CN104872170A - Efficient cyhalothrin methylamino abamectin benzoate microsphere water dispersible granules - Google Patents
Efficient cyhalothrin methylamino abamectin benzoate microsphere water dispersible granules Download PDFInfo
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Abstract
The invention relates to efficient cyhalothrin/methylamino abamectin benzoate microsphere water dispersible granules, which mainly consist of 50 percent to 80 percent of efficient cyhalothrin and methylamino abamectin benzoates, 1 percent to 5 percent of wetting agents, 3 percent to 10 percent of dispersing agents, 1 percent to 5 percent of disintegrating agents, 0.5 percent to 4 percent of bonding agents, 0 percent to 3 percent of defoaming agents and the balance carriers. The microsphere water dispersible granules can be applied to cauliflowers, cabbages, Chinese cabbages, cotton, soybean and the like, has the obvious effects on the prevention and the treatment of plutella xylostella, asparagus caterpillar, cabbage caterpillar and the like, and simultaneously has the advantages that the medicine effect is strong, the slow release effect is good, the photolysis is low, the effect preserving period is prolonged, the toxicity is low, the storage and the transportation are convenient, the environment is protected, and the like.
Description
Technical field
The invention belongs to the preparation field of pesticidal preparations, be specifically related to a kind of gamma cyhalothrin/emamectin-benzoate aqueous microsphere shot agent.
Background technology
Gamma cyhalothrin, English name is λ-Cyhalothrin, and chemical name is 3-(2-chloro-3,3,3 ,-trifluoropropene base)-2,2-dimethyl cyclopropane carboxylic acid's alpha-cyano-3-phenoxybenzyl ester.Gamma cyhalothrin belongs to never poison, act on periphery and the central nervous system of insect, it can suppress the conduction at insect neural axon position, changes neu to the permeability of ion, cause reignition by the cell that excites nerve and cause insect paralysis, having and knock down fast feature.The main effect model of gamma cyhalothrin is tagged and stomach toxicity, and biologically active is high, and insecticidal range is wide, effective to Lepidoptera, Semiptera, coleoptera, thrips, Hymenoptera, orthoptera, dipterous various pests.
Emamectin-benzoate (emamectin benzoate), English name is Emamectin benzoate, is usually called emamectin benzoate for short.It is a kind of antibiotic compound Avermectin being carried out chemical modification and obtains.Emamectin benzoate can strengthen the unstrung effect such as glutamic acid, γ-aminobutyric acid (GABA), causes a large amount of Cl
-enter in cell through cell membrane, cell various functions reduces, and neural regular event potential conductance is damaged, and causes poisoning insect larva to be benumbed, stops taking food.The main effect model of emamectin benzoate is stomach toxicity, there is action of contace poison simultaneously, there is very high biologically active, particularly prevent and treat splendid, as cotton bollworm, beet armyworm, diamond-back moth, tomato hawkmoth, cabbage heart snout moth's larva, colorado potato beetle, wild cabbage horizontal stripe snout moth's larva etc. to Lepidoptera and diptera class pest.Emamectin benzoate is as biogenic pesticide, and its safety is good, uses general in the production of green agricultural product.
