CN101069506A - Pymetrozine suspension agent and preparation method - Google Patents

Pymetrozine suspension agent and preparation method Download PDF

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Publication number
CN101069506A
CN101069506A CN 200710024513 CN200710024513A CN101069506A CN 101069506 A CN101069506 A CN 101069506A CN 200710024513 CN200710024513 CN 200710024513 CN 200710024513 A CN200710024513 A CN 200710024513A CN 101069506 A CN101069506 A CN 101069506A
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agent
suspending agent
ether
sodium
agent according
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CN 200710024513
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CN100482075C (en
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吴重言
孙琴
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KESHENG GROUP CO Ltd JIANGSU PROV
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KESHENG GROUP CO Ltd JIANGSU PROV
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Abstract

The present invention discloses a pymetrozine suspension and its preparation method. It is formed from the following components: (by wt%) 3%-60% of pymetrozine, 1%-10% of defoaming agent, 0.5%-50% of dispersing agent, 0.1%-5% of antifreezing agent, 0.3%-10% of thickening agent, 0.01%-20% of stabilizing agent, 0%-10% of penetrating agent, 10%-80% of water and pH regulating agent for regulating pH value to 5-9. Said invention also provides the concrete steps of its preparation method.

Description

Pymetrozine suspension agent and preparation method thereof
Technical field
The invention belongs to pesticide field, be specifically related to suspending agent of a kind of insecticide and preparation method thereof.
Background technology
Pyrrole aphid ketonize formal name used at school claims: (E)-4, and 5-2 hydrogen-6-methyl-4-(3-pyridine methylene amine)-1,2,4-triazine-3 (2H)-ketone.
Pyrrole aphid ketone is high-efficient low toxicity insecticide, and it is to environment, people, animal, pest natural enemy and other beneficial organism safety, and control of insect is difficult for producing resistance, and it belongs to the insecticide of friendly environment, at present domestic-developed wetting powder.In recent years, national requirements exploitation friendly environment novel form, formulations of pesticide exploitation is to water baseization, ultramicronising, no dust and the development of sustained release aspect.Wherein water baseization is exactly one of main direction of agricultural chemicals development.Water can reduce the consumption of organic solvent as the suspending agent of solvent, the dust pollution that does not have wetting powder and pulvis to bring again, and reduced the pesticide producing cost, become a kind of very important formulation in the pesticide manufacturing.
Summary of the invention
The objective of the invention is by the effect of dispersant and the physics peptizaiton of ball mill; pyrrole aphid ketone is dispersed in the deionized water with small solid state; thereby a kind of consumption that can reduce the organic solvent in the pesticidal preparations is provided, can also protects the suspending agent of pyrrole aphid ketone better.
Another object of the present invention provides a kind of preparation method of above-mentioned suspending agent
Purpose of the present invention can reach by following measure:
A kind of pymetrozine suspension agent, form by following components in weight percentage:
Pyrrole aphid ketone 3%~60% defoamer 1%~10%
Dispersant 0.5%~50% antifreezing agent 0.1%~5%
Thickener 0.3~10% bleeding agent 0%~10%
Stabilizing agent 0.01%~20% water 10%~80%
It is 5~9 that the pH value is regulated in the pH regulator agent.
Dispersant is selected from sodium lignin sulfonate, the lignin calcium iodate, lauryl alcohol polyethylene glycol oxide base ether sodium sulfate, the alkyl naphthalene formaldehyde condensate sulfonates, neopelex, lauryl sodium sulfate, potassium oleate, enuatrol, alkyl polyoxyethylene ether sulfonate, alkylphenol-polyethenoxy base ether formaldehyde condensation products, alkylphenol-polyethenoxy base ether Nonyl pheno base ether, polyoxyethylene polyoxypropylene base ether block copolymers, draw back powder, poly-second carboxylic esters sodium salt, in dodecyl polyoxyethylene ether phosphate or the alkyl naphthalene formaldehyde condensate sulfonates one or more.
Thickener is selected from one or more in xanthans, CMC, hydroxyethylcellulose, methylcellulose or the polyvinyl alcohol.
