CN101379964A - Hexythiazox suspension agent and preparation method thereof - Google Patents

Hexythiazox suspension agent and preparation method thereof Download PDF

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CN101379964A
CN101379964A CNA2008101325838A CN200810132583A CN101379964A CN 101379964 A CN101379964 A CN 101379964A CN A2008101325838 A CNA2008101325838 A CN A2008101325838A CN 200810132583 A CN200810132583 A CN 200810132583A CN 101379964 A CN101379964 A CN 101379964A
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hexythiazox
suspending agent
ether
dispersant
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CN101379964B (en
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张少武
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Abstract

The invention discloses a hexythiazox suspending agent which consists of the components in the weight percentage: 1-50% of hexythiazox, 0.1-1% of defoamer, 0.5-10% of dispersant, 1-10% of antifreeze, 0.1-5% of thickening agent, 0.01-20% of stabilizing agent, 0-10% osmotic agent and 10-80% of water. The invention also discloses a method for preparing the hexythiazox suspending agent. The hexythiazox suspending agent has the advantages of high flash point, no combustion and explosion, safe production, storage and use, little dust, no environmental pollution, low product cost, easy package, good desinsection effect, etc.

Description

A kind of hexythiazox suspension agent and preparation method thereof
Technical field
The invention belongs to the agricultural chemicals preparation field, be specifically related to a kind of hexythiazox suspension agent and preparation method thereof.
Background technology
Hexythiazox, (hexythiazox), chemical name: (4RS, 5RS)-5-(4-chlorphenyl)-N-cyclohexyl-4-methyl-2-oxo-1,3-thiazoles alkane-3 carboxylic acid amides.It is novel thiazolidine ketone miticide.The evil mite is had and tags by force and stomach poison function; The crop epidermis is had stronger osmosis, can infiltrate in the blade and be penetrated into the harmful mite that blade back kills blade back, but do not have systemic action; To the mite ovum, if mite and young mite are all effective, to becoming the mite virulence very little, yet, touch incubation rate that the female one-tenth mite of medicament laid eggs is at half behind the medicine and arrived the drug effect peak in 7-10 days very much, 40-50 days lasting periods, the effect of using when high temperature or low temperature does not have significant difference, at present domestic-developed Hexythiazox wetting powder and missible oil.
This year, the friendly insecticidal/acaricidal agent of national requirements exploitation, the acute exploitation of agricultural chemicals 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, does not have the dust pollution that wetting powder, pulvis bring and the smell of missible oil to pollute again, and has reduced the pesticide producing cost, has become the very important formulation in the pesticidal preparations.
Summary of the invention
The objective of the invention is Hexythiazox to be dispersed in the deionized water with small solid state, thereby a kind of suspending agent that can reduce the consumption of the organic solvent in the pesticidal preparations is provided by the effect of dispersant and the physics peptizaiton of ball mill.
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 hexythiazox suspension agent, form by following components in weight percentage:
Hexythiazox 1%~50% defoamer 1%~15%
Dispersant 0.5%~50% antifreezing agent 0.1%~10%
Thickener 0.3%~10% stabilizing agent 0.01%~20%
Bleeding agent 0~10% water 10%~80%
Dispersant is selected from sodium lignin sulfonate, calcium lignosulfonate, lauryl alcohol polyethylene glycol oxide base ether sodium sulfate, 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, draws back powder, in the poly-second carboxylic esters sodium salt one or more.
Thickener is selected from one or more in xanthans, CMC, hydroxyethylcellulose, methylcellulose, Magnesiumaluminumsilicate 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, citric acid, hydroxy benzoate or the propylparaben.
Defoamer is selected from one or more in silicone oil, silicone compound, C10-20 saturated fat acid compounds, the C8-10 aliphatic alcohols compound.Wherein silicone compound such as organosilicon etc., C10-20 saturated fat acid compounds such as hendecanoic acid, tridecanoic acid, pentadecanoic acid etc., C8-10 aliphatic 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, the sorbierite.