Although gamma cyhalothrin and emamectin benzoate all belong to high activity agricultural chemicals, due to Irrational Use of Drugs, the resistance problem of two kinds of agricultural chemicals is also more and more serious, and dosage increases rapidly.Gamma cyhalothrin and emamectin benzoate are composite according to a certain percentage has obvious synergistic effect, thus reduces formulation rate, and delays drug-fast generation and further develop.The several gamma cyhalothrin occurred in the market and the complex preparation of emamectin benzoate are mainly aqueous emulsion, microemulsion, missible oil.Wherein cream preparation organic solvent content is higher, and in aqueous emulsion and microemulsion, emulsifier content is higher, have larger pollution, and these three kinds of formulations is liquid preparation to environment, is not easy to transport and storage, does not meet the developing direction of pesticidal preparations curable type.And these three kinds of dosage form product do not solve emamectin benzoate and to degrade fast shortcoming, and especially emamectin benzoate very easily photodissociation, if do not make microballoon protection, very easily has a strong impact on the lasting period of medicine because of photodissociation in field.In addition, at present other people institute's investigation and application be pesticide water dispersible granules or agricultural chemicals microballoon suspending agent.Water dispersible granules directly pesticide active ingredient is processed into water dispersible granules (for curable type agent type), and water dispersible granules directly can use (spraying after dilute with water) in production.But the shortcoming directly emamectin benzoate-chlorfenapyr active ingredient being processed into water dispersible granules is that dosage form of water dispersible granule can not solve the defect of the easy photodissociation of emamectin benzoate, if by agricultural chemicals (emamectin benzoate) as being wrapped in microballoon, be prepared into agricultural chemicals microballoon, the defect of the easy photodissociation of emamectin benzoate effectively can be solved; And agricultural chemicals (emamectin benzoate) microballoon also has slowly-releasing extends drug action, but agricultural chemicals microballoon directly can not use in production, need to be prepared into agricultural chemicals microballoon suspending agent (for liquid dosage form) and regenerative ratio directly could use (spraying after dilute with water), and agricultural chemicals microballoon suspending agent (for liquid dosage form) is not easy to transport and storage.Therefore, prepare the agent of agricultural chemicals aqueous microsphere shot and can solve the easy photodissociation defect of emamectin benzoate, and there is slowly-releasing prolongation drug action, meanwhile, again can spraying use after direct dilute with water in production.Pesticide active ingredient is first made the microballoon (being wrapped in microballoon by agricultural chemicals) having slowly-releasing He slow down degradation by the present invention, and then this microballoon is made the water dispersible granules of curable type.
Summary of the invention
The object of the invention is the deficiency for existing water dispersible granules, a kind of gamma cyhalothrin/emamectin-benzoate aqueous microsphere shot agent is provided.The aqueous microsphere shot agent that the present invention obtains, can improve drug effect, expands insecticidal spectrum, and having slow releasing function, extend drug effect, reduce photodissociation, not containing organic solvent, and is curable type chemical preparation, is convenient to transport storage and environmental protection low-residual.
The technical solution used in the present invention is as follows:
A kind of gamma cyhalothrin/emamectin-benzoate aqueous microsphere shot agent, each constituent mass percentages is: gamma cyhalothrin/emamectin-benzoate microballoon 50% ~ 80%, wetting agent 1% ~ 5%, dispersant 3% ~ 10%, disintegrant 1% ~ 5%, binding agent 0.5% ~ 4%, defoamer 0% ~ 3%, surplus are carrier.
Described gamma cyhalothrin/emamectin-benzoate aqueous microsphere shot agent, each component is preferably by mass percentage: gamma cyhalothrin/emamectin-benzoate microballoon 60% ~ 75%, wetting agent 2% ~ 4%, dispersant 4% ~ 8%, disintegrant 2% ~ 4%, binding agent 1% ~ 2.5%, defoamer 1% ~ 2%, surplus are carrier.
In described gamma cyhalothrin/emamectin-benzoate microballoon, gamma cyhalothrin and emamectin-benzoate mass ratio are 0.1 ~ 35:35 ~ 0.1, and core and wall material mass ratio are: 1:1 ~ 4; In emulsifier solution, emulsifier mass body volume concentrations is: 5 ~ 25 g/L.
In described gamma cyhalothrin/emamectin-benzoate microballoon, gamma cyhalothrin and emamectin-benzoate mass ratio are preferably 1 ~ 30:30 ~ 1; Core and wall material mass ratio are preferably: 1:2 ~ 3; In emulsifier solution, emulsifier mass body volume concentrations is preferably: 10 ~ 20 g/L.
