The invention relates to the technical field of pesticides, and particularly provides a pesticide adjuvant and a preparation method thereof. The first aspect of the invention provides a pesticide auxiliary agent which at least comprises the following preparation raw materials in parts by weight: 4-30 parts of calcium dodecylbenzene sulfonate, 1-20 parts of nonylphenol polyoxyethylene ether, 1-20 parts of an emulsifier, 0.1-10 parts of dodecylbenzene sulfonic acid, 0.1-6 parts of triethanolamine, 2-20 parts of a wetting agent and 30-100 parts of a solvent. The wetting agent is alkyl glycoside with a carbon chain length of 8-14.

Pesticide adjuvant and preparation method thereof

The invention discloses a preparation method of a bendiocarb intermediate and an active ingredient. The preparation method includes: allowing pyrogallic acid to react with 2, 2-dimethoxypropane to generate a 2, 2-dimethyl-4-hydroxyl-1, 3-benzodioxoles solution, and directly using light components 2, 2-dimethoxypropane, 2-methoxypropene and methanol which are evaporated out for next batch after alkali washing; allowing the 2, 2-dimethyl-4-hydroxyl-1, 3-benzodioxoles solution to react with methyl isocyanate to obtain the bendiocarb active ingredient. By recycling raw materials and byproducts, cost is lowered, operation is simplified, production efficiency is improved, and convenience is brought for industrial production.

Preparation method of bendiocarb intermediate and active ingredient

The invention discloses a production process of dimethylamino sulfonyl chloride. The production process comprises the steps of reacting dimethylamine hydrochloride with chlorosulfonic acid to generatedimethylamine salt of dimethylaminosulfonic acid, slowly adding a reaction product into a sodium hydroxide solution, distilling off dimethylamine and water to obtain dimethylamine sodium sulfonate, reacting with phosphorus pentachloride, and rectifying to obtain the product. According to the method disclosed by the invention, highly toxic dimethylamine gas is avoided, the purity of the product dimethylamino sulfonyl chloride reaches 99% or above, and the maximum molar yield is close to 80%.

Production process of dimethylamino sulfonyl chloride

The invention discloses a preparation method for methomyl oxime. The preparation method comprises the following steps: (1) respectively dissolving acetaldehyde oxime and chlorine gas in an organic solvent to obtain an organic solution of acetaldehyde oxime and an organic solution of chlorine gas, and dissolving sodium methyl mercaptide and sodium hydroxide in an organic solvent to obtain a mixed organic solution; (2) with the organic solution of acetaldehyde oxime and the organic solution of chlorine gas as raw materials, carrying out continuous feeding for a chlorination reaction; and (3) immediately subjecting a chlorinated mixed solution obtained by a chlorination reaction to a methylthio substitution reaction with the mixed organic solution, removing the solvent from a crude methomyl oxime product obtained by the reaction, and adding a small amount of water to wash the crude methomyl oxime product so as to obtain high-quality methomyl oxime. The method is controllable in reaction heat, small in by-product influence, short in time, capable of avoiding decomposition of chloroacetaldoxime, low in the amount of generated wastewater and free of wasterwater odor, and the obtained finished methomyl oxime is high in yield and quality.

Preparation method of methomyl oxime

The invention discloses a solid catalyst and application thereof to preparing methyl formate isothiocyanate through catalysis. The catalyst is prepared in the steps that rare earth element precursor nitrate is prepared into a nitrate aqueous solution with the mass fraction of 15-25%, modified nano attapulgite is added into the nitrate aqueous solution under the stirring condition, the mixture is stirred evenly, still standing and aged for 24-48 h, the mixture is dried at 100-120 DEG C after ageing and then calcined for 3-5 h at 400-600 DEG C, and the solid catalyst is obtained, wherein the weight of the modified nano attapulgite is 8-12 times that of nitrate. The modified nano attapulgite is prepared in the steps that 30-40 parts of nano attapulgite is dispersed in 45-55 parts of ammonia water with the mass fraction of 15-25% and stirred for 25-35 min at 40-50 DEG C, then 10-20 parts of nano titanium dioxide is added and stirred for 20-30 min, the product is cooled, filtered and dried, and the solid catalyst is obtained. The prepared solid catalyst is stable in catalytic performance and can be repeatedly used, catalysis efficiency is not obviously reduced after repeated use, and prepared methyl formate isothiocyanate is high in purity and yield.

