CN101568256A - Water soluble granule of chlorfenapyr and its preparation - Google Patents

Water soluble granule of chlorfenapyr and its preparation Download PDF

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Publication number
CN101568256A
CN101568256A CNA2008800000748A CN200880000074A CN101568256A CN 101568256 A CN101568256 A CN 101568256A CN A2008800000748 A CNA2008800000748 A CN A2008800000748A CN 200880000074 A CN200880000074 A CN 200880000074A CN 101568256 A CN101568256 A CN 101568256A
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Prior art keywords
chlorfenapyr
water soluble
soluble granule
span
agent
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Chinese (zh)
Inventor
栾贵书
王志祥
迟云英
李海旭
刘长春
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Jiamusi Xingyu Biotechnique Development Co., Ltd.
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栾贵书
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    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION 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
    • A01N43/00Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
    • A01N43/34Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one nitrogen atom as the only ring hetero atom
    • A01N43/36Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one nitrogen atom as the only ring hetero atom five-membered rings

Abstract

The invention provides a water soluble granule of chlorfenapyr. It is made from (by wt%) chlorfenapyr 0.5-50%, emulsifier 1-30%, dispersing agent 1-10%, wetting agent 1-5%, binder 2-4%, stabilizer 1-3% and the rest is filling material. The invention comprises no or small toxic and inflammable aromatic hydrocarbon solvent, therefore the risk of burning and exploding during manufacture, storage and transportation can be reduced. Its advantages include no poison and pollution, no unpleasant odor, low eye irritation, higher safety for producers, transporters and users.