Described wetting agent is lauryl sodium sulfate, pull open in powder, Terwet 1004, Morwet EFW one or more.
Described dispersant is one or more in sodium lignin sulfonate, NNO, Dispersant MF, Morwet D-425, Tersperse 2700.
Described disintegrant is one or more in sodium sulphate, ammonium sulfate, sodium chloride, aluminium chloride, urea.
Described binding agent is one or more in polyvinyl alcohol, polyethylene glycol, gum Arabic, carboxymethyl cellulose.
Described carrier is one or more in white carbon, bentonite, kaolin, diatomite.
Described defoamer is one or more in DF-66, DF-160, DF-1561.
Gamma cyhalothrin and the composite microballoon of emamectin benzoate, its preparation process is as follows:
To add in emulsifier aqueous solution with the consoluet gamma cyhalothrin that mixes according to a certain percentage of organic solvent and emamectin benzoate (core) and PLA (wall material), be stirred to organic solvent after high speed shear to volatilize completely, then suction filtration, drying, collects microsphere powder.
Described organic solvent is one or more in carrene, chloroform, acetone, ether.
Described emulsifier is one or more in gelatin, gum Arabic, polyvinyl alcohol, sodium carboxymethylcellulose.
Described gamma cyhalothrin and emamectin benzoate microballoon are prepare under best composition mass ratio, and the theoretical drugloading rate of microballoon (active ingredient gross mass accounts for microspheres quality percentage, is determined by core wall material ratio) is 25.0% ~ 33.3%.
Gamma cyhalothrin and emamectin benzoate composite aqueous microsphere shot agent preparation method as follows:
Each composition comprises by mass percentage: gamma cyhalothrin and the composite microballoon 50% ~ 80% of emamectin benzoate, wetting agent 1% ~ 5%, dispersant 5% ~ 12%, disintegrant 1% ~ 5%, binding agent 0.5% ~ 4%, defoamer 0% ~ 3%, surplus are carrier; Pulverize with airslide disintegrating mill after all the components is fully mixed, adopt the granulation of rotary table granulation method, through super-dry.Screening obtains the agent of aqueous microsphere shot.
The present invention has the following advantages compared with the prior art:
(1) composite microballoon is mixed with water dispersible granules by the present invention, and not containing organic solvent in preparation, endanger little to environment and operator in production and use procedure, safety is good, and owing to being that molecule preparation is convenient to transport and storage;
(2) composite microballoon is mixed with water dispersible granules by the present invention, not only overcome emamectin benzoate easy photodissociation when directly emamectin benzoate-chlorfenapyr active ingredient being processed into water dispersible granules and cause the unabiding defect of pesticide efficacy, and the shortcoming that the composite microballoon of emamectin benzoate directly can not use on producing; Obtain a kind of aqueous microsphere shot agent used of can spraying after direct dilute with water on producing, possess outstanding progress;
(3) aqueous microsphere shot footpath obtained by the present invention, when the composite mass ratio of gamma cyhalothrin and emamectin benzoate is identical, compared with tieing up high chlorine fluorine aqueous emulsion with commercially available first, calculate compound water dispersible granule according to the abundant co-toxicity coefficient method of Sun Yun and be far longer than 120 relative to the co-toxicity coefficient of aqueous emulsion, there is obvious synergistic effect.
Embodiment
By embodiment, the present invention will be further described, but the present invention not limited by following examples.
embodiment 1
Gamma cyhalothrin and emamectin benzoate total content are the water dispersible granules of 5wt%
Gamma cyhalothrin and emamectin benzoate are mixed according to mass ratio 4:1, core and the wall material that mass ratio is 1:3 is dissolved with carrene, core wall material solution is joined in the polyvinyl alcohol water solution of mass body volume concentrations 10 g/L, be stirred to organic solvent after high speed shear to volatilize completely, then suction filtration, drying, collects microsphere powder.Microballoon drugloading rate is 23.5% after measured, i.e. active ingredient gross mass about 23.5 grams in every hectogram microballoon, and condition and a batch difference are prepared the actual drugloading rate of thus obtained microsphere and had minute differences.