Stabilizing agent is selected from one or more in catechol, butyl glycidyl ether, phenyl glycidyl ether, cresyl glycidyl ether, polyethylene glycol diglycidyl ether, chloropropylene oxide, sodium sorbate, Sodium Benzoate, epoxidised soybean oil, linseed oil, quinhydrones, anthraquinone, eugenol, citric acid, hydroxy benzoate or the nipasol.
Defoamer is selected from silicone oil, silicone compound, C 10-20Saturated fat acid compounds, C 8-10In aliphatic alcohols compound or the П-ethyl hexanol one or more.Wherein silicone compound such as organosilicon etc., C 10-20Saturated fat acid compounds such as hendecanoic acid, tridecanoic acid, pentadecanoic acid etc., C 8-10Aliphatic alcohols compound such as certain herbaceous plants with big flowers alcohol, ten alkanols etc.
Antifreezing agent is selected from one or more in ethylene glycol, glycerine, propane diols, polyethylene glycol, sorbierite or the urea.
The pH regulator agent is selected from one or more in sodium hydroxide, ammoniacal liquor, acetic acid, citric acid or the phosphoric acid.The consumption of pH regulator agent is that to make the pH value of suspending agent be 5~9.
Bleeding agent is an organosilicon.
A kind of method for preparing pymetrozine suspension agent, pyrrole aphid ketone and dispersant, thickener, stabilizing agent, defoamer, antifreezing agent, bleeding agent, PH conditioning agent and water are mixed according to the above ratio, ball milling is 2~3 hours in ball mill, makes particle diameter all below the 5 μ m.
In the formulations of pesticide, conventional dosage forms is based on EC (emulsifiable concentrate), WP (wetting powder), and water baseization formulation came into the market successively in nearly 2 years, and suspending agent (SC) then is representative wherein.Because it is a matrix with water, particle diameter is generally 1-3um, average 90% particle diameter≤5um, and suspensibility 〉=90%, high the opening up and adhesivity of performance on the crop blade face, it uses drug effect to compare with WP, and very big difference is arranged.
The present invention is scattered in the particle of pyrrole aphid ketone with miniaturization in the water, thereby has:
1. the flash-point height does not burn and does not explode, and produces storage and safe in utilization;
2. dust is few, and environmental pollution is little, to the producer and user and Environmental security;
3. with water matrix, aboundresources, product cost is low, easily packing;
4. pyrrole aphid ketone had protective effect;
5. after the said preparation spraying, be distributed in crop surface with fine particle, thus " instantaneous " concentration height of insect's food-taking, good disinsection effect;
6. preventive effect is better after adding bleeding agent.
Embodiment
Embodiment 1 25% pymetrozine suspension agent
Each constituent content (by weight) is the former powder 25% of pyrrole aphid ketone, dispersant sodium lignin sulfonate 10%, thickener xanthans 2%, stabilizing agent catechol 2%, defoamer silicone oil 1%, bleeding agent organosilicon 2%, antifreeze glycol 3%, it is 6 that the pH regulator agent makes suspending agent pH value in right amount, adds deionized water to 100%.The back ball milling 2~3 hours in ball mill that is mixed makes particle diameter all below 5 μ m.
Embodiment 2 20% pymetrozine suspension agents
Each component is the former powder 20% of pyrrole aphid ketone by weight, dispersant lauryl alcohol polyethylene glycol oxide base ether sodium sulfate 10%, thickener CMC 3%, stabilizing agent butyl glycidyl ether 2.5%, defoamer П-ethyl hexanol 1%, it is 7 that antifreezing agent glycerine 3%, pH regulator agent make suspending agent pH value in right amount, adds deionized water to 100%.The back ball milling 2~3 hours in ball mill that is mixed makes particle diameter all below 5 μ m.
Embodiment 3 10% pymetrozine suspension agents
Each constituent content (by weight) is the former powder 10% of pyrrole aphid ketone, dispersant alkyl naphthalene formaldehyde condensate sulfonates 40%, thickener hydroxyethylcellulose 9%, stabilizing agent chloropropylene oxide 12%, defoamer organosilicon 9%, it is 8 that antifreezing agent propane diols 4%, pH regulator agent make suspending agent pH value in right amount, adds deionized water to 100%.The back ball milling 2~3 hours in ball mill that is mixed makes particle diameter all below 5 μ m.
Embodiment 4 35% pymetrozine suspension agents
Each component is the former powder 35% of pyrrole aphid ketone by weight, dispersant neopelex 10%, poly-second carboxylic esters sodium salt 10%, thickener methylcellulose 1%, stabilizing agent sodium sorbate 2%, defoamer silicone oil 3%, bleeding agent organosilicon 5%, it is 9 that antifreezing agent polyethylene glycol 1%, pH regulator agent make suspending agent pH value in right amount, adds deionized water to 100%.The back ball milling 2~3 hours in ball mill that is mixed makes particle diameter all below 5 μ m.