Description

Water soluble granule of chlorfenapyr and preparation method thereof
Technical field
The present invention relates to a kind of insecticide of novel form, relate in particular to a kind of water dissolvable granula that contains chlorfenapyr and preparation method thereof.
Background technology
Along with the raising of people to environmental protection consciousness; and national governments are to the attention of ecotope, people to be fit to controlling crop diseases and insect pests and nuisanceless production needs efficiently, the demand of low toxicity, low-residual, free of contamination environment protection biological agricultural chemicals and chemical pesticide is increasing.
Chlorfenapyr is the pyroles insecticidal/acaricidal agent of American Cyanamid Company exploitation, and chemical name is 4-bromo-2-(4-chlorphenyl)-1-ethoxyl methyl-5-trifluoromethyl pyrpole-3-nitrile, have another name called eliminate, capillary, hygron, AC303630 etc.This medical instrument have tag, stomach poison function, its mechanism of action uniqueness, lasting period is long, various pests on vegetables, cotton, fruit, the Soybean and Other Crops, evil mite there is preventive effect preferably, low to the person poultry toxicity, prove that through for many years field control effectiveness test chlorfenapyr is the good kind with application value and development prospect.
The kind of the insecticide that plant protection is used is a lot, and it is kind of formulation surplus missible oil, suspending agent, wetting powder, pulvis, granula, aqua, poison bait, mother liquor, the female powder etc. ten that various countries use maximum formulations at present.As everyone knows, contain a large amount of organic solvents in the missible oil, be easy to volatilization catch fire, toxic to human body and plant, contaminated environment, transportation is also inconvenient; Wetting powder has a large amount of dust in producing, using, contaminated environment influences operating personnel's health.Present stage, the developments of the formulations of pesticide mainly was to advocate exploitation environment-friendly type novel form, as: 1. liquid formulation trend Water-borne modification.Aqueous emulsion (EW), microemulsion (ME), aqueous suspension (SC), water dissolvable liquor (SL) etc. are representative Water-borne modification novel forms, its common feature is to replace a large amount of organic solvents with water, reduce the waste and the pollution of solvent, reduce preparation toxicity, improving safety, is the novel form that replaces missible oil.2. solid formulation spheroidizing.With the powderous preparations spheroidizing, avoid dust pollution, being convenient to pack also is the direction of dosage form research.Water-dispersible granules (WDG) is representative granular dose.This formulation, outward appearance is a graininess, drops into disintegration dispersion rapidly in the water during use, forms the dispersion of higher suspension, uses in order to spraying.Formulation content and suspensibility all substantially exceed the wettable granula, good fluidity, and no dust pollution, packing, storing are that the advantage of collection wetting powder, suspension emulsion, granule is the novel form of one conveniently.But these formulations all do not have both advantages are combined, and embody simultaneously.
Summary of the invention
Purpose of the present invention is exactly in order to overcome the shortcoming that above-mentioned prior art exists, provide a kind of and replace a large amount of organic solvents with water, reduce the waste and the pollution of solvent, reduce preparation toxicity, improve safety, outward appearance is a graininess, and that drops into during use in the water that disintegration rapidly disperses contains water dissolvable granula (WSG) of chlorfenapyr and preparation method thereof.
For solving the problems of the technologies described above, the present invention is achieved through the following technical solutions:
A kind of water soluble granule of chlorfenapyr, mainly make by the material of following percentage by weight:
Chlorfenapyr: 0.5~50%;
Emulsifier: 1~30%;
Dispersant: 1~10%;
Wetting agent: 1~5%;
Binding agent: 2~4%;
Stabilizing agent: 1~3%;
Surplus is a filler.
Water soluble granule of chlorfenapyr of the present invention, wherein said emulsifier are selected from one or both mixtures in alkylphenol polyoxyethylene, benzylphenol APEO and analog, fatty alcohol-polyoxyethylene ether and analog or Span and the ethylene oxide adduct thereof.
Described alkylphenol polyoxyethylene can be polyoxyethylene nonylphenol ether, OPEO etc.; Described benzylphenol APEO and analog can be benzylphenol APEO, benzyl alkylphenol polyoxyethylene etc.; Described fatty alcohol-polyoxyethylene ether and analog can be for being the products C of principal component with the laruyl alcohol nH 2n+1O (EO) mH, n=12~16 wherein, m=15~30; Described Span and ethylene oxide adduct thereof can be Span-20, Span-40, Span-60, Span-65, Span-80, Span-85 or Tween20, Tween21, Tween40, Tween60, Tween61, Tween65, Tween80, Tween81, Tween85 etc.
Water soluble granule of chlorfenapyr of the present invention, wherein said dispersant is selected from alkylnaphthalene sulfonate, two naphthalenesulfonate formaldehyde condensation compound or sodium lignin sulfonate.
Described alkylnaphthalene sulfonate can be for Nekal BX, draw back powder AC etc.; Described pair of naphthalenesulfonate formaldehyde condensation compound can be dispersant N, dispersant NNO etc.
Water soluble granule of chlorfenapyr of the present invention, wherein said wetting agent are selected from one or both mixtures in alkylbenzenesulfonate, fatty acid amide N-metilsulfate, the alkylaryl polyoxyethylene ether sulfate.
Water soluble granule of chlorfenapyr of the present invention, wherein said binding agent are selected from one or both mixtures in beta-schardinger dextrin-, polyvinyl alcohol, the methylcellulose.
Water soluble granule of chlorfenapyr of the present invention, wherein said stabilizing agent are selected from a kind of in Sodium Benzoate, the glucose.
Water soluble granule of chlorfenapyr of the present invention, wherein said filler are selected from one or both mixtures in bicarbonate, anhydrous citric acid, maltose, the anhydrous sodium sulfate.
The preparation method of water soluble granule of chlorfenapyr of the present invention is: described material is proportionally carried out homogeneous, kneading and extruder grain, and 65~75 ℃ of following vacuum dryings were sieved after 1~2 hour, and the product that sieves is the back packing after testing; The product of not crossing sieve repeats above step.
Its concrete preparation method may further comprise the steps:
1. homogeneous: the former medicine of chlorfenapyr and binding agent, wetting agent are mixed in 50~60 ℃ of water, in 420~450 kilograms per centimeter 2High pressure stirs homogeneous down;
