WO1995028835A1 - Procede pour produire une matrice de cire contenant un pesticide, et preparation utilisable en agriculture - Google Patents

Procede pour produire une matrice de cire contenant un pesticide, et preparation utilisable en agriculture Download PDF

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Publication number
WO1995028835A1
WO1995028835A1 PCT/JP1995/000780 JP9500780W WO9528835A1 WO 1995028835 A1 WO1995028835 A1 WO 1995028835A1 JP 9500780 W JP9500780 W JP 9500780W WO 9528835 A1 WO9528835 A1 WO 9528835A1
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WO
WIPO (PCT)
Prior art keywords
wax
pesticide
extruder
present
matrix
Prior art date
Application number
PCT/JP1995/000780
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English (en)
Japanese (ja)
Inventor
Kouichi Nakamichi
Shougo Izumi
Hiroyuki Yasuura
Original Assignee
Nippon Shinyaku Co., Ltd.
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Nippon Shinyaku Co., Ltd. filed Critical Nippon Shinyaku Co., Ltd.
Publication of WO1995028835A1 publication Critical patent/WO1995028835A1/fr

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Classifications

    • A—HUMAN NECESSITIES
    • A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
    • A01N25/08—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests containing solids as carriers or diluents

Definitions

  • a multi-screw extruder is a screw-type kneading extruder in which multiple screws can entangle and interfere with each other to generate physically high energy.
  • This multi-screw extruder is a machine that has completely different performance and applications from single-screw extruders, because it can perform processing on raw materials that cannot be obtained with single-screw extruders. be able to.
  • Multiaxial extruders have developed mainly in the food and plastic fields, and are widely used in the processing of food (cereals, proteins, livestock meat, fish meat, etc.) and injection molding of plastic. Recently, its use in the pharmaceutical field has been reported (PCT W092 / 18106, PCT W094 / 08568, PCT W095 / 05809, etc.).
  • the single-screw extruder is a screw-type kneading extruder whose main functions are simple mixing and granulation operations, so no further effects can be expected. It is thought that it is difficult to mix these with uniformity.
  • An object of the present invention is to provide a method for producing pesticide-containing ⁇ xmatrictus which can respond to environmental changes such as changes in temperature and changes in soil moisture more than conventional pesticide-containing ⁇ xmatrices.
  • the pesticide-containing ⁇ xmatrix in which the release of pesticides from the wax matrix and the melting temperature of the wax matrix itself, is highly controlled, can be achieved in a practical and economical manner. It is to provide a manufacturing technology that can be manufactured.
  • extruder multi-axial type extruder
  • the present invention is a method for producing a pesticide-containing wax matrix, characterized in that a plurality of pesticides having different physical properties and a pesticide are used as essential components and processed collectively by an extruder.
  • wax refers to not only wax in the narrow sense of “high-alcohol esters of high-fatty acids” but also wax in a broad sense, ie, 40-90 ′ with the properties of wax (plasticity, glossiness, opacity, etc.). It also means a substance that melts in C.
  • tas examples include melting point, solubility in water (hydrophobic, hydrophilic).
  • wax according to the present invention examples include natural waxes derived from animals and plants, natural waxes derived from petroleum oil or minerals, and synthetic or semi-synthetic waxes *.
  • Hydrophobic waxes include, for example, carnauba wax, wood wax, black wax, wool wax, microcrystalline wax, polyethylene wax, chlorinated naphthalene wax, hydrogenated castor oil, hydrogenated rapeseed oil, beeswax, stearic acid, paraffinic wax. Examples include wax, beef tallow, and cocoa butter.
  • hydrophilic waxes examples include polyethylene glycol 20,000, polyethylene glycol 6,000, polyethylene glycol 4,000, polyethylene glycol 2,000, polyethylene glycol 1,540, and polyethylene glycol. 1,000,000 Polyoxyethylene [105] Polyoxypropylene [5] Glycol, Polyoxyethylene [160] Polyoxypropylene [30] Glycol, Polyoxyethylene [196] Polyoxypropylene [67] Glycol And so on.
  • a pesticide-containing paint matrix can be produced by combining two or more of the above paints. Conventionally, it is possible to arbitrarily combine a hydrophobic box and a hydrophilic box, which has been difficult.
  • the total mixing ratio of wax varies depending on the type of wax used, the type of pesticide or additive, the type and type of extruder, etc., but can be 10 to 99.999% (w / w). Preferably, it is 50-99.9% (w / w), more preferably 90-99.9% (w / w).
  • the mixing ratio of each box can be arbitrarily set depending on the desired pesticide release rate, melting temperature, and the like. In general, increasing the ratio of hydrophilic wax can speed up the output of pesticides. Also Five
