by adjusting the active ingredient content, granules or powders with low active ingredient content are used for pesticides (1) and granules or powders with high active ingredient content are used for pesticides (2). In this case, the active ingredient content for pesticides (1) and (2) is determined empirically under a predetermined polymer content. The number of polymer layers is 1 to 20, preferably 1 to 15. The active ingredient content of pesticides (1) and (2) is 1 to 50% by weight based on the total weight of each granule or powder, provided that the active ingredient content of the former killing agent is the latter killing agent. The content of the active ingredient shall be lower.
[0020]
If the release control is to be achieved by adjusting the polymer content and the active ingredient content, the polymer content is 15-50% by weight for the pesticide (1), preferably 20-40, based on the total weight of the pesticide (1). It is 1 to 20% by weight, preferably 2 to 15% by weight for the agricultural chemical (2) based on the total weight of the agricultural chemical (2). The polymer content can be determined empirically for each of the pesticides (1) and (2) so that the desired release characteristics are obtained, the release characteristics being the active ingredients in the granules or powder of the pesticides (1) and (2) Depending on the type and content and the natural conditions for applying the composition of the present invention. The number of the polymer coating layers varies with the thickness of each layer, but is usually 1 to 20, preferably 1 to 15. In this case, the active ingredient content can be selected within a wide range, for example 1 to 50% by weight, based on the total weight of the granule or powder. The active ingredient content of pesticides (1) and (2) is 1 to 50% by weight based on the total weight of the respective granules or powders, provided that the former (1) is the latter (2). ) Active ingredient content can be lower or higher. This combination makes it possible to control the release within a very wide range.
[0021]
The granules or powders of the pesticides (1) and (2) are preferably non-dispersible in water and can optionally be coated with another component to prevent sticking to each other, eg inorganic particles such as talc, clay, bentonite , Calcium carbonate or the like, preferably talc. Such ingredients may be added in an amount of 0.01 to 10% by weight, preferably 0.05 to 5% by weight, most preferably 0.1 to 2% by weight, based on the total weight of the respective pesticide.
[0022]
The agrochemicals (1) and / or (2) can additionally contain other components commonly used in the art, such as fertilizers, binders, carrier materials and the like.
[0023]
If necessary, the composition according to the invention comprises the following further components:
(1) 'another pesticidal active ingredient (hereinafter referred to as "another active ingredient") is formulated with an inert carrier and a surfactant to form granules or powder, Another sustained-release coated solid pesticide coated with a water-emulsifiable thermoplastic polymer and
(2) 'Another active ingredient' is formulated together with an inert carrier and a surfactant to form granules or powder, and the granules or powder is coated with water in an emulsifying thermoplastic polymer. Release coated solid pesticides
In addition, the sustained release and immediate release can be controlled only by adjusting the content of the thermoplastic polymer, only by adjusting the content of the “other active ingredient”, or by adjusting the content of the thermoplastic polymer and the above-mentioned “other effective”. It is characterized by being adjusted by adjusting the content of “component”. The foregoing applies exactly to the pesticides (1) ′ and (2) ′. Such compositions are particularly useful if desired to maintain one or more pest killing functions, such as fungicidal and insecticidal functions, substantially constant under varying and particularly elevated temperature conditions.
[0024]
The present invention further relates to a method for producing the composition as described above, and this method comprises the steps of producing the agricultural chemicals (1) and (2) and subsequently mixing them.
[0025]
The manufacturing method of pesticide (1) consists of the following steps;
1. charging the mixer with granules or powder,
2. Add hydrophobic liquid in some cases,
3. Add aqueous emulsion of polymer,
4. Remove water from the mixture produced in steps 1-3 by contacting with overflowing air,
5. Repeat steps 3-4 as needed until the desired number of polymer coatings have been formed,
6. Post-dry the coated granules or powder.
[0026]
(However, steps 2 to 5 are performed while rotating the mixer).
[0027]
In a preferred embodiment, steps 3-4 are performed simultaneously and sequentially. Step 4 is advantageously performed with pre-dried air maintained at a temperature of 25-50 ° C. As the mixer used in Step 1, any mixer known in the art, such as onion pan, can be used. A concrete mixer usually used in construction engineering is particularly preferred. The amount of granules or powder to be loaded into the mixer is determined by the volume of the mixer and the required amount of pesticide (1). Step 2 is an optional step. However, it is preferable to incorporate this step 2 in view of preventing the formation of agglomerates or agglomerates of granules or powders that eventually result in an incomplete coating layer. Any hydrophobic liquid may be used, such as olive oil, palm oil and soybean oil. The most preferred hydrophobic liquid is liquid paraffin. The hydrophobic liquid is added in an amount of 0.01 to 10% by weight, preferably 0.05 to 5% by weight, more preferably 0.1 to 1% by weight, based on the total weight of the agrochemical (1). The aqueous emulsion of the polymer used in step 3 is prepared from a water-emulsifiable thermoplastic polymer by mixing with water. Contact with dry air is usually achieved by air blowing commonly used in the art. The blowing rate can be selected depending on the amount of granules or powder in step 1 and the amount of polymer aqueous emulsion in step 2. For example, if the amount of granules in step 1 (diameter 1 mm, length 3 mm) is 200 kg and the amount of PVAc (polyvinyl acetate) aqueous emulsion (50% emulsion) in step 2 is 11.9 kg, 45 m^ThreeIt is convenient to use a blowing speed of / min. The decrease in the drying rate can be examined by any known method such as moisture detection. Steps 3-4 are repeated until a set of coating layers is formed, the coating layers occupying a predetermined content in the granule or powder. The number of coating layers is selected according to the above description. When coating the granules, it is convenient to use a rotational speed of 5-100 rpm, preferably 5-50 rpm, more preferably 5-30 rpm. After step 4 or 5, another component that prevents the granules or powder from sticking together may be added as described above.
[0028]
The method for producing the pesticide (2) is the same as the method for the pesticide (1), except that the granule or powder in step 1 is different from that of the pesticide (1) if the control of the release includes adjustment of the active ingredient content. Shall have different active ingredient content, and the polymer to be used in pesticide (2) is usually the same as the polymer used in pesticide (1), but the type of polymer emulsion added in step 3 may be different. If the release control includes adjustment of the polymer content and each coating layer has the same thickness over the pesticides (1) and (2), then the number of coating layers in step 5 is the same as that of the pesticide (1). Are usually different. The selection of the number of polymer layers and the content of active ingredients is as described above.
