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Preparation method of indoxacarb

A technology of indoxacarb and toluene, which is applied in the field of insecticide preparation, can solve the problems of waste of raw materials, increase of production cost, and non-recyclable raw materials, and achieve the effect of saving raw materials and cost

Inactive Publication Date: 2018-04-17
安徽富田农化有限公司
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  • Abstract
  • Description
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  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, the existing indoxacarb preparation method is relatively complicated, and the raw materials in the production process of the prepared indoxacarb product cannot be recycled, which not only causes waste of raw materials, but also increases production costs

Method used

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  • Preparation method of indoxacarb
  • Preparation method of indoxacarb
  • Preparation method of indoxacarb

Examples

Experimental program
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preparation example Construction

[0036] combine Figure 1 to Figure 4 , a preparation method of indoxacarb, comprising the following steps:

[0037] S1. Put 5-chloroindanone and toluene into the batching kettle, stir and heat up to 40-50°C, add dimethyl carbonate after 30 minutes and stir evenly to obtain a mixed solution;

[0038] S2. Put toluene into the reaction kettle, add sodium methoxide, raise the temperature and reflux to the temperature of the kettle at 100-110°C, then add dimethyl carbonate, continue to heat and reflux to keep the top temperature at 80°C, and mix the mixture prepared by S1 at a constant speed Add it dropwise into the reaction kettle, cool down to 20°C, filter, and dry to obtain indanone ester sodium salt;

[0039] The synthetic chemical reaction equation of indanone ester sodium salt is:

[0040] C 9 h 7 OCl+C 3 h 6 o 3 +CH 3 ONa→C 11 h 8 o 3 ClNa+2CH 3 OH;

[0041] S3. Put dry indanone ester sodium salt and water into the neutralization kettle, freeze the ice brine to ...

Embodiment

[0067] Embodiment, a kind of preparation method of indoxacarb comprises the following steps:

[0068] S1. Put 215kg 5-chloroindanone and 1150kg toluene into a 2000L batching kettle, stir and heat up to 40-50°C, add 65kg dimethyl carbonate after 30 minutes and stir evenly to obtain a mixed solution;

[0069] S2. Put 1150kg of toluene into the 5000L reactor, then add 91kg of sodium methoxide, raise the temperature and reflux to the kettle temperature of 100-110°C, then add 55kg of dimethyl carbonate, continue to heat and reflux to stabilize the top temperature at 80°C, and prepare S1 Add the good mixture dropwise into the reaction kettle at a constant speed. When the top temperature is lower than 70°C, the kettle temperature is about 102°C at this time, start collecting fractions, keep the top temperature at 65-70°C, and continue to use the same collection speed after the dropwise addition Collect fractions until the top temperature is 110°C, cool down to 20°C, filter, wash the ...

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Abstract

The invention provides a preparation method of indoxacarb, and relates to the technical field of preparation of insecticides. The preparation method comprises the following steps of synthesizing of indanone ester sodium salt, synthesizing of hydroxylation matter, condensing of cyclization matter, cyclizing, concentrating, crystallizing, synthesizing of TPC (paraphthaloyl chloride), photochemical treatment, separating and crystallizing, preparing of cyclization matter solution and TPCC solution, performing hydrogenolysis, and condensing, so as to prepare the indoxacarb with high content and fewer impurities. The preparation method of the indoxacarb has the advantages that a large amount of Toluene, methanol and dimethyl carbonate-methanol can be recycled and reutilized in the production process, so that the raw material can be saved, and a large amount of cost is reduced; the preparation method is suitable for the large-scale production of the indoxacarb.

Description

technical field [0001] The invention relates to the technical field of pesticide preparation, in particular to a preparation method of indoxacarb. Background technique [0002] Indoxacarb is an insecticide. Other names of indoxacarb are Avatar preparation, 30% Avatar water dispersible granule, and 15% Avatar suspension concentrate. According to the classification standard of pesticide toxicity in China, Anta is a low-toxicity insecticide. 30% tap water dispersible granules rat acute oral LD50 1867 mg / kg (male), 687 mg / kg (female); rat acute percutaneous LD50 greater than 5000 mg / kg, no carcinogenic, teratogenic and mutagenic effects , Anta by blocking the sodium ion channels in insect nerve cells, so that nerve cells lose their function. Indoxacarb is a high-efficiency, low-toxicity, and low-residue pesticide. It has strong toxicity to pests, but is safe for animals. It is a new type of broad-spectrum high-efficiency insecticide. The preparation contains 30% WDG And 15% S...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D273/04
CPCC07D273/04
Inventor 吴学群宛传井聂诗兴
Owner 安徽富田农化有限公司
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