  • the melting temperature of the wax matrix itself can be increased by increasing the ratio of the wax having a high refractive index.
  • insecticides such as ethiofundalp, benfracarp, carbofuran, aldirube, acephate, diazinon, imidacloprid, benomyl, thiophanate methyl, hexaconazole, isobrothiolane, furaside, Fungicides such as penconazole, fludizazole, vitelenol, buventenazole, triazimefone triazimenol, triflumibule, tricyclazole, josetilamino, etaconazol, etc., mefenacet, falacurl, metrachlor, atrazine And herbicides such as cyanadine, trifluralin and the like.
  • insecticides such as ethiofundalp, benfracarp, carbofuran, aldirube, acephate, diazinon, imidacloprid, benomyl, thiophanate methyl,
  • Pesticides can be used alone or in combination of two or more.
  • the mixing ratio of the pesticide varies depending on the type of pesticide, the type of wax and additive used, the type and type of extruder, etc., but can be 0.001 to 50% (w / w), which is preferable. Is 0.01% to 20% (w / w), more preferably 0.1% to 10% (w / w).
  • additives such as cellulose derivatives, starch, starch derivatives, saccharides, inorganic substances, and mineral substance carriers can be added as necessary. Specifically, for example, the following can be mentioned.
  • Methyl pill cellulose low-substituted hydroxypropyl pill cellulose, hydr xybu pill methyl cellulose 228, hydroxypropyl pilmethyl cellulose 290, hydroxypropyl methylcellulose 290, hydroxy pill pill Methylcellulose acetate succinate, carboxydimethylcellulose, carboxymethylcellulose calcium, croscarmellose sodium.
  • Kaolin Kaolin, talc, magnesium stearate, titanium oxide, precipitated calcium oxide, calcium hydrogen phosphate, clay, bentonite, diatomaceous earth, white carbon.
  • Triethyl citrate Triacetin, medium fatty acid triglyceride, propylene glycol.
  • Soybean oil beannut oil, sesame oil, rapeseed oil, camellia oil, olive oil, peanut oil, Uyuri oil.
  • additives can be incorporated up to 50% (w / w).
  • the main part of the extruder is a barrel called a barrel, equivalent to an exit 7
  • the screw elements include trapezoidal screw elements, trapezoidal cut screw elements, trapezoidal reverse cuts, ball screw elements, needing paddles (kneading discs), and any combination of them. Can be performed.
  • the components sent into the barrel are moved in the barrel by a screw, and are subjected to processing such as shearing and mixing by a screw element such as a kneading paddle in the barrel, and are extruded from the pores of the die.
  • each barrel and die can be independently temperature controlled.
  • a function of transporting water and oil (2) a mixing function, a shearing function, a compressing function, a crushing function, and a heating function, which are generally used in the food and plastic fields.
  • Any extruder can be used as is. It should be noted that a wax matrix according to the present invention can be manufactured sufficiently by using a biaxial extruder having two screws.
  • evening extruders there are various types of evening extruders, such as non-interlocking different direction or co-rotating extruder and full or partially interlocking different direction or co-rotating extruder.
  • a completely interlocking co-rotating extruder is preferable, and a fully interlocking co-rotating twin-screw extruder having a needling paddle (kneading disc) on the shaft is particularly preferable. preferable.
  • the batch matrix according to the present invention can be sufficiently manufactured by performing batch processing in and after a certain barrel.
  • collector processing means that all the raw materials are subjected to shearing, mixing, kneading, and extrusion at substantially the same time.
  • the method of batch processing of raw materials with an extruder is as follows: 1 All raw materials (wax, pesticide, other additives) are simply mixed in advance, and this is supplied from the main supply hole of the extruder and batch processed. , 2 A method of pre-mixing some raw materials among the raw materials, supplying them through the main supply hole of the extruder, and supplying the remaining raw materials through the auxiliary supply holes, and performing batch processing. For example, a method of supplying one raw material j from the main supply hole of the extruder and supplying the “remaining raw material” from the auxiliary supply hole to collectively process the raw material j can be used. Of these methods, 12 is preferred.
  • the main supply hole refers to the most basic supply hole for supplying raw materials into the barrel
  • the auxiliary supply hole refers to a main supply hole capable of supplying auxiliary components to the barrel in an auxiliary manner.
  • any raw material can be further supplied from the auxiliary supply hole.
  • wax and pesticides can be (some) raw materials j, and other additives can be r remaining raw materials j.
  • the present Pixmatrix can be obtained.
  • the wax is one of the "several ingredients”. "The remaining raw material J can be supplied as a mixture from one auxiliary feed hole, 9
  • Individual raw materials or mixtures of arbitrary raw materials can be supplied from a plurality of auxiliary supply holes. It should be noted that one or more of the raw materials J supplied from the main supply hole can be included in the “remaining raw material” and supplied from the auxiliary supply hole.
