CN103098799A - Pymetrozine-azone suspension emulsion and preparation method thereof - Google Patents

Pymetrozine-azone suspension emulsion and preparation method thereof Download PDF

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CN103098799A
CN103098799A CN2013100404458A CN201310040445A CN103098799A CN 103098799 A CN103098799 A CN 103098799A CN 2013100404458 A CN2013100404458 A CN 2013100404458A CN 201310040445 A CN201310040445 A CN 201310040445A CN 103098799 A CN103098799 A CN 103098799A
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azone
pymetrozine
agent
suspended emulsion
emulsion
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CN103098799B (en
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杨勇林
彭述明
周斌
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Sichuan Woye agrochemical Co. Ltd.
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Guangdong Zhongxun Agri Science Corp
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Abstract

The invention relates to a pymetrozine-azone suspension emulsion and a preparation method thereof. The pymetrozine-azone suspension emulsion comprises the following components in percentage by weight: 1-50% of pymetrozine, 1-20% of azone, 1-15% of solvent, 1-10% of emulsifier, 1-10% of wetting agent, 0.1-2% of thickening agent, 1-10% of antifreezing agent, 0.1-1% of defoamer, 0.1-0.5% of preservative, 0.1-1% of pH regulator, and the balance of de-ionized water. The azone is dissolved in a solvent and then the emulsifier and the de-ionized water are orderly added to the solution to obtain azone emulsion in water. After the pymetrozine, the wetting agent, the deformer, the antifreezing agent and the left de-ionized water are formed into grains, the azone emulsion in water, the thickening agent and the pH regulator are added for blending and shearing. The pymetrozine-azone suspension emulsion is high in flashing point, not easy to burn and explode, safe for production, storage and use, low in environmental pollution, low in product cost, easy to package and the like.