2. the aforesaid liquid mixture behind the homogeneous is carried out atomized drying, make compound female medicine;
3. mediate: after the emulsifier heat of solution, mix with dispersant, stabilizing agent, filler and compound female medicine heat under 45~50 ℃ of temperature, again in 4~6 kilograms per centimeter 2Pressure stirs down, mediates evenly, the group's of obtaining agent;
4. extruder grain: will roll into a ball agent in 6~12 kilograms per centimeter 2Extrude into cylindrical particle under the pressure;
5. cylindrical particle is sieved shaping 70 ℃ of following vacuum dryings after 1 hour.
Water dissolvable granula of the present invention meets and replaces organic solvent, medicine shape solid particleization or tableted, agricultural chemicals high-loadization and four requirements of functionalization such as dimethylbenzene, methyl alcohol, toluene with aqueous solvent in the current agricultural chemicals development trend, wherein former medicine effect of the embedding of binding agent and stabilizing agent stablizes and antioxidation, the anti-width of cloth of former medicine is penetrated with the illumination ability improved, prolonged the medicine shelf-life; Bicarbonate in the filler and citric acid can play the effect of effervescent agent, promote the granula dissolving.Water dissolvable granula of the present invention can be dissolved in water fast, the dispersion rate height, nothing floats and sinkage, has with water to replace a large amount of organic solvents, reduces the waste and the pollution of solvent, reduce preparation toxicity, improve safety, outward appearance is a graininess, drops into disintegration dispersion rapidly in the water during use, transportation and keeping are convenient, the characteristics of long shelf-life, and its preparation method is simple, be easy to operate and control.
The present invention compares with existing main flow insecticide formulation, does not contain or only contain poisonous, inflammable on a small quantity aromatic hydrocarbon solvent, thus can avoid producing with transporting procedures in inflammable and explosive phenomenon.This formulation does not have unpleasant poisonous smell, and is little to eye irritation, reduced the pollution to environment, improved the safety to production, storing and user greatly.Therefore after forming industrialization, not only economic benefit is obvious, and helps promoting the development of high-new environment friendly agricultural technology, to promoting environmental protection, has obvious social, is the Research on Sustainable Development direction.
Embodiment
Below in conjunction with embodiment, the invention will be further described:
Embodiment 1
The preparation process of water soluble granule of chlorfenapyr:
1. get the raw materials ready: be ready to raw material by following prescription:
Chlorfenapyr: 1%;
Wang Ji phenol polyethenoxy ether: 3%;
Beta-schardinger dextrin-: 1%;
Neopelex: 5%;
Dispersant NNO:4%;
Sodium Benzoate: 1%;
Sodium bicarbonate: 47%;
Anhydrous citric acid: 38%;
2. the former medicine of chlorfenapyr and beta-schardinger dextrin-, neopelex are mixed in 55 ℃ of water, in 420 kilograms per centimeter 2High pressure stirs homogeneous down, and the aforesaid liquid mixture behind the homogeneous is carried out atomized drying, makes compound female medicine;
3. with after the heat of solution of Wang Ji phenol polyethenoxy ether, mix with dispersant NNO, Sodium Benzoate, sodium bicarbonate, anhydrous citric acid and compound female medicine heat under 45 ℃ of temperature, again in 6 kilograms per centimeter 2Pressure stirs down, mediates evenly, the group's of obtaining agent;
4. will roll into a ball agent in 8 kilograms per centimeter 2Extrude into cylindrical particle under the pressure;
5. cylindrical particle is sieved after 1 hour 70 ℃ of following vacuum dryings, the product that sieves is the back packing after testing; The product of not crossing sieve repeats after the above process after testing qualified packing again.
With above preparation, every mu is used 460g that brassicaceous vegetable insect beet armyworm, diamond-back moth are prevented and treated test, and preventive effect is good, and control efficiency sees Table 1:
Table 1
Figure A20088000007400071
Embodiment 2
Preparation process is with embodiment 1, and raw materials used prescription is:
Chlorfenapyr: 10%;
OPEO: 6%;
Benzylphenol APEO: 1%;
Sodium lignin sulfonate: 3%;
Fatty acid amide N-metilsulfate: 5%;
Methylcellulose: 2%;
Sodium Benzoate: 1%;
Sodium bicarbonate: 37%;
Anhydrous citric acid: 35%.
Use 46g that brassicaceous vegetable insect beet armyworm, diamond-back moth are prevented and treated test in every mu in this preparation, preventive effect is good, and control efficiency sees Table 2:
Table 2
Figure A20088000007400081
Embodiment 3
Preparation process is with embodiment 1, and raw materials used prescription is:
Chlorfenapyr: 30%;
OPEO: 10%;
Fatty alcohol-polyoxyethylene ether: 2%;
Dispersant N:4%;
Alkylaryl polyoxyethylene ether sulfate: 4%;
Polyvinyl alcohol: 2%;
Glucose: 1%;
Anhydrous sodium sulfate: 27%;
Anhydrous citric acid: 20%.
With this preparation, every mu is used 14g that brassicaceous vegetable insect beet armyworm, diamond-back moth are prevented and treated test, and preventive effect is good, and control efficiency sees Table 3:
Table 3
Figure A20088000007400082
Embodiment 4
Preparation process is with embodiment 1, and raw materials used prescription is:
Chlorfenapyr: 50%;
Span: 12%;
Draw back powder AC:3%;
Nekal BX: 1%;
Dodecyl sodium naphthalene sulfonate: 4%;
Polyvinyl alcohol: 2%;
Glucose: 1%;
Maltose: 15%;
Anhydrous citric acid: 12%.
Use 9g that brassicaceous vegetable insect beet armyworm, diamond-back moth are prevented and treated test in every mu in this preparation, preventive effect is good, and control efficiency sees Table 4:
Table 4
Figure A20088000007400091
Industrial applicibility
The present invention compares with existing main flow pesticide formulation, and do not contain or only contain on a small quantity poisonous, inflammable aromatic hydrocarbon solvent, thereby can To avoid the inflammable and explosive phenomenon in the producing and casting process. This formulation does not have unpleasant poisonous smell, and is little to eye irritation, Reduce the pollution to environment, greatly improved the security to production, storing and user. Therefore after forming industrialization, no Only economic benefit is obvious, and is conducive to promote the development of high-new environment friendly agricultural technology, to promoting environmental protection, has significantly Social benefit is the research direction of sustainable development.
Explanation to application documents: unless otherwise indicated, the percentage that relates in the present specification all is weight percentage.