Bleeding agent is organosilicon, azone, fatty alcohol-polyoxyethylene ether etc.
A kind of method for preparing hexythiazox suspension agent, it is characterized in that Hexythiazox and dispersant, thickener, stabilizing agent, defoamer, antifreezing agent, bleeding agent and water are mixed in the described ratio of claim 1, with ball milling in the ball mill 2~3 hours, make particle diameter all below 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.Having in it is matrix with water, and particle diameter is generally 1~35 μ m, average 90% particle diameter≤5 μ m, and suspensibility 〉=90%, high the opening up and tackness 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 Hexythiazox with miniaturization in the water, thereby has:
1) flash-point height, nonflammable difficult blast, safer to production, storage and user;
2) dust is few, and environmental pollution is little, to the producer and user and Environmental security;
3) with water be matrix, aboundresources, product cost is low, easily packing;
4) Hexythiazox is killed mite active ingredient and have 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 behind the adding bleeding agent.
Embodiment
Embodiment 1 5% hexythiazox suspension agent
Each constituent content (by weight) is the former powder 5g of Hexythiazox, dispersant sodium lignin sulfonate 10g, and thickener xanthans 2g, stabilizing agent catechol 2g, defoamer silicone oil 1g, bleeding agent organosilicon 2g, antifreeze glycol 3g adds deionized water to 100g.Mix back ball milling 2~3 hours in ball mill, make particle diameter all below 5 μ m.
Embodiment 2 10% hexythiazox suspension agents
Each constituent content (by weight) is the former powder 10g of Hexythiazox, dispersant lauryl alcohol polyethylene glycol oxide base ether sodium sulfate 10g, thickener CMC 3g, stabilizing agent butyl glycidyl 2.5g, defoamer silicone oil 1g, bleeding agent organosilicon 2g, antifreezing agent glycerine 3g adds deionized water to 100g.Mix back ball milling 2~3 hours in ball mill, make particle diameter all below 5 μ m.
Embodiment 3 15% hexythiazox suspension agents
Each constituent content (by weight) is the former powder 15g of Hexythiazox, dispersant lauryl alcohol polyethylene glycol oxide base ether sodium sulfate 8g, thickener CMC 3g, stabilizing agent butyl glycidyl 2.5g, defoamer silicone oil 1%, bleeding agent organosilicon 2g, antifreezing agent glycerine 3g adds deionized water to 100g.Mix back ball milling 2~3 hours in ball mill, make particle diameter all below 5 μ m.
Embodiment 4 20% hexythiazox suspension agents
Each constituent content (by weight) is the former powder 20g of Hexythiazox, and dispersant gathers second carboxylic esters sodium salt 10g, thickener xanthans 2g, and stabilizing agent sodium sorbate 2g, defoamer tridecanoic acid 2g, bleeding agent organosilicon 2g, antifreezing agent glycerine 3g adds deionized water to 100g.Mix back ball milling 2~3 hours in ball mill, make particle diameter all below 5 μ m.5% hexythiazox suspension agent agent control citrus red mite field control effectiveness test
1, test objective
Explore best field using dosage, concentration and the spraying time of reagent agent 5% hexythiazox suspension agent control citrus red mite, tentatively estimating test medicine influences trial crops, for the evaluating drug effect and the safety of agriculture chemical registration, reasonable operation technique provide foundation.2 experimental conditions
2, subjects, crop and breed selection
Citrus red mite (Panonychus citri).Citrus, kind are emerging Tianjin of series, Wenzhou kind.
Environmental condition: 13 mu of test tangerine garden areas, ground, north orientation sun gentle slope by east, kind is the Xing Jin of satsuma mandarin series, the age of tree 9 years, 1.5 * 3 meters of seeding row spacings, density 148 strain/mus, soil are yellow mud crust soil, the content of organic matter 1.54%, pH value 6.5, the poor ridge of fertility, irrigation conditions is relatively poor.Winter in 2006, mu was executed 100 kilograms of carbon ammoniums, 50 kilograms of general calcium, 500 kilograms of farmyard manures.
3, experimental scheme and arrangement
3.1 medicament
3.1.1 test medicine 5% hexythiazox suspension agent, autogamy.