Description

Pymetrozine and azone suspended emulsion and preparation method thereof
Technical field
The invention belongs to pesticide field, be specifically related to a kind of pymetrozine and azone suspended emulsion and preparation method thereof.
Background technology
Pymetrozine, chemical name: 4,5~dihydro~6~methyl~4~(3~pyridine methylene is amino)~1,2,4~3 (2H)~ketone, belonging to pyridines or Triazinone insecticide, is the brand-new non-insects agent of killing livestock, and the sucking pest of various crop is shown the control efficiency of excellence.As long as aphid or plant hopper one touch pymetrozine and almost produce immediately the lancet blocking effect, stop at once taking food, and final hungry lethal, and this process is irreversible.Pymetrozine has action of contace poison to insect, also has simultaneously systemic activity.
Azone, chemical name: 1~dodecyl-aza-cycloheptane alkane~2~ketone; N~lauryl azepan~2~ketone; N~lauryl caprolactam.Azone can promote insecticide to the infiltration of polypide, promote weed killer herbicide to the infiltration of weeds, wetting plant leaf surface, promote plant to the absorption of medicine, therefore azone can be used in the medicines such as Insecticides (tech) ﹠ Herbicides (tech), plant growth regulator, improve the effect of effective ingredient and reduce drug dose, thereby reducing agricultural chemicals to the pollution of environment, except low use cost.
Summary of the invention
The object of the present invention is to provide a kind of stable performance, suspensibility is high, the suspended emulsion that the pymetrozine of reliable in quality and azone are composite.
Technical scheme: a kind of pymetrozine and azone suspended emulsion, each weight percentages of components is: pymetrozine 1%~50%, azone 1~20%, solvent 1%~15%, emulsifier 1%~10%, wetting agent 1%~10%, thickener 0.1%~2%, antifreezing agent 1%~10%, defoamer 0.1%~1%, preservative 0.1%~0.5%, pH adjusting agent 0.1~1%, surplus are deionized water.
Described emulsifier is selected sodium lignin sulfonate, lignin calcium iodate, polycarboxylic acid salt, lauryl alcohol polyethylene glycol oxide base ether sodium sulfate, alkyl naphthalene formaldehyde condensate sulfonates, lauryl sodium sulfate, the oleic acid salt, the mixing of one or more in alkyl polyoxyethylene ether sulfonate, alkylphenol-polyethenoxy base ether formaldehyde condensation products, polyoxyethylene polyoxypropylene base ether block copolymers, alkylpolyoxyethylene phosphate or alkyl naphthalene formaldehyde condensate sulfonates.
Described wetting agent is selected neopelex, is pulled open powder, one or more the mixing in SOPA, alkylphenol-polyethenoxy base ether Nonyl pheno base ether, detergent, emulsifier 2000 series, the fast T of wetting and penetrating agent.
Described thickener is selected one or both mixing in water-soluble resin, xanthans, carboxymethyl cellulose, carboxyethyl cellulose, methylcellulose, hydrated SiO 2, bentonite, polyvinyl alcohol, polyvinyl alcohol.
Described antifreezing agent is selected a kind of in ethylene glycol, propane diols, glycerine, urea.
Described defoamer is selected silicone oil, organic silicone, C 10~C 20Saturated fat acid compounds, C 8~C 10The aliphatic alcohols compound in a kind of.
Described preservative is selected a kind of in potassium sorbate, sodium sorbate, Sodium Benzoate, Kathon CG KF88.
Described pH adjusting agent is selected sodium hydroxide.One or more in ammoniacal liquor, acetic acid, citric acid or phosphoric acid.
Described solvent is methyl alcohol, dimethylbenzene, loose base oil, one or more in ethanol, ether, acetone, benzene, cyclohexane, cyclohexanone.
The preparation method of above-mentioned pymetrozine and azone suspended emulsion comprises the steps:
1, use by a certain percentage the dissolution with solvents azone, then add emulsifier, add appropriate amount of deionized water to make the aqueous emulsion of azone under shear conditions;
2, pymetrozine, wetting agent, defoamer, antifreezing agent and suitable quantity of water shear-mixed is even, the percentage that each component accounts for gross mass is: pymetrozine content 1%~50%, emulsifier 1%~10%, wetting agent 1%~10%, antifreezing agent 1%~10%, defoamer 0.1%~1%, preservative 0.1%~0.5%;
3, step 2 mixture is passed through the sand mill sand milling 4~6 times, require 90% particle diameter<=5um;
4, load weighted thickener and the ready-made azone aqueous emulsion of step 1 are added, shear-mixed is even more at last;
5, add at last pH adjusting agent, the pH value is adjusted between 6~8.
In recent years, due to the enhancing of people's environmental consciousness, make the green pesticide forms such as suspending agent have gradually and will replace the trend of the non-green pesticide form such as missible oil, pulvis in the past, agricultural chemicals new component newly developed goes on the market mainly with suspending agent greatly in recent years.And its particle diameter is little, and suspensibility is high, has at crop leaf the adhesivity that height is being opened up, and improves a lot than conventional dosage forms on drug effect.
The present invention is scattered in the particle of pymetrozine with miniaturization in water, has following advantage.
1, product cost is low, easily packing.
2, take water as matrix, without dust, environmental pollution is little, to producing and user's safety.
3, water baseization product, flash-point is high, does not fire not quick-friedly, produce to store safety.
4, after the said preparation spraying, be distributed in crop surface with fine particle, good disinsection effect.
Specific embodiments