Embodiment 5 55% pymetrozine suspension agents
Each constituent content (by weight) is the former powder 55% of pyrrole aphid ketone, dispersant alkyl polyoxyethylene ether sulfonate 10%, thickener polyvinyl alcohol 2%, stabilizing agent linseed oil 2%, defoamer hendecanoic acid 1%, bleeding agent organosilicon 9%, antifreezing agent sorbierite 3%, it is 5 that the pH regulator agent makes suspending agent pH value in right amount, adds deionized water to 100%.The back ball milling 2~3 hours in ball mill that is mixed makes particle diameter all below 5 μ m.
Embodiment 6 20% pymetrozine suspension agents
Each component is the former powder 20% of pyrrole aphid ketone by weight, dispersant gathers second carboxylic esters sodium salt 10%, thickener xanthans 3%, stabilizing agent eugenol 12%, defoamer tridecanoic acid 2%, bleeding agent organosilicon 8%, antifreezing agent glycerine 3%, it is 6 that the pH regulator agent makes suspending agent pH value in right amount, adds deionized water to 100%.The back ball milling 2~3 hours in ball mill that is mixed makes particle diameter all below 5 μ m.
Effect experiment
1 material and method
1.1 reagent agent
1.1.1 25% pyrrole aphid ketone WP (being pyrrole aphid ketone wetting powder), gram wins group to be provided
1.1.2 25% pyrrole aphid ketone SC (pymetrozine suspension agent of embodiment 1 gained)
1.2 Treatment Design
1.2.1 25% pyrrole aphid ketone WP is 20g/667m respectively 2
1.2.2 25% pyrrole aphid ketone SC is 20g/667m respectively 2
1.2.3 blank (CK)
1.3 test method
Establish 3 processing altogether, each is handled and repeats sub-district area 60m 3 times 2Local rice field four generations brown planthopper nymph peak period dispenser in 1 age on September 17th, 2006, every 667m 2Press above-mentioned design dosage to water 45kg.Aim at manually evenly complete stool spraying of rice seedling, during dispenser and behind the medicine in the week field keep water layer.
This experimental field rice varieties is for raising the spoke round-grained rice No. 7.During dispenser, field brown planthopper hundred cave worms are measured average 3345, wherein 1 age nymph account for 96.4%.
1.4 investigation method
1.4.1 security survey
Sub-district rice seedling growing state is respectively handled in irregular observation after the dispenser, and the record rice shoot is analyzed the safety of medicament to rice seedling to the reaction or the symptom of chemical damage of medicament.
1.4.2 preventive effect effect research
Investigation insect population radix before the dispenser was respectively looked into one time the residual worm amount in field in 1,3,7,10,15 day behind the medicine.3 samplings in every sub-district, every some company looks into 6 caves, and 18 caves are looked in every sub-district.Calculate control efficiency with the insect population survival rate, computing formula is as follows:
Proofread and correct preventive effect (%)=(check plot insect population survival rate-applying area insect population survival rate) ÷ check plot insect population survival rate * 100
2 medicaments are to the safety of rice seedling
Observe after the dispenser, it is normal that each handles sub-district rice seedling growth, any poisoning situation do not occur.
3 results and analysis
25% pyrrole aphid ketone WP and 25% pyrrole aphid ketone SC are obvious to paddy rice brown planthopper preventive effect effect, all showing aspect quick-acting and the Sustainable Control well, to rice seedling safety.Test data represents that the correction preventive effect of 25% pyrrole aphid ketone SC obviously is better than 25% pyrrole aphid ketone WP (seeing Table 1 in detail).These characteristics with SC (suspending agent) itself are associated, and can reach bigger even covering at the control target behind the suspending agent formulation thin up.Compare WP (wetting powder), the no dust of SC (suspending agent) mixes easily, and suspensibility improves, and degree of wetting also is improved.
Table 1 25% pyrrole aphid ketone WP and 25% pyrrole aphid ketone SC are to paddy rice brown planthopper preventive effect effect
Handle Behind the medicine 1 day Behind the medicine 3 days Behind the medicine 7 days Behind the medicine 10 days Behind the medicine 15 days
Preventive effect % Preventive effect % Preventive effect % Preventive effect % Preventive effect %
25% pyrrole aphid ketone WP20g/ mu 75.39 81.20 83.57 84.75 85.37
25% pyrrole aphid ketone SC20g/ mu 86.46 90.35 96.68 93.86 96.52