  • one raw material J is wax
  • the “remaining raw material” can be supplied as a mixture from one auxiliary supply hole, or individual raw materials or arbitrary raw materials can be supplied. Can be supplied from a plurality of auxiliary supply holes. It should be noted that a part of the primary raw material j supplied from the main supply hole can be included in the remaining raw material j and supplied from the auxiliary supply hole.
  • Simple mixing of the raw materials can be performed by a machine such as a kneader mixer, a V-type mixer, a double cone type mixer, a cubic type mixer, a ribbon type mixer, or manually.
  • a machine such as a kneader mixer, a V-type mixer, a double cone type mixer, a cubic type mixer, a ribbon type mixer, or manually.
  • the supply of the raw material into the barrel can be performed manually or by a raw material feeder generally provided in the extruder to be used, but there is no particular limitation as long as the equipment can supply the raw material at a constant speed. It can be carried out.
  • a raw material feeder generally provided in the extruder to be used, but there is no particular limitation as long as the equipment can supply the raw material at a constant speed. It can be carried out.
  • Examples of such an apparatus include a screw feeder, a table feeder, a slurry feeder, a pressure feeder, a belt conveyer-type quantitative feeder, and a magnetic feeder.
  • the temperature of the barrel and die of the extruder can be appropriately set according to the type of wax used. Normally, a temperature about 5 to 30 ° C lower than the melting point of the wax with the highest melting point among the waxes used.
  • the temperature can be set as low as about 10-20.
  • the wax matrix according to the present invention can be obtained even at a higher temperature, but at a higher temperature, the wax usually comes out of the die in a molten state, so that any shape can be obtained. It is difficult to obtain a molded body of
  • the screw rotation speed can be set as appropriate depending on the type and type of extruder, raw material, screw shape, etc. It can be set within the allowable range of the extruder used. .
  • Discharge pressure 10 ⁇ 150kg / cm 2 is suitably, 30 ⁇ 120kg / cm 2 is favorable preferable.
  • the shape and combination of the screw elements that can be used can be selected without any particular limitation. However, it is preferable to use one or more kneeling paddles (kneading discs) having strong kneading action and shearing action.
  • the discharge die can be appropriately changed depending on the purpose. Specific examples include a circular discharge die having various diameters for obtaining a columnar processed product, and a flat discharge die for obtaining a plate-like processed product.
  • Preparations containing Pexmatrix produced by the present invention are also included in the present invention.
  • the formulation is not particularly limited ⁇ Specific examples include powders, powders, tablets and the like. 1 1
  • the preparation according to the present invention can be produced as follows.
  • the raw material batch-processed by the extruder is continuously extruded from the pores of the die as the composition of the present invention.
  • This can be cut to a desired length by a suitable cutting machine, for example, a roller-type crusher, a cutter mill, a pin mill, or the like.
  • This cut product can be used as it is as a granular preparation of the present invention.
  • the wax matrix of the present invention extruded from the pores of the die is used, for example, by a rotary cutter equipped at the tip of the die (for example, a rotary cutter for KBXN-30 manufactured by Kurimoto Iron Works).
  • a rotary cutter equipped at the tip of the die for example, a rotary cutter for KBXN-30 manufactured by Kurimoto Iron Works.
  • the tablet-form preparation of the present invention can be obtained by compression-molding the cut-off granular Matrix according to the present invention.
  • the present invention may also include those obtained by applying a coating treatment or the like to Pex Matrix extruded from the pores of the die, cut granular Pex Matrix, or compression-molded Pex Matrix tablets. it can.
  • a plurality of powders having different physical properties can be mixed sufficiently uniformly, and the release of the pesticide from the wax matrix and the melting temperature of the wax matrix itself are highly controlled.
  • Pexmatrix can be manufactured. Therefore, it is possible to provide a pesticide-containing extract matrix suitable for the situation (seasonal) at the time of spraying, such as the temperature at the time of spraying and the amount of soil moisture. In addition, it is possible to manufacture pesticide-containing plex-matrix that releases pesticides at any temperature. 12
  • pesticides containing pesticides containing pesticides can be provided that release pesticides when the temperature reaches a temperature at which pests and diseases easily occur, and suppress the release of pesticides when the temperature drops.
