CN107232190B - Clothianidin controlled-release embedded granule as well as preparation and application thereof - Google Patents
Clothianidin controlled-release embedded granule as well as preparation and application thereof Download PDFInfo
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- CN107232190B CN107232190B CN201710401099.XA CN201710401099A CN107232190B CN 107232190 B CN107232190 B CN 107232190B CN 201710401099 A CN201710401099 A CN 201710401099A CN 107232190 B CN107232190 B CN 107232190B
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- 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
- A01N25/26—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 in coated particulate form
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- 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
- A01N51/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds having the sequences of atoms O—N—S, X—O—S, N—N—S, O—N—N or O-halogen, regardless of the number of bonds each atom has and with no atom of these sequences forming part of a heterocyclic ring
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- Pest Control & Pesticides (AREA)
- Agronomy & Crop Science (AREA)
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Abstract
The invention discloses clothianidin controlled-release embedded granules, which consist of clothianidin and a carrier, wherein the carrier is a low-melting-point carrier, and the melting point of the carrier is 53-90 ℃; the clothianidin accounts for 10.0-30.0% of the mass of the clothianidin controlled-release embedded granules. The invention also provides a preparation method and application of the clothianidin controlled-release embedded granules. The controlled release embedded granule which is environment-friendly, low in cost and easy for industrial production is prepared by taking a degradable organic compound with low melting point as a carrier, enabling the carrier to be in a molten state by proper heating, uniformly dispersing or dissolving the active ingredients of the pesticide in the molten carrier, naturally cooling, mechanically crushing and sieving. The preparation steps are simple, the embedding rate of the pesticide active ingredients is high, the pesticide active ingredients are gradually released along with the degradation of the carrier, and the effect of preventing and treating plant diseases and insect pests is exerted more efficiently.
Description
Technical Field
The invention belongs to the field of agriculture, and particularly relates to a nicotine pesticide clothianidin, and preparation and application thereof.
Background
The effective utilization rate of the conventional pesticide spray is only 20-30%, most of the active ingredients of the pesticide are lost to the environment such as the atmosphere, soil, water and the like, so that the environment is polluted and the waste is serious. Therefore, the development of a novel pesticide formulation which is safe, environment-friendly, long in lasting period and capable of reducing environmental pollution is one of the development directions of future pesticide formulations.
The controlled release embedded granule is a new pesticide formulation with slow release performance, the low melting point organic compound carrier is in a molten state by heating, the active ingredients of the pesticide are uniformly mixed with the molten carrier or dissolved in the molten carrier, and a granular formulation with a certain particle size range is formed by cooling, crushing and sieving, and the active ingredients in the granule are embedded in a high molecular polymer to form uniform spherical particles, which are also called as amplified microspheres (corresponding to micron-sized microsphere formulations). The appearance of the granule is the same as that of the conventional granule, but the carrier selected by the conventional granule is the conventional filler (such as kaolin, clay, kieselguhr, calcium carbonate and the like) without slow release performance, so that the conventional granule does not have the slow release performance.
Similarly, the controlled release coated granule also has the slow release performance, and can be regarded as an amplified dosage form of the microcapsule (corresponding to a microcapsule dosage form of micron scale). The conventional granules are coated with a layer of degradable plastic film with sustained and controlled release performance to ensure that the granules have sustained and controlled release performance, and the technology is widely applied to sustained and controlled release fertilizers at present. The conventional pesticide granules can also realize the sustained and controlled release performance of the granules by secondary processing by means of the technology, and the controlled release coated granules are prepared.
Clothianidin (clothianidin) is an insecticide among the second generation neonicotinoids, and was co-developed by Bayer corporation and Takeda Wutian corporation, Japan. Clothianidin is a novel pesticide with high efficiency, safety and high selectivity, has the similar action to a nicotine acetylcholine receptor, and has contact poisoning, stomach toxicity and systemic activity. The insecticidal composition is mainly used for preventing and treating homoptera, diptera and certain lepidoptera pests such as aphids, leafhoppers, thrips, plant hoppers and the like on rice, vegetables, fruit trees and other crops, has the advantages of high efficiency, broad spectrum, low dosage, low toxicity, long lasting period, no phytotoxicity to crops, safe use, no cross resistance with conventional pesticides and the like, and has excellent systemic and osmotic effects. The pesticide has the advantages of novel structure, special action mechanism and more excellent performance compared with the traditional nicotine pesticide, and is likely to become a worldwide large-tonnage pesticide variety.
Disclosure of Invention
Aiming at the defects in the field, the invention aims to provide the controlled-release embedded granules which are environment-friendly, low in cost and easy for industrial production.