3.1.2 contrast medicament
5% Hexythiazox missible oil; Kesheng Group Co., Ltd., Jiangsu Prov. produces.Commercial
15% pyridaben missible oil; The Hubei sand swell reaches limited company and produces.Commercial
3.1.3 dosing and numbering
Table 1 reagent agent experimental scheme
Handle numbering Medicament Dispenser dosage (amount of formulation) Formulation rate (active ingredient amount mg/kg)
1 5% Hexythiazox SC 3000 166.7
2 5% Hexythiazox SC 3500 142.8
3 5% Hexythiazox SC 4000 125.0
4 5% Hexythiazox EC 2000 125.0
5 15% pyridaben EC 2000 75.0
6 The CK clear water / /
3.2 the sub-district arranges the 3.2.1 sub-district to arrange
Figure A200810132583D00091
3.2.2 sub-district area and repetition
Sub-district area: two fruit trees in every sub-district.
Number of repetition: 4 times.
3.3 application method
3.3.1 the using method hand spray squirts whole blade desires with soup and does not drip degree of being.
3.3.2 spraying equipment.
Singapore produces Jacto board HD-400 type knapsack hand sprayer, operating pressure 8Kgf/cm2, injection diameter 1.33mm.
3.3.3 a spraying time and a number of times dispenser on June 24.
3.3.4 the capacity of use administration of medical fluid amount is 2220 liters/hectare (citrus density 148 strain/mus).
3.3.5 prevent and treat the medicament data of other damage by disease and insect
On December 12nd, 2006 was killed the citrus germ that survives the winter with 28 times of liquid of 20% lime sulfur;
4, investigation, record and measuring method
4.1 meteorology and soil information
4.1.1 meteorological data is fine June 24,26.3 ℃ of mean temperature of air, relative air humidity 70%.
4.1.2 soil information
Soil is yellow mud crust soil, the content of organic matter 1.54%, and pH value 6.5, fertility is barren, and irrigation conditions is relatively poor.
4.2 investigation method, time and number of times
4.2.1 control time and number of times
Investigation radix (June 24) before the dispenser is done investigation in 1 day, 3 days, 10 days, 15 days, 20 days, 30 days behind the medicine respectively on June 25, June 27, July 4, July 9, July 14, July 24.
4.2.2 investigation method
Every sub-district 2 strains tree, east, south, west, north, the tender tip of middle five positions mark of every strain tree are investigated 25 movable mite quantity on the blade altogether.
4.2.3 drug effect computational methods
Figure A200810132583D00101
Figure A200810132583D00102
4.3 direct influence to crop
Each processing of reagent agent 5% hexythiazox suspension agent does not have the poisoning phenomenon to citrus.
4.4 the quality of product and output
Reagent agent 5% hexythiazox suspension agent can improve the output of product.
4.5 other biological is influenced
4.5.1 influence to other damage by disease and insect
Reagent agent 5% hexythiazox suspension agent has certain inhibitory action to the citrus arrowhead scales.
4.5.2 influence to other non-target organisms
Reagent agent 55% hexythiazox suspension agent obviously influences the nothing of other non-target organism.
5, result and analysis
Table 2 5% hexythiazox suspension agent control citrus red mite field control effectiveness test result
Adopt the new multipole of Deng Kenshi poor (DMRT) method to carry out statistical analysis, utilize the DPS analysis software to analyze.
Reagent agent 5% hexythiazox suspension agent has the better prevention effect to citrus red mite, and its 3000 times of liquid are handled and the preventive effect and the two contrast chemicals treatment of 3500 times of liquid processing relatively have clear superiority.
Recommending using dosage is 166.7~142.8 (ai) mg/kg, and dispenser when two spotted spider mite is taken place in a large number should be noted during use being used alternatingly with other insecticide, to prevent drug-fast generation.
Table 3-1 5% hexythiazox suspension agent control citrus red mite field control effectiveness test result's statistics (2007)
Figure A200810132583D00121
Table 3-2
Figure A200810132583D00122
Figure A200810132583D00131
Table 4 dispenser same day is weather conditions table (2007) experimental field
The dispenser date Weather conditions Wind direction and wind-force Temperature (℃) Relative moisture (%) Other climatic factors
June 24 Fine Gentle breeze 26.3 70
Table 5 duration of test meteorological data table (2007)
Figure A200810132583D00141

