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Chemical synthesis method of diphenyl chlorophosphate

A technology of diphenyl chlorophosphate and diphenyl phosphate, which is applied in the field of chemical synthesis of diphenyl chlorophosphate, can solve the problems of high production cost, equipment corrosion, high corrosion, etc., and achieve great economic value and environmental protection value, product The effect of high yield and quality and mild reaction conditions

Inactive Publication Date: 2019-09-17
HEZE DIJADE CHEM CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] This process method uses phosphorus oxychloride, which seriously corrodes the equipment, and a large amount of high-phosphorus wastewater is difficult to treat, resulting in serious pollution; at the same time, there are many by-products in this process, which requires high-vacuum high-temperature distillation products, high energy consumption, and large amounts of distillation residues. solid waste
This method has problems such as high corrosion, high energy consumption, high pollution, low yield, high production cost and other problems that need to be solved urgently

Method used

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  • Chemical synthesis method of diphenyl chlorophosphate
  • Chemical synthesis method of diphenyl chlorophosphate
  • Chemical synthesis method of diphenyl chlorophosphate

Examples

Experimental program
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Effect test

Embodiment 1

[0030] Put 120g of dichloromethane and 7.3g of N,N-dimethylformamide into a 500ml four-necked reaction flask equipped with a thermometer, reflux condenser and mechanical stirring, stir and control the temperature below 10°C, and put in 28g of bis(trichloro Methyl)carbonate, add a solution of 50g diphenyl phosphate and 120g dichloromethane, after the addition is complete, react for 3 hours, after the detection reaction is completed, control the temperature below 10°C, slowly add 20g of water, stir and separate, and the organic phase Dry with anhydrous sodium sulfate; filter to remove the desiccant, evaporate the filtrate to remove dichloromethane at normal pressure, cool to 0°C, filter to remove insoluble matter, and obtain 48.9 g of diphenyl chlorophosphate, with a purity of 99.2% and a yield of 90.3% by GC .

Embodiment 2

[0032] Put 120g of dichloromethane and 3.6g of N,N-dimethylformamide into a 500ml four-necked reaction flask equipped with a thermometer, reflux condenser and mechanical stirring, stir and control the temperature below 10°C, and put 28g of bis(trichloro Methyl)carbonate, add a solution of 50g diphenyl phosphate and 120g dichloromethane, after the addition is complete, react for 3 hours, after the detection reaction is completed, control the temperature below 10°C, slowly add 20g of water, stir and separate, and the organic phase Dry with anhydrous sodium sulfate; filter to remove the desiccant, evaporate the filtrate to remove dichloromethane at normal pressure, cool to 0°C, filter to remove insoluble matter, and obtain 47.2g of diphenyl chlorophosphate, the purity of GC detection is 98.1%, and the yield is 86.2% .

Embodiment 3

[0034] Put 330g of dichloromethane and 7.3g of N,N-dimethylformamide into a 500ml four-necked reaction flask equipped with a thermometer, a reflux condenser and mechanical stirring, stir and control the temperature below 10°C, and put in 28g of bis(trichloro Methyl)carbonate, add 55g of diphenyl phosphate sodium salt in batches, after the addition, react for 5 hours, after the detection reaction is completed, control the temperature below 10°C, slowly add 20g of water, stir and separate, and use anhydrous sulfuric acid for the organic phase Sodium drying; filter to remove the desiccant, evaporate the filtrate to remove dichloromethane at normal pressure, cool to 0°C, filter to remove insoluble matter, and obtain 47.5 g of diphenyl chlorophosphate, with a purity of 99.3% by GC and a yield of 87.8%.

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Abstract

The invention relates to a synthesis method of diphenyl chlorophosphate. The method comprises the following steps: by taking certain amount of organic ammonia as a catalyst, mixing certain amount of diphenyl phosphate or diphenyl phosphate salt or mixing both at any proportion, and reacting with certain amount of bis(trichloromethyl)carbonate ester in an organic solvent for 1-10h, wherein the reaction temperature is 0-60 DEG C, and the diphenyl phosphate salt is sodium diphenyl phosphate or potassium diphenyl phosphate; after the reaction in the step 1) is over, cooling, washing and drying the product drying; performing normal-pressure or reduced-pressure recovery of solvent; cooling to filter out insolubles to obtain diphenyl chlorophosphate. The method provided by the invention has the following beneficial effects: the process line is simple, the reaction conditions are mild, the aftertreatment energy consumption is low, high-vacuum and high-temperature distillation is not needed, the production cost is low, and the product yield and quality are both relatively high; meanwhile, the problem of generation of much phosphorous-containing wastewater and solid waste is avoided.

Description

technical field [0001] The invention relates to the technical field of chemical industry, in particular to a chemical synthesis method of diphenyl chlorophosphate. Background technique [0002] Diphenyl chlorophosphate is an important intermediate used in the synthesis of penem drugs, phosphorus-containing flame retardants and liquid crystal materials, such as the production of drugs such as meropenem and 4-biphenoxy diphenyl phosphate. [0003] Before the present invention was given, the chemical synthesis methods of diphenyl chlorophosphate in the prior art mostly used phosphorus oxychloride and phenol as raw materials, and synthesized under Lewis acid catalysis. [0004] The synthetic route is as follows: [0005] [0006] Such as: Chemical Research 2012, 23 (6) proposed to use 0.8g of anhydrous aluminum trichloride and 15.3g of phosphorus oxychloride to raise the temperature to 60°C, and add dropwise a mixture of 10ml of dichloroethane and 18.8g of phenol into the re...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/14
CPCC07F9/1406
Inventor 张文杰王尚启李娟尚杰超丁红军
Owner HEZE DIJADE CHEM CORP