Claims (11)

1. water soluble granule of chlorfenapyr is characterized in that: mainly made by the material of following percentage by weight:
Chlorfenapyr: 0.5~50%;
Emulsifier: 1~30%;
Dispersant: 1~10%;
Wetting agent: 1~5%;
Binding agent: 2~4%;
Stabilizing agent: 1~3%;
Surplus is a filler.
2. water soluble granule of chlorfenapyr as claimed in claim 1 is characterized in that described emulsifier is selected from one or both mixtures in alkylphenol polyoxyethylene, benzylphenol APEO and analog, fatty alcohol-polyoxyethylene ether and analog or Span and the ethylene oxide adduct thereof.
3. water soluble granule of chlorfenapyr as claimed in claim 2 is characterized in that described alkylphenol polyoxyethylene is polyoxyethylene nonylphenol ether, OPEO; Described benzylphenol APEO and analog are benzylphenol APEO, benzyl alkylphenol polyoxyethylene; Described fatty alcohol-polyoxyethylene ether and analog are for being the products C of principal component with the laruyl alcohol nH 2n+1O (EO) mH, n=12~16 wherein, m=15~30; Described Span and ethylene oxide adduct thereof are Span-20, Span-40, Span-60, Span-65, Span-80, Span-85 or Tween20, Tween21, Tween40, Tween60, Tween61, Tween65, Tween80, Tween81, Tween85.
4. water soluble granule of chlorfenapyr as claimed in claim 1 is characterized in that described dispersant is selected from alkylnaphthalene sulfonate, two naphthalenesulfonate formaldehyde condensation compound or sodium lignin sulfonate.
5. water soluble granule of chlorfenapyr as claimed in claim 4 is characterized in that described alkylnaphthalene sulfonate is Nekal BX, draws back powder AC; Described pair of naphthalenesulfonate formaldehyde condensation compound is dispersant N, dispersant NNO.
6. as each described water soluble granule of chlorfenapyr of claim 1~5, it is characterized in that described wetting agent is selected from one or both mixtures in alkylbenzenesulfonate, fatty acid amide N-metilsulfate, the alkylaryl polyoxyethylene ether sulfate.
7. water soluble granule of chlorfenapyr as claimed in claim 6 is characterized in that described binding agent is selected from one or both mixtures in beta-schardinger dextrin-, polyvinyl alcohol, the methylcellulose.
8. water soluble granule of chlorfenapyr as claimed in claim 7 is characterized in that described stabilizing agent is selected from a kind of in Sodium Benzoate, the glucose.
9. water soluble granule of chlorfenapyr as claimed in claim 8 is characterized in that described filler is selected from one or both mixtures in bicarbonate, anhydrous citric acid, maltose, the anhydrous sodium sulfate.
10. the preparation method of a water soluble granule of chlorfenapyr, it is characterized in that: described material is proportionally carried out homogeneous, kneading and extruder grain, and 65~75 ℃ of following vacuum dryings were sieved after 1~2 hour, and the product that sieves is the back packing after testing; The product of not crossing sieve repeats above step.
11. the preparation method of water soluble granule of chlorfenapyr according to claim 10 is characterized in that: may further comprise the steps:
1. homogeneous: the former medicine of chlorfenapyr and binding agent, wetting agent are mixed in 50~60 ℃ of water, in 420~450 kilograms per centimeter 2High pressure stirs homogeneous down;
2. the aforesaid liquid mixture behind the homogeneous is carried out atomized drying, make compound female medicine;
3. mediate: after the emulsifier heat of solution, mix with dispersant, stabilizing agent, filler and compound female medicine heat under 45~50 ℃ of temperature, again in 4~6 kilograms per centimeter 2Pressure stirs down, mediates evenly, the group's of obtaining agent;
4. extruder grain: will roll into a ball agent in 6~12 kilograms per centimeter 2Extrude into cylindrical particle under the pressure;
5. cylindrical particle is sieved shaping 70 ℃ of following vacuum dryings after 1 hour.
CNA2008800000748A 2008-01-09 2008-01-09 Water soluble granule of chlorfenapyr and its preparation Pending CN101568256A (en)