  • Barrel numbers are assigned in ascending order from the barrel on the sample supply side (entrance side).
  • Example 3 4 and 5 and the die were set to 55, and the same conditions as in Example 1 were applied to manufacture a Pex Matrix according to the present invention.
  • Example 3
  • Example 4 4 g of Mefenaset, 120 g of Carnauba wax powder and 280 g of polyethylene glycol powder are mixed in a glass V-type mixer for 15 minutes, and the barrel 1 of the twin-screw extruder is mixed with 2 g.
  • the processing was performed under the same conditions as in Example 1 except that the barrels 2, 3, 4, and 5 and the die were set to 55'C, to produce a PEX matrix according to the present invention.
  • Axial extruder barrel 1 was set at 25, barrels 2, 3, 4, 5 and die were set at 35, the extrusion speed was set at 100 rpm, and processing was performed under the same conditions as in Example 1. Performed The Pex Matrix according to the present invention was manufactured.
  • a mixture of 5 g of Mephenaset, 350 g of ⁇ , raffin wax, 50 g of cocoa butter, 100 g of polyethylene glycol, and 100 g of powder of 1500 g was mixed with a glass V-type mixer for 15 minutes.
  • step 25 the nozzles 2, 3, 4, 5 and the die were set to 33'C, and processing was performed under the same conditions as in Example 4 to produce a black matrix according to the present invention. did.
  • the Pixmatrix according to the above was manufactured.
  • a mixture of 5 g of Mephenaset, 250 g of Raffin Wax, 250 g of cocoa butter, 50 g of cocoa butter and 200 g of Polyethylene glycol 150 g was mixed with a glass V-type mixer for 15 minutes. Was processed under the same conditions as in Example 8 to produce an exhaust matrix according to the present invention.
  • step 25 the barrels 2, 3, 4, and 5 and the die were set to 3C, and processing was performed under the same conditions as in Example 4 to produce a cell matrix according to the present invention.
  • Example 2 In addition to using 4 g of edible blue No. 1 pigment in place of Mehnaset, treatment was performed under the same conditions as in Example 2 to obtain a sample of the present invention.
  • a mixed powder having the same composition as that of the sample of the present invention was put into a transparent glass beaker (diameter: 11.6 cm, height: i 6 cm), and was heated and melted in a warm bath heated to 90 ° C. The mixture was stirred and mixed with a spatula. After that, the beaker was taken out, allowed to stand in an environment of 25'C, and allowed to cool naturally, thereby producing a Pexmatrix for a comparative test (natural cooling method).
  • a powdered mixture of the same composition was placed in a stainless steel beaker (diameter 20 cm, height 2).
  • Stir-mix cooling operation was performed using a motor stirrer (1200 RTS; manufactured by Shinto Kagaku) to prepare a Pex matrix for a comparative test (stir-mix cooling method).
  • the wax matrix produced by the method of the present invention and the Pex matrix produced by the conventional stirring-mixing cooling method were used with a roll granulator (GRN-101 type; manufactured by Nippon Grannyle Ichiyu Co., Ltd .; the same applies hereinafter).
  • the particles in the range of No. 16 (1000) to No. 30 (0000) were used as samples for the dissolution test. 60 mg of each of these samples was treated with 30 mg of purified water 9 0 ml, and the paddle method (Pad 17
  • the number of elutions of Blue No. 1 was measured over time under the conditions of a rotational speed of 100 rpm and a measurement wavelength of 629 nm. The results are shown in Table 2.
  • the wax matrix according to the present invention manufactured according to Examples 1, 2, and 3 was crushed using a roll granule, and the wax matrix was mixed with a No. 16 (100 ⁇ ) to a No. 30 (50)
  • the melting point was measured using a melting point instrument with a micro-gun.
  • the above sample was dissolved in 3 (900 ml of purified TC water).
  • the elution amount of mefnaset was measured over time under the conditions of the paddle method (paddle rotation speed: 100 rpm) of the Japanese Pharmacopoeia, and the results are shown in Table 3. 18
  • the melting point of the Pex Matrix obtained by the method of the present invention indicates a temperature change relative to the composition ratio of the Pex used, and a Pex Matrix having a desired melting temperature is obtained. Things have come. Also, the release rate increased as the amount of the polyethylene glycol added increased. From this, it was found that release control was possible by changing the composition ratio of hydrophilic and hydrophobic resins.
  • the melting point of the wax matrix can be controlled to a commercial value by changing the composition ratio of three types of waxes (paraffin wax, cocoa butter, and polyethylene glycol) with different melting characteristics and melting points.
  • a drug release was also provided by a Pexmatrix exhibiting the same melting point, and that a rapid drug release was observed when tested at the melting point temperature of wax matrix. It has been found that opposing drug release can be promoted.

