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CN101379964B - Hexythiazox suspending agent and preparation method thereof - Google Patents

Hexythiazox suspending agent and preparation method thereof Download PDF

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CN101379964B
CN101379964B CN2008101325838A CN200810132583A CN101379964B CN 101379964 B CN101379964 B CN 101379964B CN 2008101325838 A CN2008101325838 A CN 2008101325838A CN 200810132583 A CN200810132583 A CN 200810132583A CN 101379964 B CN101379964 B CN 101379964B
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hexythiazox
agent
suspension
dispersant
sodium
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CN101379964A (en
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张少武
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Abstract

本发明公开了一种噻螨酮悬浮剂,这种悬浮剂由以下重量百分比的组分组成:噻螨酮1%~50%,消泡剂0.1%~1%,分散剂0.5%~10%,防冻剂1%~10%,增稠剂0.1%~5%,稳定剂0.01%~20%,渗透剂0~10%,水10%~80%。本发明还公开了上述噻螨酮悬浮剂的制备方法。本发明的噻螨酮悬浮剂具有闪点高,不燃烧不爆炸,生产、储存、使用安全,粉尘少,环境污染小,产品成本低,容易包装,杀虫效果好等优点。The invention discloses a hexythiazox suspension, which is composed of the following components in weight percentage: 1% to 50% of hexythiazox, 0.1% to 1% of defoamer, 0.5% to 10% of dispersant, 1% to 10% of antifreeze, 0.1% to 5% of thickener, 0.01% to 20% of stabilizer, 0% to 10% of penetrant, and 10% to 80% of water. The invention also discloses a preparation method of the hexythiazox suspension. The hexythiazox suspension has the advantages of high flash point, no combustion and no explosion, safe production, storage and use, less dust, less environmental pollution, low product cost, easy packaging, good insecticide 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 and be at half very much behind the medicine and arrived drug effect peak, lasting period 40-50 days in 7-10 days; 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
The object of the invention can reach through following measure:
A kind of hexythiazox suspension agent, form by following components in weight percentage:
Hexythiazox 1%~50% antifoaming agent 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, draw back powder, gather in the 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.
Antifoaming agent 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, AEO etc.
A kind of method for preparing hexythiazox suspension agent; It is characterized in that Hexythiazox and dispersant, thickener, stabilizing agent, antifoaming agent, antifreezing agent, bleeding agent and water even by the described mixed 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 main with 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 is high, and nonflammable difficult blast is 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, so " instantaneous " concentration of insect's food-taking is high, good disinsection effect with fine particle;
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, antifoaming agent 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, antifoaming agent 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, antifoaming agent 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, antifoaming agent 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
Exploration supplies best field using dosage, concentration and the spraying time of reagent agent 5% hexythiazox suspension agent control citrus red mite, and 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 supplies 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 / /
Figure S2008101325838D00061
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 method for using 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 S2008101325838D00071
4.3 direct influence to crop
Supply each processing of reagent agent 5% hexythiazox suspension agent that citrus is not had the poisoning phenomenon.
4.4 the quality of product and output
Supply 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
Supply reagent agent 5% hexythiazox suspension agent that the citrus arrowhead scales is had certain inhibitory action.
4.5.2 influence to other non-target organisms
Supply reagent agent 55% hexythiazox suspension agent that the nothing of other non-target organism is obviously influenced.
5, result and analysis
Table 2 5% hexythiazox suspension agent control citrus red mite field control effectiveness test result
Figure S2008101325838D00081
Adopt the new multipole of Deng Kenshi poor (DMRT) method to carry out statistical analysis, utilize the DPS analysis software to analyze.
Supply reagent agent 5% hexythiazox suspension agent that citrus red mite is had the better prevention effect, 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 S2008101325838D00091
Table 3-2
Figure S2008101325838D00092
Figure S2008101325838D00101
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 S2008101325838D00102
Figure S2008101325838D00111

Claims (2)

1.一种噻螨酮悬浮剂,其特征在于:所述的悬浮剂由以下重量百分比组成:1. a suspension of hexythiazox, characterized in that: said suspension consists of the following percentages by weight:
Figure FSB00000670265900011
Figure FSB00000670265900011
所述的分散剂选自木质素磺酸钠、月桂醇聚氧乙烯基醚硫酸钠、聚乙羟酸酯钠盐中的一种或几种;The dispersant is selected from one or more of sodium lignosulfonate, sodium lauryl polyoxyethylene ether sulfate, polyglycolic acid ester sodium salt; 所述的增稠剂选自黄原胶、羟甲基纤维素中的一种或多种;Described thickening agent is selected from one or more in xanthan gum, hydroxymethyl cellulose; 所述的稳定剂选自邻苯二酚、丁基缩水甘油、山梨酸钠中的一种或多种;The stabilizer is selected from one or more of catechol, butyl glycidol, sodium sorbate; 所述的消泡剂选自硅油、十三烷酸中的一种或多种;The defoamer is selected from one or more of silicone oil and tridecanoic acid; 所述的防冻剂选自乙二醇、丙三醇中的一种或多种;Described antifreezing agent is selected from one or more in ethylene glycol, glycerol; 所述的渗透剂选自有机硅。The penetrating agent is selected from silicone.
2.根据权利要求1中所述的悬浮剂,其特征在于:将噻螨酮与分散剂、增稠剂、稳定剂、消泡剂、防冻剂、渗透剂和水按权利要求1所述的比例混合均匀,于球磨机中球磨2~3小时,使粒径全部在5μm以下。2. according to the suspending agent described in claim 1, it is characterized in that: hexythiazox and dispersant, thickener, stabilizer, defoamer, antifreeze, penetrating agent and water are pressed according to claim 1 The ratio is mixed evenly, and ball milled in a ball mill for 2 to 3 hours, so that the particle size is all below 5 μm.
CN2008101325838A 2008-07-17 2008-07-17 Hexythiazox suspending agent and preparation method thereof Expired - Fee Related CN101379964B (en)

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Publication number Priority date Publication date Assignee Title
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
CN111406754B (en) * 2020-04-28 2021-06-15 浙江禾本科技股份有限公司 Hexythiazox water suspending agent and preparation method thereof

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