[0029]
The agricultural chemicals (1) and (2) thus produced are then mixed in the desired mixing ratio, thereby obtaining the composition of the invention.
[0030]
Contains a first sustained release pesticide (1), a first immediate release pesticide (2), a second sustained release pesticide (1) 'and a second immediate release pesticide (2)' If it is desirable to produce a composition (where the active ingredients of (1) 'and (2)' are different from those of (1) and (2)), the pesticides (1), (2), (1 ) 'And (2)' can be prepared separately and then mixed in the desired mixing ratio. As mentioned above, this composition exhibits two different pest killing functions corresponding to the active ingredient, which functions remain constant under increasing temperature conditions. Such a composition can also be obtained by subjecting the mixture of granules or powders for pesticides (1) and (1) ′ to steps 1-6 above, thereby having the same polymer coating layer of sustained release pesticides (1) and (1) ′. It can be produced by obtaining a mixture. A mixture of immediate release pesticides (2) and (2) ′ is produced in the same manner, followed by mixing with the previously produced mixture of sustained release pesticides (1) and (1) ′. The mixing ratio of granules for pesticides (1) and (1) 'or (2) and (2)' is the desired mixing ratio of pesticides (1) and (1) 'or (2) and (2)' Correspond. First, granules or powders containing active ingredients for agricultural chemicals (1) and (1) ′ are manufactured, and then the steps 1 to 6 are applied to differ only in the types and contents of the active ingredients. It is further possible to produce such a composition by obtaining a mixture of (1) and (1) ′. A mixture of immediate release pesticides (2) and (2) ′ is produced in the same manner, followed by mixing with the previously produced mixture of sustained release pesticides (1) and (1) ′. The mixing ratio between the active ingredients for pesticides (1) and (1) 'or (2) and (2)' is the desired mix of pesticides (1) and (1) 'or (2) and (2)' Corresponds to the ratio.
[0031]
(Example)
The following materials were used to produce the compositions of the present invention and their slight release behavior was examined.
[0032]
Bion / Aktara Core (Bion / Actara core) GR (2.5 + 2.5);
A rod-like granule having a diameter of about 1 mm and a length of about 3 mm, comprising the following components:
2.5% by weight of acibenzolar-S-methyl, a plant activator that protects plants from attack by pathogens by activating the plant's natural defense system, a product of Novartis Crop Protection,
2.5% by weight thiamethoxam, insecticide, Novartis Crop Protection,
15% by weight of ZEEKLITE SGW, a product of Sieglite,
5.6% by weight Amycol C (pre-gelatinized dendritic) Nippon Starch Chemical products and
74.4% by weight Neorait clay, a product of Neolite Kosan.
Bion / Aktara Core GR (3.3 + 3.3) ;
A rod-like granule having a diameter of about 1 mm and a length of about 3 mm, comprising the following components:
3.3 wt% acibenzolar-S-methyl,
3.3% by weight thiamethoxam,
15% by weight Siegrite SGW,
7.2% by weight Amicol C (pre-gelatinized dendritic powder) and
71.2 wt% neolite clay.
[0033]
Piroquiron / Aktara Core GR (2.4 + 2.4) ;
A rod-like granule having a diameter of about 1 mm and a length of about 3 mm, comprising the following components:
2.4% by weight Pyroquilon, pesticides, Novartis crop protection company products,
2.4 wt% thiamethoxam,
50% AX clay, Neolite Kosan product,
3.0% SH-502, 50% PVAc emulsion, Showa Polymer Co., Ltd.
5.0% by weight Amicol C (pre-gelatinized den powder) and
37.2 wt% neolite clay.
[0034]
Piroquiron / Aktara Core GR (36.5 + 3.3) ;
A rod-like granule having a diameter of about 1 mm and a length of about 3 mm, comprising the following components:
36.5% by weight of pyrokilone,
3.3% by weight thiamethoxam,
30% AX clay,
3.0 wt% SH-502,
5.0% by weight Amicol C (pre-gelatinized den powder) and
32.2 wt% neolite clay.
[0035]
Piroquiron / Aktara Core GR (4.7 + 2.4) ;
A rod-like granule having a diameter of about 1 mm and a length of about 3 mm, comprising the following components:
4.7% by weight of pyrokilone,
2.4 wt% thiamethoxam,
50% AX clay,
3.0 wt% SH-502,
5.0% by weight Amicol C (pre-gelatinized den powder) and
34.9% by weight neolite clay.
[0036]
Piroquiron / Aktara Core GR (32.2 + 3.3) ;
A rod-like granule having a diameter of about 1 mm and a length of about 3 mm, comprising the following components:
32.2% by weight of pyrokilone,
3.3% by weight thiamethoxam,
30% AX clay,
3.0 wt% SH-502,
5.0% by weight Amicol C (pre-gelatinized den powder) and
26.5% by weight neolite clay.
[0037]
Piroquiron / Aktara Core GR (9.4 + 2.4) ;
A rod-like granule having a diameter of about 1 mm and a length of about 3 mm, comprising the following components:
9.4% by weight of pyrokilone,
2.4 wt% thiamethoxam,
50% AX clay,
3.0 wt% SH-502,
5.0% by weight Amicol C (pre-gelatinized den powder) and
30.2 wt% neolite clay.
[0038]
Piroquiron / Aktara Core GR (26.3 + 3.3) ;
A rod-like granule having a diameter of about 1 mm and a length of about 3 mm, comprising the following components:
26.3% by weight of pyrokilone,
3.3% by weight thiamethoxam,
30% AX clay,
3.0 wt% SH-502,
5.0% by weight Amicol C (pre-gelatinized den powder) and
32.4 wt% neolite clay.
[0039]
Piroquiron core GR 63.1 ;
A rod-like granule having a diameter of about 1 mm and a length of about 3 mm, comprising the following components:
63.1% by weight of pyrokilone,
0.1% by weight SORPOL 5115, (alkenyl sulfonate), a product of Toho Chemical Industries,
5.0% by weight Amicol H (pre-gelatinized den powder), Nippon Starch Chemical products, and
31.8% by weight neolite clay.
[0040]
Thiamethoxam core GR 5.1 ;
A rod-like granule having a diameter of about 1 mm and a length of about 3 mm, comprising the following components:
5.1 wt% thiamethoxam,
0.1% by weight Solpol 5115,
15% by weight Zeklite SGW,
5.0% by weight Amicol H (pre-gelatinized den powder) and
74.8 wt% neolite clay.
[0041]
Piroquiron / Aktara Core GR (3.8 + 3.8) ;
A rod-like granule having a diameter of about 1 mm and a length of about 3 mm, comprising the following components:
3.8% by weight of pyrokilone,
3.8% by weight thiamethoxam,
0.1% by weight Solpol 5115,
15% by weight Zeklite SGW,
5.0% by weight Amicol C (pre-gelatinized den powder) and
72.3 wt% neolite clay.
[0042]
All of the granules are products of Novartis Agro.
[0043]
PVAc; Polyvinyl acetate
SH − 502; PVAc 50% emulsion, Showa Polymer Co., Ltd. product
Moresco white (Moresco white)P-70: Liquid paraffin, Matsumura Oil products
Talcum ( Talcum ) TA ;Talc, Kunimine Indus Trees products
Example 1 (Production example)
(1) 890 g of Bion / Actara Core GR (2.5 + 2.5) was loaded into an onion pan (manufactured by Hata Iron Works) and then the pan was continuously rotated at a speed of about 20 rpm.
[0044]
(2) Next, 5 g of Moresco White P-70 was added.
[0045]
(3) Subsequently, 100 g of SH-502 was added, followed by about 0.6 m using air dried at 25 ° C. for 5-15 minutes.^ThreeDry with air blowing per minute.
[0046]
(4) Step (3) was repeated twice.
[0047]
(5) Then 5 g of talcum TA was added.
[0048]
(6) Finally, the double-coated Bion / Actara core GR (2.5 + 2.5) thus obtained was post-dried under conditions of an inlet air temperature of 60 ° C. and an outlet air temperature of 50 ° C. or more.
[0049]
A mixture of fast-release coated solid pesticides having the following composition was thus produced:

(7) Next, 660 g of Bion / Actara core GR (3.3 + 3.3) was loaded into an onion pan (manufactured by Hata Iron Works Co., Ltd.), and then rotated continuously at a speed of about 20 rpm.
[0050]
(8) Next, 5 g of Moresco White P-70 was added.
[0051]
(9) Then 82 g of SH-502 was added, followed by 0.6m of air dried at 25 ° C for 5-15 minutes.^ThreeDry with air blowing per minute.
[0052]
(10) Step (9) was repeated 8 times.
[0053]
(11) Then 5 g of talcum TA was added.
[0054]
(12) Finally, the eight times coated Bion / Actara core GR (3.3 + 3.3) thus obtained was post-dried under conditions of an inlet air temperature of 60 ° C. and an outlet air temperature of 50 ° C. or more.
[0055]
Thus, a corresponding sustained release coated solid agrochemical mixture having the following composition was prepared:

(13) The mixture of the fast-release coated pesticide prepared as described above and the mixture of the sustained-release coated pesticide are mixed at a weight ratio of 1: 1, whereby the present invention having two active ingredients is mixed. A composition was obtained.
[0056]
Example 2 (Production example)
A composition was prepared in the same manner as in Example 1 except that the mixture of the fast-release coated pesticide and the sustained-release coated pesticide were mixed at a weight ratio of 6: 4.
[0057]
Example Three (Production example)
A composition was prepared in the same manner as in Example 1, except that the mixture of the immediate release coated pesticide and the sustained release coated pesticide were mixed at a weight ratio of 4: 6.
[0058]
Example Four (Production example)
(1) 890 g of Pyrokylon / Actala core GR (2.4 + 2.4) is loaded into an onion pan (manufactured by Hata Iron Works Co., Ltd.), and after that, the pan is continuously rotated at a speed of about 20 rpm.
[0059]
(2) Next, 5 g of Moresco White P-70 was added.
[0060]
(3) Subsequently, 67 g of SH-502 was added, followed by 0.6 m of air dried at 25 ° C. for 5 to 15 minutes.^ThreeDrying with air blowing / min.
[0061]
(4) Step (3) was repeated 3 times.
[0062]
(5) Then 5 g of talcum TA was added.
[0063]
(6) Finally, the triple-coated Pyrochilone / Actala core GR (2.4 + 2.4) thus obtained was post-dried under conditions of an inlet air temperature of 60 ° C. and an outlet air temperature of 50 ° C. or more.
[0064]
Thus, an immediate release coated pesticide mixture having the following composition was prepared:

(7) Next, 640 g of Pyroxylone / Actala core GR (36.5 + 3.3) was loaded into an onion pan, and after that, the pan was continuously rotated at a speed of about 20 rpm.
[0065]
(8) Then 5 g of Moresco white was added.
[0066]
(9) Subsequently, 140 g of SH-502 was added, followed by 0.6 m of air dried at 25 ° C. for 5 to 15 minutes.^ThreeDrying with air blowing / min.
[0067]
(10) Then 70 g of SH-502 is added, followed by 0.6 m of dry air at 25 ° C. for 5-15 minutes.^ThreeDrying with air blowing / min.
[0068]
(11) Step (10) was repeated 4 times.
[0069]
(12) Then 2.5 g of talc was added.
[0070]
(13) The thus-obtained Pyroxylon / Actala core GR (36.5 + 3.3) coated 5 times was subjected to post-drying under conditions of an inlet air temperature of 60 ° C. and an outlet air temperature of 50 ° C. or more.
[0071]
(14) The five times coated Pyroxylon / Actala core GR (36.5 + 3.3) was reloaded into an onion pan that was constantly rotating at a speed of about 20 rpm.
[0072]
(15) Subsequently, 70 g of SH-502 was added, followed by 0.6 m of air dried at 25 ° C. for 5-15 minutes.²Drying with air blowing / min.
[0073]
(16) Step (15) was repeated 4 times.
[0074]
(17) Then 2.5 g of talc was added.
[0075]
(18) The nine times coated Pyroxylone / Actala core GR (36.5 + 3.3) thus obtained was post-dried under conditions of an inlet air temperature of 60 ° C. and an outlet air temperature of 50 ° C. or more.
[0076]
Thus, a corresponding sustained release coated pesticide mixture having the following composition was prepared:

(18) The mixture of the fast-release coated pesticide prepared as described above and the mixture of the sustained-release coated pesticide are mixed at a weight ratio of 1: 1, whereby the present invention having two active ingredients is mixed. A composition was obtained.
[0077]
Example Five (Production example)
(1) 890 g of Pyrokylone / Actala core GR (4.7 + 2.4) was loaded into an onion pan (manufactured by Hata Iron Works), and the pan was then continuously rotated at a speed of about 20 rpm.
[0078]
(2) Next, 5 g of Moresco White P-70 was added.
[0079]
(3) Subsequently, 67 g of SH-502 was added, followed by 0.6m of dry air at 25 ° C for 5-15 minutes.^ThreeDrying with air blowing / min.
[0080]
(4) Step (3) was repeated 3 times.
[0081]
(5) Then 5 g of talcum TA was added.
[0082]
(6) Finally, the triple-coated Pyrochilone / Actala core GR (4.7 + 2.4) thus obtained was post-dried under conditions of an inlet air temperature of 60 ° C. and an outlet air temperature of 50 ° C. or more.
[0083]
A mixture of fast-release coated pesticides having the following composition was thus produced:

(7) 640 g of Pyroxylone / Actala core GR (32.2 + 3.3) was loaded into an onion pan, and then rotated at a speed of about 20 rpm.
[0084]
(8) Then 5 g of Moresco white was added.
[0085]
(9) Subsequently, 140 g of SH-502 was added, followed by 0.6 m of dry air at 25 ° C. for 5-15 minutes.^ThreeDrying with air blowing / min.
[0086]
(10) Then 70 g of SH-502 is added, followed by 0.6 m of dry air at 25 ° C. for 5-15 minutes.^ThreeDrying with air blowing / min.
[0087]
(11) Step (10) was repeated 4 times.
[0088]
(12) Then 2.5 g of talc was added.
[0089]
(13) The thus-obtained Pyroxylone / Actala core GR (32.2 + 3.3) coated five times was subjected to post-drying under conditions of an inlet air temperature of 60 ° C. and an outlet air temperature of 50 ° C. or more.
[0090]
(14) The dry, 5 times coated Pyroxylon / Actara Core GR (32.2 + 3.3) was reloaded into an onion pan that constantly rotates at a speed of about 20 rpm.
[0091]
(15) Subsequently, 70 g of SH-502 was added, followed by 0.6 m of dry air at 25 ° C. for 5-15 minutes.^ThreeDrying with air blowing / min.
[0092]
(16) Step (15) was repeated 4 times.
[0093]
(17) Then 2.5 g of talc was added.
[0094]
(18) The nine times coated Pyroxylone / Actala core GR (32.2 + 3.3) thus obtained was post-dried under conditions of an inlet air temperature of 60 ° C. and an outlet air temperature of 50 ° C. or more.
[0095]
Thus, a sustained release coated pesticide mixture having the following composition was prepared:

(18) The mixture of the fast-release coated pesticide prepared as described above and the mixture of the sustained-release coated pesticide are mixed at a weight ratio of 1: 1, whereby the present invention having two active ingredients is mixed. A composition was obtained.
[0096]
Example 6 (Production example)
(1) 890 g of Pyrokylone / Actala core GR (9.4 + 2.4) was loaded into an onion pan (manufactured by Hata Iron Works Co., Ltd.), and the pan was continuously rotated at a speed of about 20 rpm.
[0097]
(2) Next, 5 g of Moresco White P-70 was added.
[0098]
(3) Subsequently, 67 g of SH-502 was added, followed by 0.6 m of air dried at 25 ° C. for 5 to 15 minutes.^ThreeDrying with air blowing / min.
[0099]
(4) Step (3) was repeated 3 times.
[0100]
(5) Then 5 g of talcum TA was added.
[0101]
(6) Finally, the triple-coated Pyrochilone / Actala core GR (9.4 + 2.4) thus obtained was subjected to post-drying under conditions of an inlet air temperature of 60 ° C. and an outlet air temperature of 50 ° C. or more.
[0102]
A mixture of fast-release coated pesticides having the following composition was thus produced:

(7) 640 g of Pyroxylone / Actala core GR (26.3 + 3.3) was loaded into an onion pan, and the pan was then rotated at a rate of about 20 rpm.
[0103]
(8) Then 5 g of Moresco white was added.
[0104]
(9) Subsequently, 140 g of SH-502 was added, followed by 0.6 m of dry air at 25 ° C. for 5-15 minutes.^ThreeDrying with air blowing / min.
[0105]
(10) Then 70 g of SH-502 is added, followed by 0.6 m of dry air at 25 ° C. for 5-15 minutes.^ThreeDrying with air blowing / min.
[0106]
(11) Step (10) was repeated 4 times.
[0107]
(12) Then 2.5 g of talc was added.
[0108]
(13) The thus-obtained Pyroxylone / Actala core GR (26.3 + 3.3) coated 5 times was subjected to post-drying under conditions of an inlet air temperature of 60 ° C. and an outlet air temperature of 50 ° C. or more.
[0109]
(14) The dry, 5 times coated Pyroxylon / Actala Core GR (26.3 + 3.3) GR was reloaded into an onion pan that rotates constantly at a speed of about 20 rpm.
[0110]
(15) Subsequently, 70 g of SH-502 was added, followed by 0.6 m of dry air at 25 ° C. for 5-15 minutes.^ThreeDrying with air blowing / min.
[0111]
(16) Step (15) was repeated 4 times.
[0112]
(17) Then 2.5 g of talc was added.
[0113]
(18) The nine times coated Pyroxylon / Actala core GR (26.3 + 3.3) thus obtained was post-dried under conditions of an inlet air temperature of 60 ° C. and an outlet air temperature of 50 ° C. or more.
[0114]
Thus, a sustained release coated pesticide mixture having the following composition was prepared:

(19) A mixture of a fast-release coated pesticide prepared as described above and a mixture of sustained-release coated pesticide are mixed at a weight ratio of 1: 1, whereby the present invention having two active ingredients is mixed. A composition was obtained.
[0115]
Example 7 (Production example)
(1) 890 g of Pyrokylone / Actala core GR (3.8 + 3.8) is loaded into an onion pan (manufactured by Hata Iron Works), and then the pan is rotated at a constant speed of about 20 rpm.
[0116]
(2) Next, 20 g of Moresco White P-70 was added.
[0117]
(3) Subsequently, 107 g of SH-502 was added, followed by 0.6 m of dry air at 25 ° C. for 5-15 minutes.^ThreeDrying with air blowing / min.
[0118]
(4) Step (3) was repeated twice.
[0119]
(5) Then 5 g of talcum TA was added.
[0120]
(6) Finally, the twice-coated Pyroxylone / Actala core GR (3.8 + 3.8) thus obtained was subjected to post-drying under conditions of an inlet air temperature of 60 ° C. and an outlet air temperature of 50 ° C. or more.
[0121]
A mixture of fast-release coated pesticides having the following composition was thus produced:

(7) 640 g of Pyrochiron Core GR 63.1 was loaded into an onion pan and the pan was then rotated at a constant speed of about 20 rpm.
[0122]
(8) Then 22 g of Moresco White was added.
[0123]
(9) Subsequently, 94 g of SH-502 was added, followed by 0.6m of dry air at 25 ° C for 5-15 minutes.^ThreeDrying with air blowing / min.
[0124]
(10) Step (9) was repeated 4 times.
[0125]
(11) Next, 2 g of talc was added.
[0126]
(12) The four times coated Pyrochilone Core GR 63.1 thus obtained was post-dried under conditions of an inlet air temperature of 60 ° C. and an outlet air temperature of 50 ° C. or more.
[0127]
(13) The dried, four times coated Pyrochilone Core GR 63.1 was reloaded into an onion pan that rotates constantly at a speed of about 20 rpm.
[0128]
(14) Subsequently, 94 g of SH-502 was added, followed by 0.6m of dry air at 25 ° C for 5-15 minutes.^ThreeDrying with air blowing / min.
[0129]
(15) Step (14) was repeated 3 times.
[0130]
(16) Then 2 g of talc was added.
[0131]
(17) The thus-obtained Pyroxylone GR GR 63.1 coated seven times was subjected to post-drying under conditions of an inlet air temperature of 60 ° C and an outlet air temperature of 50 ° C or higher.
[0132]
(18) The dried, seven times coated Pyrochilone Core GR 63.1 was reloaded into an onion pan rotating at a constant speed of about 20 rpm.
[0133]
(19) Subsequently, 94 g of SH-502 was added, followed by 0.6m of dry air at 25 ° C for 5-15 minutes.^ThreeDrying with air blowing / min.
[0134]
(20) Step (19) was repeated 3 times.
[0135]
(21) Then 1 g of talc was added.
[0136]
(22) The thus-obtained Pyroxylone GR GR 63.1 coated 10 times was post-dried under conditions of an inlet air temperature of 60 ° C. and an outlet air temperature of 50 ° C. or more.
[0137]
Thus, a sustained-release coated pesticide having the following composition was produced:

(23) 640 g of thiamethoxam core GR 5.1 was loaded into an onion pan and the pan was then rotated at a rate of about 20 rpm.
[0138]
(24) Then 20 g of Moresco white was added.
[0139]
(25) Subsequently, 73 g of SH-502 was added, followed by 0.6 m of dry air at 25 ° C. for 5-15 minutes.^ThreeDrying with air blowing / min.
[0140]
(26) Step (25) was repeated 3 times.
[0141]
(27) Then 2 g of talc was added.
[0142]
(28) The dried, three times coated Timethoxam Core GR 5.1 was reloaded into an onion pan that rotates constantly at a speed of about 20 rpm.
[0143]
(29) Subsequently, 73 g of SH-502 was added, followed by 0.6m of dry air at 25 ° C for 5-15 minutes.^ThreeDrying with air blowing / min.
[0144]
(30) Step (29) was repeated 3 times.
[0145]
(31) Then 2 g of talc was added.
[0146]
(32) The thus-coated 6-coated Timethoxam Core GR 5.1 was post-dried under conditions of an inlet air temperature of 60 ° C. and an outlet air temperature of 50 ° C. or more.
[0147]
(33) The dried, six-time coated Timethoxam Core GR 5.1 was reloaded into an onion pan rotating at a constant speed of about 20 rpm.
[0148]
(34) Subsequently, 73 g of SH-502 was added, followed by 0.6 m of dry air at 25 ° C. for 5-15 minutes.^ThreeDrying with air blowing / min.
[0149]
(35) Step (34) was repeated 3 times.
[0150]
(36) Then 1 g of talc was added.
[0151]
(37) The thus-obtained 9-coated Timethoxam Core GR 5.1 was post-dried under conditions of an inlet air temperature of 60 ° C. and an outlet air temperature of 50 ° C. or more.
[0152]
A sustained-release coated pesticide having the following composition was thus produced:

A mixture of the immediate release coated pesticide prepared above and each of the two sustained release coated pesticides were mixed in a 1: 1: 1 weight ratio, thereby combining the two active ingredients. A composition of the invention having was obtained.
[0153]
Example 8 (Release test)
1000 ml of water having a German hardness of 3 times was charged into a 1000 ml stoppered flask, and 250 mg of the pesticide produced in step (6) or (12) of Example 1 or step (6) or (4) of Example 4 250 mg of the pesticide produced in 17) was added. The water temperature was kept at 25 + -2 ° C. If some granules were floating on the surface of the water, they were allowed to settle at the bottom of the flask.
[0154]
(2) Three days after the production of the test system, 10 ml of liquid was pipetted out using a 10 ml hole pipette, and then transferred to a centrifuge tube with a stopper. When pipetting the liquid, the tip of the hole pipette was placed at the midpoint between the liquid surface and the bottom of the flask. After removing the liquid with a pipette, 10 ml of water having a German hardness of 3 degrees was added to the test system. If some granules floated or agglomerated in the liquid transferred to the centrifuge tube, they were centrifuged to settle the granules.
[0155]
(3) Next, the liquid transferred to the centrifuge tube was subjected to HPLC and / or GLC analysis, and the concentration of the active agricultural chemical component in the liquid was measured. This measurement was performed for each active ingredient.
[0156]
(4) Steps (2) to (3) after 1, 3, 7, 14, 21, 28, 36, 42, 50, 56, 63, 71, 77, 80, 101 and 133 days after the production of the test system. 3) was repeated.
[0157]
The results are shown in Table 1.
[0158]
Example 9 (Release test)
The experiment is carried out in the same manner as in Example 8, except that 250 mg of the composition of Step (13) of Example 1 is produced by the agricultural chemical produced in Step (6) or (12) of Example 1 or the step of Example 4. (6) or (17) shall be used in place of the agrochemicals, the release test shall be conducted at 25 ° C and 15 ° C, and the steps (2) to (3) of Example 7 were conducted by producing a test system. 1, 3, 7, 14, 28, 42, 56, 71, 80 and 101 days later, and only the concentration of thiamethoxam shall be measured.
[0159]
The results are shown in Table 2.
[0160]
Table 1 Release test results