The invention also aims to provide a preparation method of the clothianidin controlled-release embedded granule.
The third purpose of the invention is to provide the application of the clothianidin controlled-release embedded granules in agriculture.
The technical scheme for realizing the above purpose of the invention is as follows:
a clothianidin controlled-release embedded granule is composed of clothianidin and a carrier, wherein the carrier is a low-melting-point carrier, and the melting point of the carrier is 53-90 ℃; the clothianidin accounts for 10.0-30.0% of the mass of the clothianidin controlled-release embedded granules.
Because the thermal storage temperature of the pesticide is 54 ℃, the carrier selected by the invention can ensure that the granules can not melt under thermal storage.
Further, the carrier is selected from one or more of polyethylene glycol with the molecular weight of 2000-8000, polycaprolactone polyol, beeswax with the melting point of 62-67 ℃, Fischer-Tropsch wax with the melting point of 60-80 ℃ and carnauba wax with the melting point of 80-86 ℃.
Preferably, the polyethylene glycol is polyethylene glycol 4000, and the melting point of the polyethylene glycol is 53-56 ℃.
More preferably, the carrier is one or a combination of two of polyethylene glycol and polycaprolactone polyol, beeswax, Fischer-Tropsch wax and carnauba wax, and the polyethylene glycol accounts for 20-40% of the total mass of the carrier.
The invention relates to a preparation method of clothianidin controlled-release embedded granules, which comprises the steps of heating a carrier to be molten, mixing the carrier with clothianidin raw pesticide, and stirring the mixture to be transparent or semitransparent under the condition of keeping the heating state; stirring and cooling are maintained, and then crushing is carried out.
Further, the carrier is one or a combination of two of polyethylene glycol, polycaprolactone polyol, beeswax, Fischer-Tropsch wax and carnauba wax, and the carriers are added respectively, and the other carrier is added after the carrier added in the former is heated to be molten.
Further, the mixture is crushed and sieved, and particles with the particle size of 60-140 meshes are obtained.
Wherein the clothianidin bulk drug contains 90-99.9% of clothianidin; the added mass of the clothianidin is 20 percent of the mass of the carrier.
The clothianidin controlled-release embedded granule is applied to control psyllids, aphids, scale insects, whiteflies and the like which harm fruit trees, wherein the fruit trees comprise oranges, pears, apple trees, apricot trees, plum trees and peach trees but are not limited thereto; or for controlling homoptera sucking mouth parts pests which harm crops, including but not limited to rice, wheat, corn and cotton, including rice planthopper, leafhopper, rice thrips, wheat aphid, cotton aphid and corn aphid.
According to the method for applying the clothianidin controlled-release embedded granules, the clothianidin controlled-release embedded granules are applied to the roots of plants by being mixed with soil, and the application dosage is 100-300 mg a.i./fruit trees.
Today, the ecological environment sustainable development is increasingly emphasized, and the requirement on the environment is higher and higher. Environmentally unfriendly technologies would be undesirable. The development of new technologies will be towards the direction of environmental friendliness. The controlled release embedded granule which is environment-friendly, low in cost and easy for industrial production is prepared by taking a degradable organic compound with low melting point as a carrier, enabling the carrier to be in a molten state by proper heating, uniformly dispersing or dissolving the active ingredients of the pesticide in the molten carrier, naturally cooling, mechanically crushing and sieving. The preparation steps are simple, the embedding rate of the pesticide active ingredients is high, the pesticide active ingredients are gradually released along with the degradation of the carrier, and the effect of preventing and treating plant diseases and insect pests is exerted more efficiently.
Detailed Description
The following examples are intended to illustrate the invention but are not intended to limit the scope of the invention.
Unless otherwise specified, the means in the examples are all technical means well known in the art.
The clothianidin technical product is purchased from Shandong Hailier chemical Co., Ltd, and has a content of 97%.
Example 1:
8g of polycaprolactone polyol (melting point about 60 ℃) is poured into a 25mL beaker, heated to a molten state, and then 4g of polyethylene glycol 4000 is added and heated on a heating magnetic stirrer until the polycaprolactone polyol is completely dissolved and transparent. After the clothianidin is completely transparent, 4g of 97% clothianidin raw drug is added into the clothianidin raw drug, the mixture is continuously heated and stirred until the mixture is clear and transparent, and then 4g of beeswax (melting point of 62-67 ℃) is added and the mixture is continuously stirred until the mixture is semitransparent. Then cooling, stirring continuously in the cooling process, pouring the mixture onto a prepared valve bag after the temperature is reduced, and spreading the mixture. And after the clothianidin is completely cooled, crushing the clothianidin by using a small universal crusher, and collecting powder with the granularity of less than 100 meshes to obtain the clothianidin controlled-release embedded granules.