Take raw material components (mass percent): gamma cyhalothrin and the composite microballoon of emamectin benzoate about 21.3%, wetting agent Terwet 1,004 2%, dispersant Tersperse 2,700 4%, disintegrant sodium sulphate 3%, binding agent polyvinyl alcohol 1.5%, defoamer DF-66 1%, kaolin polishing.Pulverize with airslide disintegrating mill after all the components is fully mixed, adopt the granulation of rotary table granulation method, through super-dry.Screening obtains the agent of aqueous microsphere shot.Adopt leaching leaf feeding method pair: 1) the 5% gamma cyhalothrin emamectin benzoate aqueous microsphere shot agent (gamma cyhalothrin and emamectin benzoate mass ratio 4:1), 2 of the present embodiment) 5% commercially available first ties up high chlorine fluorine aqueous emulsion (gamma cyhalothrin and emamectin benzoate mass ratio 4:1), 3) commercially available 5.0% gamma cyhalothrin microemulsion, 4) 4 kinds of preparations such as commercially available 1.5% emamectin-benzoate missible oil have carried out Toxicity Determination, calculate LC according to the lethality after 48h
50value, four kinds of preparations are to the LC of diamond-back moth
50be respectively 18.22,17.96,160.0,6.345 mg/L, as can be seen from toxicity test result: when the composite mass ratio of gamma cyhalothrin and emamectin benzoate is identical, it is close that formulation products of the present invention and commercially available 5% first tie up the indoor virulence of high chlorine fluorine aqueous emulsion to diamond-back moth, calculating compound water dispersible granule relative to the co-toxicity coefficient of two kinds of single doses according to the abundant co-toxicity coefficient method of Sun Yun is 150.3, has obvious synergistic effect.
embodiment 2
Gamma cyhalothrin and emamectin benzoate total content are the water dispersible granules of 10wt%
Gamma cyhalothrin and emamectin benzoate are mixed according to mass ratio 10:1, core and the wall material that mass ratio is 1:3 is dissolved with chloroform, core wall material solution is joined in the gum Arabic aqueous solution of mass body volume concentrations 10 g/L, be stirred to organic solvent after high speed shear to volatilize completely, then suction filtration, drying, collects microsphere powder.Microballoon drugloading rate is about 23.0% after measured, i.e. active ingredient gross mass 23.0 grams in every hectogram microballoon, and condition and a batch difference are prepared the actual drugloading rate of thus obtained microsphere and had minute differences.
Take raw material components (mass percent): gamma cyhalothrin and the composite microballoon 43.5% of emamectin benzoate, wetting agent lauryl sodium sulfate 3%, dispersant NNO 6%, disintegrant ammonium sulfate 3%, binding agent gum Arabic 2%, defoamer DF-160 1.5%, diatomite polishing.Pulverize with airslide disintegrating mill after all the components is fully mixed, adopt the granulation of rotary table granulation method, through super-dry.Screening obtains the agent of aqueous microsphere shot.Adopt leaching leaf feeding method to carry out Toxicity Determination to the present embodiment, record the LC of the present embodiment to diamond-back moth
50be 32.55 mg/L, co-toxicity coefficient is 153.5, has notable synergistic effect.
embodiment 3
Gamma cyhalothrin and emamectin benzoate total content are the water dispersible granules of 15wt%
Gamma cyhalothrin and emamectin benzoate are mixed according to mass ratio 2:3, with core and wall material that ether dissolution mass ratio is 1:3, core wall material solution is joined in gelatin-gum arabic (mass ratio 1:1) aqueous solution of mass body volume concentrations 10 g/L, be stirred to organic solvent after high speed shear to volatilize completely, then suction filtration, drying, collects microsphere powder.Microballoon drugloading rate is about 23.3% after measured, i.e. active ingredient gross mass 23.3 grams in every hectogram microballoon, and condition and a batch difference are prepared the actual drugloading rate of thus obtained microsphere and had minute differences.