Claims (9)

1, a kind of pymetrozine suspension agent is characterized in that described suspending agent is made up of following components in weight percentage:
Pyrrole aphid ketone 3%~60% defoamer 1%~10%
Dispersant 0.5%~50% antifreezing agent 0.1%~5%
Thickener 0.3~10% bleeding agent 0%~10%
Stabilizing agent 0.01%~20% water 10%~80%
It is 5~9 that the pH value is regulated in the pH regulator agent.
2, suspending agent according to claim 1 is characterized in that described dispersant is selected from sodium lignin sulfonate, the lignin calcium iodate, lauryl alcohol polyethylene glycol oxide base ether sodium sulfate, the alkyl naphthalene formaldehyde condensate sulfonates, neopelex, lauryl sodium sulfate, potassium oleate, enuatrol, alkyl polyoxyethylene ether sulfonate, alkylphenol-polyethenoxy base ether formaldehyde condensation products, alkylphenol-polyethenoxy base ether Nonyl pheno base ether, polyoxyethylene polyoxypropylene base ether block copolymers, draw back powder, poly-second carboxylic esters sodium salt, in dodecyl polyoxyethylene ether phosphate or the alkyl naphthalene formaldehyde condensate sulfonates one or more.
3, suspending agent according to claim 1 is characterized in that described thickener is selected from one or more in xanthans, CMC, hydroxyethylcellulose, methylcellulose or the polyvinyl alcohol.
4, suspending agent according to claim 1 is characterized in that described stabilizing agent is selected from one or more in catechol, butyl glycidyl ether, phenyl glycidyl ether, cresyl glycidyl ether, polyethylene glycol diglycidyl ether, chloropropylene oxide, sodium sorbate, Sodium Benzoate, epoxidised soybean oil, linseed oil, quinhydrones, anthraquinone, eugenol, citric acid, hydroxy benzoate or the nipasol.
5, suspending agent according to claim 1 is characterized in that described defoamer is selected from silicone oil, silicone compound, C 10-20Saturated fat acid compounds, C 8-10In aliphatic alcohols compound or the Π-ethyl hexanol one or more.
6, suspending agent according to claim 1 is characterized in that described antifreezing agent is selected from one or more in ethylene glycol, glycerine, propane diols, polyethylene glycol, sorbierite or the urea.
7, suspending agent according to claim 1 is characterized in that described pH regulator agent is selected from one or more in sodium hydroxide, ammoniacal liquor, acetic acid, citric acid or the phosphoric acid.
8, suspending agent according to claim 1 is characterized in that described bleeding agent is an organosilicon.
9, a kind of method for preparing each described suspending agent in the claim 1~8, it is characterized in that pyrrole aphid ketone and dispersant, thickener, stabilizing agent, defoamer, antifreezing agent, bleeding agent, PH conditioning agent and water are mixed in the described ratio of claim 1, ball milling is 2~3 hours in ball mill, makes particle diameter all below the 5 μ m.
CNB2007100245136A 2007-06-21 2007-06-21 Pymetrozine suspension agent and preparation method Expired - Fee Related CN100482075C (en)