In order to make purpose of the present invention, technical scheme and advantage more short and sweet, the present invention describes with following specific embodiment, but the present invention only limits to absolutely not these examples.The following stated is only the present invention embodiment preferably, only is used for describing the present invention, can not be interpreted as the restriction to scope of the present invention.Should be pointed out that all any modifications of making within the spirit and principles in the present invention, be equal to replacement and improvement etc., within all should being included in protection scope of the present invention.Therefore, the protection domain of patent of the present invention should be as the criterion with claims.
In these embodiments, unless otherwise indicated, all percentages all are weight percentage.
Embodiment 1:
At first each component of weighing: pymetrozine 5%, azone 1%, emulsifier lauryl alcohol polyethylene glycol oxide base ether sodium sulfate 3%, wetting agent alkylphenol-polyethenoxy base ether 3%, thickener xanthans 0.3%, antifreeze glycol 5%, defoamer organic silicone 0.4%, preservative Kathon CG KF88 0.1%, it is 6~8 that pH adjusting agent is regulated the pH value, solvent 5% adds deionized water to 100%.Then azone dissolution with solvents in first filling a prescription adds emulsifier and appropriate amount of deionized water, makes the aqueous emulsion of azone under shear conditions; Again pymetrozine and wetting agent, preservative, deionized water etc. are mixed rear sand milling to qualified particle diameter, add at last load weighted thickener and azone aqueous emulsion, pH adjusting agent to shear and evenly namely get 6% pymetrozine azone suspended emulsion.
Embodiment 2:
At first each component of weighing: pymetrozine 10%, azone 3%, emulsifier polycarboxylic acid salt 2.5%, wetting agent SOPA3%, thickener Magnesiumaluminumsilicate 1%, antifreeze glycol 5%, defoamer organic silicone 0.4%, preservative Kathon CG KF88 0.1%, it is 6~8 that pH adjusting agent is regulated the pH value, solvent 5% adds deionized water to 100%.Then azone dissolution with solvents in first filling a prescription adds emulsifier and appropriate amount of deionized water, makes the aqueous emulsion of azone under shear conditions; Again pymetrozine and wetting agent, preservative, deionized water etc. are mixed rear sand milling to qualified particle diameter, add at last load weighted thickener and azone aqueous emulsion, pH adjusting agent to shear and evenly namely get 13% pymetrozine azone suspended emulsion.
Embodiment 3:
At first each component of weighing: pymetrozine 15%, azone 3%, emulsifier lauryl alcohol polyethylene glycol oxide base ether sodium sulfate 3%, wetting agent Nonyl pheno base ether 3%, thickener Magnesiumaluminumsilicate 1.3%, antifreeze glycol 5%, defoamer organic silicone 0.4%, preservative Kathon CG KF88 0.1%, it is 6~8 that pH adjusting agent is regulated the pH value, solvent 5% adds deionized water to 100%.Then azone dissolution with solvents in first filling a prescription adds emulsifier and appropriate amount of deionized water, makes the aqueous emulsion of azone under shear conditions; Again pymetrozine and wetting agent, preservative, deionized water etc. are mixed rear sand milling to qualified particle diameter, add at last load weighted thickener and azone aqueous emulsion, pH adjusting agent to shear and evenly namely get 18% pymetrozine azone suspended emulsion.
Embodiment 4:
At first each component of weighing: pymetrozine 30%, azone 5%, emulsifier alkylpolyoxyethylene phosphate 4%, the fast T 2% of wetting agent wetting and penetrating agent, thickener xanthans 0.15%, antifreeze glycol 5%, defoamer organic silicone 0.4%, preservative Kathon CG KF88 0.1%, it is 6~8 that pH adjusting agent is regulated pH, solvent 5% adds deionized water to 100%.Then azone dissolution with solvents in first filling a prescription adds emulsifier and appropriate amount of deionized water, makes the aqueous emulsion of azone under shear conditions; Again pymetrozine and wetting agent, preservative, deionized water etc. are mixed rear sand milling to qualified particle diameter, add at last load weighted thickener and azone aqueous emulsion, pH adjusting agent to shear and evenly namely get 35% pymetrozine azone suspended emulsion.
Embodiment 5:
At first each component of weighing: pymetrozine 50%, azone 5%, emulsifier polycarboxylate 4.5%, the fast T 1% of wetting agent wetting and penetrating agent, thickener xanthans 0.1%, antifreeze glycol 5%, defoamer organic silicone 0.4%, preservative Kathon CG KF88 0.1%, it is 6~8 that pH adjusting agent is regulated the pH value, solvent 5% adds deionized water to 100%.Then azone dissolution with solvents in first filling a prescription adds emulsifier and appropriate amount of deionized water, makes the aqueous emulsion of azone under shear conditions; Again pymetrozine and wetting agent, preservative, deionized water etc. are mixed rear sand milling to qualified particle diameter, add at last load weighted thickener and azone aqueous emulsion, pH adjusting agent to shear and evenly namely get 55% pymetrozine azone suspended emulsion.
Embodiment 6: the field control effectiveness test contrast.
Use 18% pymetrozine azone suspended emulsion (embodiment 3) of the present invention, 35% pymetrozine azone suspended emulsion (embodiment 4), be used for the control water rice hopper.Adopt 25% pymetrozine wetting powder medicament in contrast, be watered spray pesticide in the water rice hopper nymph phase of starting, result of the test sees Table 1.
Figure 559277DEST_PATH_IMAGE001
Can find out by result of the test, in the situation that the pymetrozine usage amount is identical, pymetrozine of the present invention and azone suspended emulsion obviously are better than 25% pymetrozine wetting powder to the control efficiency of water rice hopper, illustrate that the present invention can improve the availability of pymetrozine, reduce the waste of pesticide active ingredient, reduce agricultural chemicals to the adverse effect of environmental ecology.