Take raw material components (mass percent): gamma cyhalothrin and the composite microballoon 64.4% of emamectin benzoate, wetting agent Morwet EFW 4%, dispersant Morwet D-425 8%, disintegrant urea 3%, binding agent gum Arabic 2%, defoamer DF-1561 2%, white carbon polishing.Pulverize with airslide disintegrating mill after all the components is fully mixed, adopt the granulation of rotary table granulation method, through super-dry.Screening obtains the agent of aqueous microsphere shot.Adopt leaching leaf feeding method to carry out Toxicity Determination to the present embodiment, record the LC of the present embodiment to diamond-back moth
50be 8.02 mg/L, co-toxicity coefficient is 128.5, has notable synergistic effect.
embodiment 4
Gamma cyhalothrin and emamectin benzoate total content are the water dispersible granules of 20wt%
Gamma cyhalothrin and emamectin benzoate are mixed according to mass ratio 5:1, core and the wall material that mass ratio is 1:2 is dissolved with carrene, core wall material solution is joined in the aqueous gelatin solution of mass body volume concentrations 20 g/L, be stirred to organic solvent after high speed shear to volatilize completely, then suction filtration, drying, collects microsphere powder.Microballoon drugloading rate is about 31.5% after measured, i.e. active ingredient gross mass 31.5 grams in every hectogram microballoon, and condition and a batch difference are prepared the actual drugloading rate of thus obtained microsphere and had minute differences.
Take raw material components (mass percent): gamma cyhalothrin and the composite microballoon 63.5% of emamectin benzoate, wetting agent pulls open powder 4%, dispersant sodium lignin sulfonate-NNO(mass ratio 1:1) 7%, disintegrant aluminium chloride 3%, binding agent carboxymethyl cellulose 1.5%, defoamer DF-160 2%, bentonite polishing.Pulverize with airslide disintegrating mill after all the components is fully mixed, adopt the granulation of rotary table granulation method, through super-dry.Screening obtains the agent of aqueous microsphere shot.Adopt leaching leaf feeding method to carry out Toxicity Determination to the present embodiment, record the LC of the present embodiment to diamond-back moth
50be 22.07 mg/L, co-toxicity coefficient is 143.9, has notable synergistic effect.
The foregoing is only preferred embodiment of the present invention, all equalizations done according to the present patent application the scope of the claims change and modify, and all should belong to covering scope of the present invention.
Claims (10)
1. gamma cyhalothrin/emamectin-benzoate aqueous microsphere shot agent, is characterized in that: in the agent of aqueous microsphere shot, each constituent mass percentages is: gamma cyhalothrin/emamectin-benzoate microballoon 50% ~ 80%, wetting agent 1% ~ 5%, dispersant 3% ~ 10%, disintegrant 1% ~ 5%, binding agent 0.5% ~ 4%, defoamer 0% ~ 3%, surplus are carrier.
2. gamma cyhalothrin according to claim 1/emamectin-benzoate aqueous microsphere shot agent, is characterized in that: in the agent of aqueous microsphere shot, each component is by mass percentage: gamma cyhalothrin/emamectin-benzoate microballoon 60% ~ 75%, wetting agent 2% ~ 4%, dispersant 4% ~ 8%, disintegrant 2% ~ 4%, binding agent 1% ~ 2.5%, defoamer 1% ~ 2%, surplus are carrier.
3. gamma cyhalothrin according to claim 1 and 2/emamectin-benzoate aqueous microsphere shot agent, it is characterized in that: in described gamma cyhalothrin/emamectin-benzoate microballoon, gamma cyhalothrin and emamectin-benzoate mass ratio are 0.1 ~ 35:35 ~ 0.1, and core and wall material mass ratio are: 1:1 ~ 4; In emulsifier solution, emulsifier mass body volume concentrations is: 5 ~ 25 g/L.