Through content detection, the drug loading rate is 17.8%, and the embedding rate is 92%. The release simulation was performed by dialysis in medium (2.5% methanol pH7.0 buffer solution) with 53% release at 10d and 97% release at 30 d. In the same medium, clothianidin bulk drug is released by 80.1% at 10 days, and the release reaches 100% at 20 days, which shows that the prepared clothianidin controlled release embedded granule has a certain slow release effect.
Following the same procedure as example 1, the following examples can be prepared.
Example 2: preparation of 19.4% clothianidin controlled release embedded granules
7g of polycaprolactone polyol (melting point about 60 ℃) is poured into a 25mL beaker and heated to the molten state, 4g of polyethylene glycol 4000 are added and heated on a heating magnetic stirrer until the polycaprolactone polyol is completely dissolved and transparent. After the solution is completely transparent, 4g of 97% clothianidin technical material is added into the solution, the solution is continuously heated and stirred until the solution is clear and transparent, and then 5g of beeswax is added, and the solution is continuously stirred until the solution is semitransparent. Then cooling, stirring continuously in the cooling process, pouring the mixture onto a prepared valve bag after the temperature is reduced, and spreading the mixture. After cooling completely, pulverizing with a small universal pulverizer, and collecting powder with a size of less than 100 meshes. The clothianidin controlled-release embedded granules are obtained.
Through content detection, the drug loading rate is 19.4 percent, and the embedding rate is 100 percent. A dialysis method is used for carrying out a release simulation experiment in a medium (2.5% methanol pH7.0 buffer solution), 46.0% is released in 10 days, 88% is released in 40 days, and the slow release effect is better.
Example 3: preparation of 17.9% clothianidin controlled release embedded granule
Pouring 4g of polyethylene glycol 4000 into a 25mL beaker, heating to a molten state, adding 12g of carnauba wax (melting point 80-86 ℃), and heating on a heating magnetic stirrer until the mixture is completely dissolved and transparent. After the solution is completely transparent, adding 4g of 97% clothianidin technical into the solution, continuing heating and stirring the solution until the solution is clear and transparent. Then cooling, stirring continuously in the cooling process, pouring the mixture onto a prepared valve bag after the temperature is reduced, and spreading the mixture. After cooling completely, pulverizing with a small universal pulverizer, and collecting powder with a size of less than 100 meshes. The clothianidin controlled-release embedded granules are obtained.
Through content detection, the drug loading rate is 17.9 percent, and the embedding rate is 92.3 percent. A release simulation experiment is carried out in a medium (2.5 percent methanol pH7.0 buffer solution) by a dialysis method, 58.3 percent is released in 10 days, 84.7 percent is released in 30 days, and the slow release effect is obvious.
Example 4: preparation of 17.8% clothianidin controlled release embedded granules
4g of polycaprolactone polyol is poured into a 25mL beaker, heated to a molten state, and then 4g of polyethylene glycol 4000 is added, and the mixture is heated on a heating magnetic stirrer until the mixture is completely dissolved and transparent. After the pesticide is completely transparent, 4g of the clothianidin original drug with the concentration of 97 percent is added into the pesticide and is continuously heated and stirred until the pesticide is clear and transparent, and then 8g of Fischer-Tropsch wax (melting point 80 ℃) is added and is continuously stirred until the pesticide is semitransparent. Then cooling, stirring continuously in the cooling process, pouring the mixture onto a prepared valve bag after the temperature is reduced, and spreading the mixture. After cooling completely, pulverizing with a small universal pulverizer, and collecting powder with a size of less than 100 meshes. The clothianidin controlled-release embedded granules are obtained.
Through content detection, the drug loading rate is 17.8%, and the embedding rate is 91.8%. A release simulation experiment is carried out in a medium (2.5 percent methanol pH7.0 buffer solution) by a dialysis method, 58.4 percent is released in 10 days, 84.8 percent is released in 20 days, and a certain slow release effect is achieved.
Comparative example 1
The same procedure as in example 1 was followed, except that 4g of polyethylene glycol, 12g of polycaprolactone polyol, 4g of clothianidin as the starting material and no beeswax were added. The drug loading of the product with a sieve smaller than 100 meshes is 19.1 percent, the embedding rate is 99 percent, the release rate of 7d is 62.3 percent, the release rate of the original drug 7d is 57.5 percent, the release rate is higher than the release rate of the original drug, and the product has no sustained release effect.