Claims (8)

1, a kind of hexythiazox suspension agent is characterized in that described suspending agent is made up of following components in weight percentage:
Hexythiazox 1%~50% defoamer 0.1%~1%
Dispersant 0.5%~10% antifreezing agent 1%~10%
Thickener 0.3%~10% stabilizing agent 0.01%~20%
Bleeding agent 0~10% water 10%~80%.
2, suspending agent according to claim 1 is characterized in that described dispersant is selected from the acid of sodium lignin sulfonate, lignin calcium, lauryl alcohol polyethylene glycol oxide base ether sodium sulfate, 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, draws back powder, in the poly-second carboxylic esters sodium salt 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, citric acid, hydroxy benzoate or the propylparaben.
5, suspending agent according to claim 1 is characterized in that described defoamer is selected from one or more in silicone oil, silicone compound, C10-20 saturated fat acid compounds, the C8-10 aliphatic alcohols compound.
6, suspending agent according to claim 1, the antifreezing agent under it is characterized in that is selected from one or more in ethylene glycol, glycerine, propane diols, polyethylene glycol or the sorbierite.
7, require 1 described suspending agent according to power, it is characterized in that described bleeding agent is an organosilicon.
8, a kind of method for preparing each affiliated suspending agent in the claim 1~7, it is characterized in that Hexythiazox and dispersant, thickener, stabilizing agent, defoamer, antifreezing agent, bleeding agent and water are mixed in the described ratio of claim 1, with ball milling in the ball mill 2~3 hours, make particle diameter all below 5 μ m.
CN2008101325838A 2008-07-17 2008-07-17 Hexythiazox suspension agent and preparation method thereof Expired - Fee Related CN101379964B (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101642099A (en) * 2009-08-31 2010-02-10 桂林集琦生化有限公司 Pesticide suspension concentrate with organosilicon surfactant and preparation method thereof
CN102293214A (en) * 2011-09-27 2011-12-28 江苏省绿盾植保农药实验有限公司 Acaricide composition containing hexythiazox and amitraz
CN104920423A (en) * 2015-06-12 2015-09-23 福建省德盛生物工程有限责任公司 Low-volume spray with hexythiazox
CN111406754A (en) * 2020-04-28 2020-07-14 浙江禾本科技股份有限公司 Hexythiazox water suspending agent and preparation method thereof

Family Cites Families (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
PL192652B1 (en) * 1997-08-22 2006-11-30 Plaaskem Proprietary Ltd Dosage form
CN1176586C (en) * 2002-10-10 2004-11-24 华南农业大学 Pesticide prep of mixed nimbin and miticide
CN1751572A (en) * 2004-09-21 2006-03-29 葛尧伦 Composition of miticide
CN101185435A (en) * 2007-11-21 2008-05-28 张少武 Miticide composition containing diafenthiuron active ingredient and uses thereof

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101642099A (en) * 2009-08-31 2010-02-10 桂林集琦生化有限公司 Pesticide suspension concentrate with organosilicon surfactant and preparation method thereof
CN101642099B (en) * 2009-08-31 2012-10-17 桂林集琦生化有限公司 Pesticide suspension concentrate with organosilicon surfactant and preparation method thereof
CN102293214A (en) * 2011-09-27 2011-12-28 江苏省绿盾植保农药实验有限公司 Acaricide composition containing hexythiazox and amitraz
CN104920423A (en) * 2015-06-12 2015-09-23 福建省德盛生物工程有限责任公司 Low-volume spray with hexythiazox
CN111406754A (en) * 2020-04-28 2020-07-14 浙江禾本科技股份有限公司 Hexythiazox water suspending agent and preparation method thereof

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