Method for producing bifenthrin with clean synthesizing process

A production method and bifenthrin technology are applied in the field of bifenthrin production with a clean synthesis process, which can solve the problems of long reaction time, excessive waste water, and low yield, and achieve improved synthesis conversion rate, simple process, and The effect of small amount of three wastes produced

Inactive Publication Date: 2015-05-20
JIANGSU YANGNONG CHEM +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] U.S. Patent (US4341796) adopts 2-methyl-3-chloromethyl biphenyl in acid-binding agent and suitable solvent, and trifluorochrysanthemum acid (3-(2-chloro-3,3,3-trifluoro- 1-propenyl)-2,2-dimethylcyclopropanecarboxylic acid) for chemical reaction to generate bifenthrin, but the yield is low and the waste water is much
Introduced in CN103145558A adopts permethrin to carry out ester synthesis with methanol at first, then carry out transesterification with biphenyl alcohol to obtain bifenthrin, in the process of ester synthesis between permethrin and methanol, due to the reaction to generate water Relying on methanol to take out, the amount of methanol used and the amount of methanol treatment cycle are large, and the reaction time is long
In the process of transesterification with biphenyl alcohol, an excess of biphenyl alcohol is usually required, the conversion rate of the reaction process is only 95%, and the residual reactants are likely to affect the quality of bifenthrin

Method used

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  • Method for producing bifenthrin with clean synthesizing process
  • Method for producing bifenthrin with clean synthesizing process
  • Method for producing bifenthrin with clean synthesizing process

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] 194Kg of 2-methyl-3-phenylbenzyl alcohol and 700Kg of n-hexane were put into a 2000L synthesis kettle equipped with stirring, condenser and tail gas absorption device, and the temperature was raised to 45°C. Tail gas is absorbed by falling film water in three stages in series, 80L of water is added to each stage, and the absorption temperature is 10-55°C.

[0024] The temperature of the reaction kettle was controlled at 45-55°C, and 261Kg of trifluorochrysanthemum acid chloride was started to be added dropwise into the synthesis kettle for 3 hours. After the dropwise addition was completed, the reaction was incubated for 6 hours. At the end of the heat preservation reaction, the conversion rate of 2-methyl-3-phenylbenzyl alcohol in Zhongkong was 99.5%. 114.5Kg of hydrochloric acid, with a content of 30.08%, was recovered in the first stage of tail gas absorption.

[0025] The materials in the synthesis kettle were discharged into the crystallization kettle to cool dow...

Embodiment 2

[0027] 198Kg of 2-methyl-3-phenylbenzyl alcohol and 990Kg of n-hexane were put into a 2000L synthesis kettle equipped with stirring, condenser and tail gas absorption device, and the temperature was raised to 60°C. Tail gas is absorbed by falling film water in three stages in series, 80L of water is added to each stage, and the absorption temperature is 10-55°C.

[0028] The temperature of the reaction kettle was controlled at 60-65°C, and 261Kg of trifluorochrysanthemum acid chloride was started to be added dropwise into the synthesis kettle for 3 hours. After the dropwise addition was completed, the reaction was incubated for 6 hours. At the end of the heat preservation reaction, the conversion rate of 2-methyl-3-phenylbenzyl alcohol in Zhongkong was 99.7%. 115.0Kg of hydrochloric acid with a content of 30.23% is recovered in the first stage of tail gas absorption.

[0029] The materials in the synthesis kettle were discharged into the crystallization kettle to cool down a...

Embodiment 3

[0031] 198Kg of 2-methyl-3-phenylbenzyl alcohol and 790Kg of cyclohexane were put into a 2000L synthesis kettle equipped with stirring, condenser and tail gas absorption device, and the temperature was raised to 45°C. Tail gas is absorbed by falling film water in three stages in series, adding 80L of water to each stage, and the absorption temperature is 10-60°C.

[0032] The temperature of the reaction kettle was controlled at 45-55°C, and 261Kg of trifluorochrysanthemum acid chloride was started to be added dropwise into the synthesis kettle for 3 hours. After the dropwise addition was completed, the reaction was incubated for 6 hours. At the end of the heat preservation reaction, the conversion rate of 2-methyl-3-phenylbenzyl alcohol in Zhongkong was 99.2%. 115.2Kg of hydrochloric acid, with a content of 30.16%, was recovered in the first stage of tail gas absorption.

[0033] The material in the synthesis kettle was discharged into the crystallization kettle to cool down...

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Abstract

The invention provides a method for producing bifenthrin with a clean synthesizing process. According to the method, 3-(2-chloro-3,3,3-trifluoro-1-allyl)-2,2-dimethylcyclopropane formyl halide and 2-methyl-3-biphenylmethanol are adopted to directly react in one solvent or mixed solvent of more than two solvents in favor of overflow of halogen hydride, halogen hydride generated in the reaction is removed from tail gas in time by means of negative pressure, and the product is directly cooled and crystallized to obtain bifenthrin. The reaction equation is as shown in a formula (3), wherein X is Cl or Br. The production method has the characteristics of high product content, simple process flow, small output of the 'Three Wastes' and the like, and accords with the requirement for clean production.

Description

technical field [0001] The invention relates to a production method of a pyrethrin compound, in particular to a production method of bifenthrin. . Background technique [0002] Pyrethroid insecticides are one of the pillar products in today's global sanitation insecticide market. They have the characteristics of high efficiency, broad spectrum, low toxicity, and low residue. Since pyrethroid insecticides are simulants of natural products, they are easy to decompose in nature, not easy to pollute the environment after use, easy to metabolize in animals, have no accumulation effect, and will not be enriched through bioconcentration, so they have little impact on the ecosystem . [0003] Bifenthrin, also known as Uranus, Chrysanthemum, Bifenning, etc., is a highly efficient pyrethroid insecticide and acaricide, mainly used to control various Lepidoptera larvae, whiteflies, aphids, More than 20 kinds of pests such as herbivorous spider mites. Bifenthrin has fast knockdown sp...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/743C07C67/14
CPCC07C67/14C07C2601/02
Inventor 戚明珠周景梅徐海鹏范剑峰唐伟花越如杨宗志
Owner JIANGSU YANGNONG CHEM
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