Comparative example 2
The same procedure as in example 1 was followed, except that no polyethylene glycol was added, and only 16g of polycaprolactone polyol and 4g of clothianidin as the starting material were added. The drug loading rate of the prepared product is 14%, the embedding rate is 72.2%, the release rate of 7d reaches 84.5%, the release rate is far higher than the release rate of the original drug and is higher than 62.3% of that of the polyethylene glycol added in the comparative example 1, and the sustained release effect is not achieved.
While the present invention has been described in detail with reference to the preferred embodiments, it should be understood that the above description should not be taken as limiting the invention. It will be apparent to those skilled in the art that variations, or modifications, derived or suggested from the disclosure and general knowledge, that achieve the same function and result as described herein, may be substituted for those of ordinary skill in the art, and that all such variations, modifications, and equivalents may be substituted for elements thereof without departing from the scope of the present disclosure.
Claims (7)
1. A clothianidin controlled-release embedded granule is composed of clothianidin and a carrier, and is characterized in that the carrier is a low-melting-point carrier, and the melting point of the carrier is 53-90 ℃; the clothianidin accounts for 10.0-30.0% of the mass of the clothianidin controlled-release embedded granules;
the carrier is polyethylene glycol, polycaprolactone polyol and beeswax, and the polyethylene glycol accounts for 20-40% of the total mass of the carrier;
the polyethylene glycol is polyethylene glycol 4000.
2. The method for preparing clothianidin controlled-release embedded granules according to claim 1, wherein the carrier is heated to be molten, mixed with clothianidin bulk drug, and the mixture is stirred to be transparent or semitransparent under the condition of keeping the heating state; stirring and cooling are maintained, and then crushing is carried out.
3. A method for preparing clothianidin controlled-release embedded granules according to claim 2, wherein each carrier is added separately, and another carrier is added after the previously added carrier is heated to be molten.
4. The preparation method of clothianidin controlled-release embedded granules according to claim 2, wherein the granules are obtained by crushing, sieving and collecting granules of 60-140 meshes.
5. The method for preparing clothianidin controlled-release embedded granules according to any one of claims 2 to 4, wherein the clothianidin bulk drug contains 90 to 99.9 percent of clothianidin; the added mass of the clothianidin is 20 percent of the mass of the carrier.
6. The use of clothianidin controlled release coated granules as claimed in claim 1, for controlling psyllids, aphids, scale insects, whiteflies which damage fruit trees including citrus trees, pear trees, apple trees, apricot trees, plum trees, peach trees; or homoptera sucking mouth parts pests for preventing and treating crops, wherein the crops comprise rice, wheat, corn and cotton, and the homoptera sucking mouth parts pests comprise rice planthoppers, leafhoppers, rice thrips, wheat aphids, cotton aphids and corn aphids.
7. The method for applying the clothianidin controlled-release embedded granules according to claim 1, wherein the clothianidin controlled-release embedded granules are applied to the roots of plants by being mixed with soil, and the application rate is 100-300 mg a.i./fruit trees.
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| CN108935457A (en) * | 2018-07-26 | 2018-12-07 | 广西田园生化股份有限公司 | Application and method that controlled release pesticide as matrix is prepared using beeswax of the beeswax in realizing controlled-release pesticide |
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| JPH0368523A (en) * | 1989-08-08 | 1991-03-25 | Nippon Kayaku Co Ltd | Sustained release composition |
| US20070072775A1 (en) * | 2005-09-29 | 2007-03-29 | Oms Investments, Inc. | Granular controlled release agrochemical compositions and process for the preparation thereof |
| TW200800020A (en) * | 2006-01-26 | 2008-01-01 | Basf Ag | Methods to use 3-pyridyl derivatives as pesticides |
| DE102007057395A1 (en) * | 2007-11-27 | 2009-05-28 | Friedrich-Alexander-Universität Erlangen-Nürnberg | Encapsulated microparticles with a virulent core and method of making the microparticles |
| CN101642097A (en) * | 2009-09-07 | 2010-02-10 | 山东农业大学 | Clothianidin sustained and controlled release granule composite |
| CN102144642B (en) * | 2010-12-20 | 2013-02-20 | 惠州市南天生物科技有限公司 | Trichoderma pill as well as preparation method and application thereof |
| CN106035322B (en) * | 2016-05-25 | 2019-08-23 | 广西立可丰生物科技有限公司 | A kind of controlled release granular pesticide and preparation method thereof |
| CN106518492A (en) * | 2016-10-31 | 2017-03-22 | 广东中迅农科股份有限公司 | Clothianidin granule and preparing method thereof |
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