4. gamma cyhalothrin according to claim 3/emamectin-benzoate aqueous microsphere shot agent, it is characterized in that: in described gamma cyhalothrin/emamectin-benzoate microballoon, gamma cyhalothrin and emamectin-benzoate mass ratio are 1 ~ 30:30 ~ 1; Core and wall material mass ratio are: 1:2 ~ 3; In emulsifier solution, emulsifier mass body volume concentrations is: 10 ~ 20 g/L.
5. the gamma cyhalothrin according to claims 1 or 2/emamectin-benzoate aqueous microsphere shot agent, is characterized in that: described wetting agent is lauryl sodium sulfate, pull open in powder, Terwet 1004, Morwet EFW one or more.
6. the gamma cyhalothrin according to claims 1 or 2/emamectin-benzoate aqueous microsphere shot agent, is characterized in that: described dispersant is one or more in sodium lignin sulfonate, NNO, Dispersant MF, Morwet D-425, Tersperse 2700.
7. the gamma cyhalothrin according to claims 1 or 2/emamectin-benzoate aqueous microsphere shot agent, is characterized in that: described disintegrant is one or more in sodium sulphate, ammonium sulfate, sodium chloride, aluminium chloride, urea.
8. the gamma cyhalothrin according to claims 1 or 2/emamectin-benzoate aqueous microsphere shot agent, is characterized in that: described binding agent is one or more in polyvinyl alcohol, polyethylene glycol, gum Arabic, carboxymethyl cellulose.
9. the gamma cyhalothrin according to claims 1 or 2/emamectin-benzoate aqueous microsphere shot agent, is characterized in that: described carrier is one or more in white carbon, bentonite, kaolin, diatomite.
10. the gamma cyhalothrin according to claims 1 or 2/emamectin-benzoate aqueous microsphere shot agent, is characterized in that: described defoamer is one or more in DF-66, DF-160, DF-1561.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2021093266A1 (en) * | 2019-11-11 | 2021-05-20 | 南京华洲药业有限公司 | Compound insecticidal and acaricidal nano aqueous formulation containing lambda-cyhalothrin and emamectin benzoate, and use thereof |
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| CN101720777A (en) * | 2009-12-06 | 2010-06-09 | 山西科锋农业科技有限公司 | Emamectin benzoate and efficient cyfluthrin pesticide mixture preparation |
| CN102696640A (en) * | 2012-06-15 | 2012-10-03 | 福建农林大学 | Emamectin benzoate polylactic acid microsphere suspension and preparation method thereof |
| CN103798232A (en) * | 2012-11-14 | 2014-05-21 | 中国农业科学院植物保护研究所 | Emamectin benzoate microsphere and preparation method thereof |
| CN103828801A (en) * | 2014-01-15 | 2014-06-04 | 福建农林大学 | Spinosyn/emamectin benzoate microsphere and preparation method thereof |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101720777A (en) * | 2009-12-06 | 2010-06-09 | 山西科锋农业科技有限公司 | Emamectin benzoate and efficient cyfluthrin pesticide mixture preparation |
| CN102696640A (en) * | 2012-06-15 | 2012-10-03 | 福建农林大学 | Emamectin benzoate polylactic acid microsphere suspension and preparation method thereof |
| CN103798232A (en) * | 2012-11-14 | 2014-05-21 | 中国农业科学院植物保护研究所 | Emamectin benzoate microsphere and preparation method thereof |
| CN103828801A (en) * | 2014-01-15 | 2014-06-04 | 福建农林大学 | Spinosyn/emamectin benzoate microsphere and preparation method thereof |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2021093266A1 (en) * | 2019-11-11 | 2021-05-20 | 南京华洲药业有限公司 | Compound insecticidal and acaricidal nano aqueous formulation containing lambda-cyhalothrin and emamectin benzoate, and use thereof |
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