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102550588A (en) * 2011-12-22 2012-07-11 重庆大学 Method for preparing acetamiprid-containing water-soluble granules
CN104412963A (en) * 2013-08-29 2015-03-18 浙江新安化工集团股份有限公司 Agricultural auxiliary agent, granules and preparation method of agricultural auxiliary agent and granules
CN106614756A (en) * 2016-12-20 2017-05-10 陕西麦可罗生物科技有限公司 Preparation method of nikkomycin soluble granules
WO2018114409A1 (en) * 2016-12-19 2018-06-28 Basf Se High load granular dinotefuran formulation with reduced eye irritancy
CN111902043A (en) * 2018-04-13 2020-11-06 拜耳公司 Solid formulation of pesticidal mixtures

Family Cites Families (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1775027A (en) * 2005-11-21 2006-05-24 河北威远生物化工股份有限公司 Disinsection soluble granules containing methylamino avermection benzoate
CN100413414C (en) * 2006-04-19 2008-08-27 山东农业大学 Composite of insecticide and acaricide for mulberry tree without harmful to silkworm

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102550588A (en) * 2011-12-22 2012-07-11 重庆大学 Method for preparing acetamiprid-containing water-soluble granules
CN104412963A (en) * 2013-08-29 2015-03-18 浙江新安化工集团股份有限公司 Agricultural auxiliary agent, granules and preparation method of agricultural auxiliary agent and granules
WO2018114409A1 (en) * 2016-12-19 2018-06-28 Basf Se High load granular dinotefuran formulation with reduced eye irritancy
CN106614756A (en) * 2016-12-20 2017-05-10 陕西麦可罗生物科技有限公司 Preparation method of nikkomycin soluble granules
CN111902043A (en) * 2018-04-13 2020-11-06 拜耳公司 Solid formulation of pesticidal mixtures

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Application publication date: 20091028