Claims (10)

1. a pymetrozine and azone suspended emulsion, it is characterized in that: each weight percentages of components is: pymetrozine 1%~50%, azone 1~20%, solvent 1%~15%, emulsifier 1%~10%, wetting agent 1%~10%, thickener 0.1%~2%, antifreezing agent 1%~10%, defoamer 0.1%~1%, preservative 0.1%~0.5%, pH adjusting agent 0.1~1%, surplus are deionized water.
2. pymetrozine according to claim 1 and azone suspended emulsion, it is characterized in that: described emulsifier is selected sodium lignin sulfonate, lignin calcium iodate, polycarboxylic acid salt, lauryl alcohol polyethylene glycol oxide base ether sodium sulfate, alkyl naphthalene formaldehyde condensate sulfonates, lauryl sodium sulfate, the oleic acid salt, the mixing of one or more in alkyl polyoxyethylene ether sulfonate, alkylphenol-polyethenoxy base ether formaldehyde condensation products, polyoxyethylene polyoxypropylene base ether block copolymers, alkylpolyoxyethylene phosphate or alkyl naphthalene formaldehyde condensate sulfonates.
3. pymetrozine according to claim 1 and azone suspended emulsion is characterized in that: described wetting agent is selected neopelex, is pulled open powder, one or more the mixing in SOPA, alkylphenol-polyethenoxy base ether Nonyl pheno base ether, detergent, emulsifier 2000 series, the fast T of wetting and penetrating agent.
4. pymetrozine according to claim 1 and azone suspended emulsion, it is characterized in that: described thickener is selected one or both mixing in water-soluble resin, xanthans, carboxymethyl cellulose, carboxyethyl cellulose, methylcellulose, hydrated SiO 2, bentonite, polyvinyl alcohol, polyvinyl alcohol.
5. pymetrozine according to claim 1 and azone suspended emulsion is characterized in that: described antifreezing agent is selected a kind of in ethylene glycol, propane diols, glycerine, urea.
6. pymetrozine according to claim 1 and azone suspended emulsion, it is characterized in that: described defoamer is selected silicone oil, organic silicone, C 10~C 20Saturated fat acid compounds, C 8~C 10The aliphatic alcohols compound in a kind of.
7. pymetrozine according to claim 1 and azone suspended emulsion is characterized in that: described preservative is selected a kind of in potassium sorbate, sodium sorbate, Sodium Benzoate, Kathon CG KF88.
8. pymetrozine according to claim 1 and azone suspended emulsion, it is characterized in that: described pH adjusting agent is selected one or more in sodium hydroxide, ammoniacal liquor, acetic acid, citric acid or phosphoric acid.
9. pymetrozine according to claim 1 and azone suspended emulsion, it is characterized in that: described solvent is methyl alcohol, dimethylbenzene, loose base oil, one or more in ethanol, ether, acetone, benzene, cyclohexane, cyclohexanone.
10. a pymetrozine and azone suspended emulsion its preparation method, it is characterized in that: first use by a certain percentage the dissolution with solvents azone, then add successively emulsifier, appropriate amount of deionized water, obtain the azone aqueous emulsion under shear conditions, the good pymetrozine of weighing according to the above ratio again, wetting agent, defoamer, carry out shear-mixed in antifreezing agent and surplus deionized water input stirred tank even, then pass into sand mill and carry out sand milling, sand milling is to qualified particle diameter, add at last the azone aqueous emulsion, thickener and pH adjusting agent are allocated, shear, namely obtain pymetrozine of the present invention and azone suspended emulsion.
CN201310040445.8A 2013-02-02 2013-02-02 Pymetrozine and azone suspended emulsion and preparation method thereof Active CN103098799B (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104872172A (en) * 2015-06-16 2015-09-02 山东省农业科学院植物保护研究所 Compound pesticide capable of preventing and treating green plant bug and preparation method of compound pesticide
CN112293412A (en) * 2020-11-02 2021-02-02 吉林省农业科学院 Pesticide synergist and preparation method and application thereof

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2000068222A2 (en) * 1999-05-12 2000-11-16 Syngenta Participations Ag Solvates of pymetrozine
CN101077071A (en) * 2007-06-14 2007-11-28 盐城双宁农化有限公司 Insecticidal composition for preventing and controlling plant hopper
CN102334510A (en) * 2011-11-09 2012-02-01 中化蓝天集团有限公司 Suspoemulsion compounded from Pymetrozine and Chlorpyrifos
CN102696629A (en) * 2012-05-14 2012-10-03 安徽省化工研究院 Functional pymetrozine insecticide and preparation method thereof

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2000068222A2 (en) * 1999-05-12 2000-11-16 Syngenta Participations Ag Solvates of pymetrozine
CN101077071A (en) * 2007-06-14 2007-11-28 盐城双宁农化有限公司 Insecticidal composition for preventing and controlling plant hopper
CN102334510A (en) * 2011-11-09 2012-02-01 中化蓝天集团有限公司 Suspoemulsion compounded from Pymetrozine and Chlorpyrifos
CN102696629A (en) * 2012-05-14 2012-10-03 安徽省化工研究院 Functional pymetrozine insecticide and preparation method thereof

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104872172A (en) * 2015-06-16 2015-09-02 山东省农业科学院植物保护研究所 Compound pesticide capable of preventing and treating green plant bug and preparation method of compound pesticide
CN112293412A (en) * 2020-11-02 2021-02-02 吉林省农业科学院 Pesticide synergist and preparation method and application thereof

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Effective date of registration: 20161027

Address after: 610300 No. 16, Golden Road, Industrial Development Zone, Qingbaijiang District, Sichuan, Chengdu

Patentee after: Sichuan Woye agrochemical Co. Ltd.

Address before: 516000 Guangdong province Huizhou Zhongkai hi tech Development Zone No. 24 District

Patentee before: Guangdong Zhongxun Agricultural Technology Co., Ltd.