Table 2 Results of release test

As can be seen from the results in Table 1 obtained from Example 8, it is clear that the present invention achieves a constant release of one or more active ingredients under elevated temperature conditions. For example, the immediate release pesticide of Example 4 (10% coating layer) completes the release of pyrokilone in 14 days at 25 ° C, while the sustained release pesticide of the same Example (35% coating layer) is 25 It only releases 25% pyroxylone in 14 days at ° C. If the temperature rises above 25 ° C in 14 days, the immediate release pesticide is expected to complete the release of pyroxylone within a period shorter than 14 days before the temperature reaches that temperature. Is done. However, during the period when the immediate release pesticide completes the release of pyroxylone, the release of pyroxylone from the sustained release pesticide is expected to be negligibly small compared to the release of the immediate release pesticide, and the sustained release It is expected that the release rate of pyroxylone from pesticides will increase at elevated temperatures after release from the immediate release pesticides. It is therefore clear that the present invention achieves a constant release of one or more active ingredients even under increasing temperature conditions. The same can be expected from the results of the release behavior of acibenzolar-S-methyl and thiamethoxam.
[0161]
Example 9 is carried out to prove the above expectation using the composition of Example 1, which composition is an immediate-release agrochemical and sustained release whose active ingredients are acibenzolar-S-methyl and thiamethoxam It consists of pesticides. As Table 2 shows, the release rate of thiamethoxam at 25 ° C is about twice as high as the release rate at 15 ° C. However, the release rate during the first two weeks is about twice as great as the release rate during weeks 3-4 at both 15 ° C and 25 ° C. Therefore, if the temperature remains at 15 ° C for the first two weeks after application of the composition of Example 1 and then suddenly increases to 25 ° C, the release rate is 8% for the first week 7% for the 2nd week, 12% for the 3rd week, 10% for the 4th and 5th weeks, 8.5% for the 6th and 7th weeks, 8% for weeks 8 and 9. These results clearly demonstrate that the compositions of the present invention can adequately moderate the release of active ingredients under increasing temperature conditions.
[0162]
Furthermore, as the results from Pyroxylone in Table 1 show, the composition of the present invention requires that the release rate of one or more active ingredients be high at an early stage, but then low and long-term. It is also suitable for applications that need to be persistent. As described above, due to its excellent release controllability, the composition of the present invention is an agrochemical composition indispensable for current and future agricultural and horticultural use that requires further reduction of the farmer's labor force.

Claims (3)

The following components: (1) A pesticide active ingredient selected from acibenzolar-S-methyl, thiamethoxam and pyroxylone is formulated together with an inert carrier and a surfactant to form granules or powders. A solid release pesticide with a sustained release, coated with a water-emulsifiable thermoplastic polymer, and (2) the same active ingredient as the active ingredient of the pesticide (1) is inert. Contains an immediate release coated solid pesticide that is formulated with a carrier and a surfactant to form granules or powder, which is coated with a water-emulsifiable thermoplastic polymer. A pesticide composition comprising: the thermoplastic polymer content is 15-50% by weight of the pesticide (1) based on the total weight of the pesticide (1). Pesticide (2) based on the total weight of the pesticide (2) Hazardous biocides composition is 1 to 20% by weight of. The composition of claim 1 wherein the water - emulsifiable polymer is polyvinyl acetate. Hazardous biocides (1) and (2) the content of the active ingredient, each of harmful biocides (1) and granules or based on the total weight of the powder of 1-50% by weight of (2) The composition according to claim 1 or 2 , which is selected within a range.