Solid catalyst and application thereof to preparing methyl formate isothiocyanate through catalysis

The invention discloses a preparation method of 4-hydroxy-2,2-dimethyl-1,3-benzodioxole (called dioxole for short). According to the preparation method, pyrogallic acid and 2,2-dimethoxy propane are taken as raw materials, methyl benzene or dimethyl benzene is taken as a reaction solvent, methanesulfonic acid dry resin is taken as a catalyst, a rectifying catalytic reaction mode is adopted, and the catalyst is arranged at the bottom of a rectifying tower positioned between a reaction kettle and a condenser; by-products methoxyl propylene and methanol which are generated through reaction are reacted under the action of the catalyst when passing through the rectifying tower to generate the raw material 2,2-dimethoxy propane, and the 2,2-dimethoxy propane is returned to the reaction kettle to participate in the reaction for preparing the dioxole again; surplus by-product methanol is transferred from the condenser positioned on the top of the rectifying tower, and a product is obtained from a tower kettle. The preparation method disclosed by the invention is simple in technological operation and high in reaction selectivity, and can be used for promoting the reaction equilibrium to move towards a target product direction, thus achieving the effects of low material consumption, high transformation rate and high selectivity; in addition, reaction liquid obtained through synthesis can be used for synthesis of active compound bendiocarb, no three wastes are basically generated and industrialized production is facilitated.

Preparation method of 4-hydroxy-2,2-dimethyl-1,3-benzodioxole

The invention discloses a method for preparing isothiocyano methyl formate. The method is characterized in that a sodium thiocyanate aqueous solution and methylclhlorofonmate are taken as raw materials, a tubular reactor is adopted, and the isothiocyano methyl formate is synthesized continuously under the action of chloroethylene-supported N-alkyl-N-methylaniline serving as a solid catalyst. By adopting the method, the conventional kettle reaction method is changed. The tubular reactor is used for preparing the isothiocyano methyl formate by continuous synthesis, so that the reaction time is shortened greatly, reaction byproducts are reduced at the same time, side reactions of the isothiocyano methyl formate are avoided, and the reaction safety is enhanced. The chloroethylene-supported N-alkyl-N-methylaniline serving as the solid catalyst is adopted, so that the problem of odor pollution due to entrance of N,N-dimethylaniline serving as a catalyst into subsequent waste water in the conventional method is solved, and the environmental protection stress is lowered. Moreover, the catalyst can be used continuously for 300 hours, so that the production cost is lowered greatly. The method is low in equipment investment, is short in reaction period, is easy to operate, and is suitable for industrial production.

Method for preparing isothiocyano methyl formate

The invention discloses a compounding composition containing chlorine chlorfenapyr. The compounding composition comprises effective components of the chlorine chlorfenapyr and adifopyropen with the weight ratio of (1:20) to (20:1). The compounded composition has the advantages that the controlling effect in controlling homopteran and lepidopteran pests is good, the pesticide applying dosage and the pesticide using times can be reduced, the pesticide tolerance can be delayed and the pesticide resistance is good and the like.

Compounded composition containing chlorine chlorfenapyr and application of composition

The invention discloses a preparation method of chloroacetaldehyde oxime. Chloroacetaldehyde oxime is prepared with acetaldehyde oxime and chlorine gas as raw reaction materials and a micro reactor asa reaction device; the preparation method comprises the following steps of simultaneously and continuously introducing acetaldehyde oxime and the chlorine gas into the micro reactor for a reaction, and conducting a neutralization reaction on an obtained product solution to obtain a chloroacetaldehyde hydrazine solution. According to the preparation method, the micro reactor is used as the reaction device, the reaction can be completed quickly within a short time, the energy consumption can be significantly reduced, the staying time can be shortened, the reaction efficiency is greatly improved, continuous feeding and discharging can be achieved, a target product and reaction discharged heat are timely removed, the decomposition of raw materials and the production of explosive by-products are reduced, the reaction yield is greatly increased, the production safety is greatly improved, and the method has the advantages of high safety, simple operation, high yield, economical performance,environmental protection and the like, and has good application value and application prospects.

Preparation method of chloroacetaldehyde oxime

The invention discloses a preparation method of dimethylcarbamoyl chloride. The preparation method comprises the following steps: simultaneously introducing dimethylamine and phosgene into a micro-reactor to perform the reaction to obtain the dimethylcarbamoyl chloride. The dimethylcarbamoyl chloride prepared in the preparation method disclosed by the invention is high in content, the content reaches 98.5 to 99 percent, and the yield is greatly increased and can reach 95.0 to 96.2 percent (referring to dimethylamine). The preparation method disclosed by the invention has the advantages of simple operation, high yield, less waste, safety, environmental protection and the like, is suitable for industrialized production and good in application value and application prospect.

Preparation method of dimethylcarbamoyl chloride

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