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Cited By (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101911932A (en) * 2010-08-03 2010-12-15 江苏天容集团股份有限公司 Pymetrozine oil suspending agent and preparation method thereof
CN101926334A (en) * 2010-09-11 2010-12-29 江西红土地化工有限公司 Pymetrozine-containing insecticidal suspension
CN102349507A (en) * 2011-09-13 2012-02-15 广西田园生化股份有限公司 Pymetrozine-containing ultralow volume liquid agent
CN101642107B (en) * 2009-07-17 2012-03-21 陕西上格之路生物科学有限公司 Insect-killing composition containing pymetrozine and etofenprox
CN101617676B (en) * 2009-08-01 2012-05-02 深圳诺普信农化股份有限公司 Pesticide compound
CN102524267A (en) * 2010-12-17 2012-07-04 南京红太阳股份有限公司 Pymetrozine suspension preparation containing vegetable oil and derivatives thereof and preparation method and application thereof
CN102550548A (en) * 2012-01-17 2012-07-11 广东中迅农科股份有限公司 Benthiavalicarb-isopropyl water suspension and preparation method thereof
CN102696629A (en) * 2012-05-14 2012-10-03 安徽省化工研究院 Functional pymetrozine insecticide and preparation method thereof
CN104054701A (en) * 2014-07-11 2014-09-24 中化化工科学技术研究总院 Pymetrozine suspension and preparation method for same
CN106577686A (en) * 2015-10-14 2017-04-26 上海师范大学 Pymetrozine suspension and preparation method thereof
CN107950547A (en) * 2017-11-21 2018-04-24 河南科技大学 A kind of composition and its application for being used to prevent crop powdery mildew
CN108041052A (en) * 2017-12-19 2018-05-18 扬州大学 A kind of pymetrozine and abamectin compounded agricultural chemicals suspension agent and preparation method thereof

Cited By (15)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101642107B (en) * 2009-07-17 2012-03-21 陕西上格之路生物科学有限公司 Insect-killing composition containing pymetrozine and etofenprox
CN101617676B (en) * 2009-08-01 2012-05-02 深圳诺普信农化股份有限公司 Pesticide compound
CN101911932A (en) * 2010-08-03 2010-12-15 江苏天容集团股份有限公司 Pymetrozine oil suspending agent and preparation method thereof
CN101926334A (en) * 2010-09-11 2010-12-29 江西红土地化工有限公司 Pymetrozine-containing insecticidal suspension
CN102524267A (en) * 2010-12-17 2012-07-04 南京红太阳股份有限公司 Pymetrozine suspension preparation containing vegetable oil and derivatives thereof and preparation method and application thereof
CN102349507B (en) * 2011-09-13 2013-09-11 广西田园生化股份有限公司 Pymetrozine-containing ultralow volume liquid agent
CN102349507A (en) * 2011-09-13 2012-02-15 广西田园生化股份有限公司 Pymetrozine-containing ultralow volume liquid agent
CN102550548A (en) * 2012-01-17 2012-07-11 广东中迅农科股份有限公司 Benthiavalicarb-isopropyl water suspension and preparation method thereof
CN102696629A (en) * 2012-05-14 2012-10-03 安徽省化工研究院 Functional pymetrozine insecticide and preparation method thereof
CN104054701A (en) * 2014-07-11 2014-09-24 中化化工科学技术研究总院 Pymetrozine suspension and preparation method for same
CN104054701B (en) * 2014-07-11 2016-02-17 中化化工科学技术研究总院 Pymetrozine suspension agent and preparation method thereof
CN106577686A (en) * 2015-10-14 2017-04-26 上海师范大学 Pymetrozine suspension and preparation method thereof
CN107950547A (en) * 2017-11-21 2018-04-24 河南科技大学 A kind of composition and its application for being used to prevent crop powdery mildew
CN107950547B (en) * 2017-11-21 2020-12-04 河南科技大学 Composition for preventing and treating crop powdery mildew and application thereof
CN108041052A (en) * 2017-12-19 2018-05-18 扬州大学 A kind of pymetrozine and abamectin compounded agricultural chemicals suspension agent and preparation method thereof

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