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  • Life Sciences & Earth Sciences (AREA)
  • General Health & Medical Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Toxicology (AREA)
  • Pest Control & Pesticides (AREA)
  • Plant Pathology (AREA)
  • Agronomy & Crop Science (AREA)
  • Engineering & Computer Science (AREA)
  • Dentistry (AREA)
  • Wood Science & Technology (AREA)
  • Zoology (AREA)
  • Environmental Sciences (AREA)
  • Agricultural Chemicals And Associated Chemicals (AREA)

Abstract

Ce procédé, qui sert à produire une matrice de cires contenant un pesticide qui soit capable de s'adapter aux changements de l'environnement, consiste à traiter un certain nombre de cires ayant différentes propriétés ainsi qu'un pesticide comme ingrédient essentiel en un seul lot dans une extrudeuse multivis. Etant donné que lesdites cires ayant différentes propriétés peuvent être mélangées entre elles d'une façon suffisament homogène, la libération du pesticide peut se faire avec un niveau de régulation élevé.
PCT/JP1995/000780 1994-04-21 1995-04-20 Procede pour produire une matrice de cire contenant un pesticide, et preparation utilisable en agriculture WO1995028835A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
JP8325694 1994-04-21
JP6/83256 1994-04-21

Publications (1)

Publication Number Publication Date
WO1995028835A1 true WO1995028835A1 (fr) 1995-11-02

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PCT/JP1995/000780 WO1995028835A1 (fr) 1994-04-21 1995-04-20 Procede pour produire une matrice de cire contenant un pesticide, et preparation utilisable en agriculture

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2012080188A1 (fr) 2010-12-17 2012-06-21 Bayer Cropscience Ag Composition contenant des particules de cire insecticide
JP2021535228A (ja) * 2018-09-20 2021-12-16 エルジー・ケム・リミテッド 溶出制御型農薬粒剤及びその製造方法

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS61122202A (ja) * 1984-11-14 1986-06-10 ヘンケル・コマンデイツトゲゼルシヤフト・アウフ・アクチエン 蒸発抑制剤およびその製法と用途
JPS62265217A (ja) * 1986-03-10 1987-11-18 アメリカン・サイアナミド・カンパニ− 持効性大形丸剤配合物の製造方法
JPH06107509A (ja) * 1991-08-23 1994-04-19 E I Du Pont De Nemours & Co 放出の遅い組成物

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS61122202A (ja) * 1984-11-14 1986-06-10 ヘンケル・コマンデイツトゲゼルシヤフト・アウフ・アクチエン 蒸発抑制剤およびその製法と用途
JPS62265217A (ja) * 1986-03-10 1987-11-18 アメリカン・サイアナミド・カンパニ− 持効性大形丸剤配合物の製造方法
JPH06107509A (ja) * 1991-08-23 1994-04-19 E I Du Pont De Nemours & Co 放出の遅い組成物

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2012080188A1 (fr) 2010-12-17 2012-06-21 Bayer Cropscience Ag Composition contenant des particules de cire insecticide
US9451764B2 (en) 2010-12-17 2016-09-27 Bayer Intellectual Property Gmbh Composition comprising insecticide-wax particles
JP2021535228A (ja) * 2018-09-20 2021-12-16 エルジー・ケム・リミテッド 溶出制御型農薬粒剤及びその製造方法
JP7184444B2 (ja) 2018-09-20 2022-12-06 エルジー・ケム・リミテッド 溶出制御型農薬粒剤及びその製造方法

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