Three-waste-free preparation method for bifenthrin

A technology of bifenthrin and three wastes, which is applied in the field of bifenthrin synthesis, can solve the problems of excessive waste water, low yield, and serious discharge of three wastes, and achieve the effects of simple process, high total yield and low cost

Active Publication Date: 2013-06-12
盐城市大丰区生产力促进中心
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This method produces a large amount of difficult-to-handle hydrogen chloride and sulfur dioxide gas in the process of preparing kung fu acid chloride, and in the second step of synthesizing bifenthrin, a large amount of saline waste water is generated. The three wastes are very serious in the whole production and preparation process.
U.S. patent (US4341796) uses 2-methyl-3-chloromethylbiphenyl in an acid-binding agent and a suitable solvent to chemically react with kung fu acid to generate bifenthrin, although there is no large amount of hydrogen chloride and sulfur dioxide gas that is difficult to handle Produced, but the yield is low and the waste water is much

Method used

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Examples

Experimental program
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Effect test

Embodiment 1

[0022] A, esterification reaction prepares methyl kung fu acid

[0023] The esterification reaction formula is as follows:

[0024]

[0025] See figure 1 , put into 500kg kungfu acid, 500kg methanol, 5kg sulfuric acid in the esterification reactor 1, pass into the interlayer 1-1 to heat with steam, open the stirrer; control the temperature of the material in the esterification reactor 1 to rise to 65 ° C, Part of methanol participates in the reaction to generate methyl kung fu acid and water, and as the reaction progresses, the temperature slowly rises to 70°C. The water generated by the esterification reaction is carried by methanol and evaporated from the top of the esterification reactor 1, and then passed into the rectification tower 5. The bottom of the rectification tower 5 is heated by steam from the reboiler 7, the reflux ratio is adjusted in time, and the temperature at the top of the tower is controlled at 64.5°C. The methanol distilled from the top of the towe...

Embodiment 2

[0032] In the esterification reaction still, drop into 500kg kongfuic acid, 700kg methyl alcohol, 5kg sulfuric acid, temperature of reaction is 60~65 ℃, reacts 21 hours, other conditions are identical with embodiment 1 step a, make colorless transparent methyl kongic acid liquid. Yield 97.9%, content ≥99.3% (GC normalization method).

[0033] In the transesterification reaction, feed materials according to step b of Example 1, control the negative pressure in the transesterification reactor to 0.079-0.081MPa, and the temperature is 59-61°C, and the other conditions are the same as step b of Example 1 to obtain white powder Bifenthrin, with a content of 98.2% (GC internal standard method), a conversion rate of 94%, and a total yield of 98.5%.

Embodiment 3

[0035] Prepare the solid acid catalyst as follows: Soak the coarse-porous microsphere silica gel with an average pore diameter of 8.0-12.0nm in a sulfuric acid solution with a mass concentration of 50%, and after 1 hour, bake at 100°C for 3 hours to obtain sulfuric acid-silica gel microspheres (that is, sulfuric acid solid acid supported by silica gel). Use sulfuric acid solid acid instead of the sulfuric acid in step a of Example 1 to carry out the esterification reaction. The esterification reaction temperature rises to 65°C, and then slowly rises to 75°C. After the esterification reaction is completed, the catalyst is directly filtered out and reused in the following For batch production, the filtrate is directly put into the distillation kettle (neutralization with powdery sodium carbonate is not required), and methanol is distilled off under negative pressure, and the 134-137°C / 0.095MPa fraction is collected to obtain a colorless and transparent methyl kung fu acid liquid....

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Abstract

The invention relates to a three-waste-free preparation method for bifenthrin. The method comprises the following steps of: subjecting cyclopropanecarboxylic acid, methanol and an acid catalyst to an esterification reaction at the temperature of 60-80 DEG C according to the mole ratio of 1:(3-9):(0.01-0.03) to generate methyl cyclopropanecarboxylic acid and water, evaporating the methanol and water, dehydrating, and then enabling the methanol to return to a reaction kettle; and removing the catalyst in the materials after the esterification reaction, distilling at the negative pressure of 0.07-0.095MPa and the temperature of 30-70 DEG C to obtain the methyl cyclopropanecarboxylic acid, mixing the methyl cyclopropanecarboxylic acid, biphenylylmethylcarbinol and a basic catalyst according to the mole ratio of 1:(0.5-2):(0.003-0.01), carrying out transesterification at the negative pressure of 0.065-0.08MPa and the temperature of 50-70 DEG C to generate bifenthrin and methanol, distilling the materials to remove the methanol, then dissolving the materials into an organic solvent, separating out a crystal at the temperature ranging from -5 DEG C to 5 DEG C, centrifuging to obtain a bifenthrin product, distilling a mother liquid to separate the organic solvent, and respectively recycling the organic solvent and a residual liquid. The three-waste-free preparation method is simple in process and high in total yield; a great number of harmful wastes are not generated in the preparation process, and the separated water, methanol and organic solvent are all recycled so that no environment pollution is caused.

Description

technical field [0001] The invention relates to a method for synthesizing bifenthrin, a compound used as a pesticide raw material, in particular to a method for preparing bifenthrin without three wastes. Background technique [0002] Bifenthrin, chemical name: (Z)-(1RS,3RS)-2,2-dimethyl-3-(2-chloro-3,3,3-trifluoro-1-propenyl)cyclopropanecarboxylic acid -2-Methyl-3-phenylbenzyl ester, invented by FMC Corporation of the United States in the 1980s, is one of the excellent pesticide varieties with a wide insecticidal spectrum, high efficiency, quick action and low toxicity among pyrethroid pesticides. Bifenthrin is mainly used to control pests on cotton, vegetables, fruit trees, tobacco, tea trees and other plants. Its mode of action is mainly contact and stomach poisoning, and it has been widely used at present. [0003] At present, most of the preparations of bifenthrin are firstly reacted with kauric acid and thionyl chloride to generate kungfu acid chloride, and then reacte...

Claims

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Application Information

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IPC IPC(8): C07C69/743C07C67/03
CPCY02P20/584
Inventor 姜诚朱光华
Owner 盐城市大丰区生产力促进中心
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