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Method for preparing dialkylphosphinate through oxidation reduction initiation system

A technology of alkyl phosphinate and dialkyl phosphinic acid is applied in the field of preparation of dialkyl phosphinate by redox initiation system, which can solve the problems of long process, explosion and production of dialkyl phosphinate. Low yield and other problems, to achieve high yield, avoid danger, the effect of low temperature

Inactive Publication Date: 2013-12-25
PRESAFER QINGYUAN PHOSPHOR CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] However, in the prior art, the process of preparing dialkylphosphinate by reaction is often very long, and, due to the reason of the initiator system itself, the reaction The temperature must be very high, which is likely to cause dangers such as explosions. At the same time, at high temperatures, the probability of side reactions is greatly increased, and the yield is often not high.

Method used

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  • Method for preparing dialkylphosphinate through oxidation reduction initiation system
  • Method for preparing dialkylphosphinate through oxidation reduction initiation system

Examples

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Embodiment 1

[0030] 1) Dissolve 530g of sodium hypophosphite monohydrate and 12.11g of benzoyl peroxide in 2500g of acetic acid, then move the solution to a 5L enamel autoclave, start stirring and heating, when the temperature rises to 60°C, then pass in ethylene Gas, so that the pressure in the kettle reaches 1.0MPa and is maintained at this pressure, 7.46g N, N-diethylaniline solution dissolved in 250g acetic acid is evenly added to the kettle with a pressure of 1.0MPa within 4 hours, and the temperature in the kettle is maintained. The reaction was continued at 60° C. for 1 h, and the pressure in the kettle was released.

[0031] 2) Distill the mixture obtained in 1) to remove acetic acid under reduced pressure, then add water until clarified, and add 403.31g of aluminum chloride hexahydrate solution dissolved in 1000g of water within 1h to obtain a slurry. Suction filter the slurry, wash the filter cake, and dry at 120°C to obtain 624.65 g of aluminum diethylphosphinate with a yield of...

Embodiment 2

[0035] 1) Dissolve 530g of sodium hypophosphite monohydrate and 12.32g of cyclohexanone peroxide in 2500g of acetic acid, then move the solution to a 5L enamel autoclave, start stirring and heating, when the temperature rises to 60°C, then pass in ethylene Gas, so that the pressure in the kettle reaches 1.0MPa and is maintained at this pressure, 6.09g N, N-dimethylaniline solution dissolved in 250g acetic acid is evenly added to the kettle with a pressure of 1.0MPa within 4 hours, and the temperature in the kettle is maintained. The reaction was continued at 60° C. for 1 h, and the pressure in the kettle was released.

[0036] 2) Distill the mixture obtained in 1) to remove acetic acid under reduced pressure, then add water until clarified, and add 559.6g of aluminum sulfate octadecahydrate dissolved in 1000g of water within 1h. Suction filter the slurry, wash the filter cake, and dry at 120°C to obtain 622.31 g of aluminum diethylphosphinate with a yield of 95.7%.

Embodiment 3

[0038] 1) Dissolve 530g of sodium hypophosphite monohydrate and 7.31g of di-tert-butyl peroxide in 2500g of acetic acid, then move the solution to a 5L enamel autoclave, start stirring and heating, when the temperature rises to 70°C, then pass in ethylene gas , so that the pressure in the kettle reaches 1.0MPa and is maintained at this pressure, 10.20g N, N-dibutylaniline solution dissolved in 250g acetic acid is evenly added to the kettle with a pressure of 1.0MPa within 4h, and the temperature in the kettle is kept at 70 The reaction was continued at ℃ for 1 h, and the pressure in the kettle was released.

[0039] 2) Distill the mixture obtained in 1) to remove acetic acid under reduced pressure, then add water until clarified, and add 626.5g of aluminum nitrate nonahydrate solution dissolved in 1000g of water within 1h to obtain a slurry. Suction filter the slurry, wash the filter cake, and dry at 120°C to obtain 627.34 g of aluminum diethylphosphinate with a yield of 96.5%...

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Abstract

The present invention discloses a method for preparing dialkylphosphinate through an oxidation reduction initiation system. The method comprises that: 1) in the presence of a peroxide initiator and a reduction agent, hypophosphrous acid and / or an alkali metal salt thereof and olefin are subjected to a reaction in a solvent to obtain a mixture containing dialkyl hypophosphrous acid and / or an alkali metal salt thereof; and 2) the solvent in the obtained mixture is removed, water is added to obtain an aqueous solution containing the dialkyl hypophosphrous acid and / or the alkali metal salt thereof, a metal salt is added to carry out a reaction to obtain a slurry, and separation, purification and drying are sequentially performed to obtain the finished product. The production method has the following characteristics that: the process time is short, the temperature is not high, risk of the reaction at the high temperature is avoided, and the prepared product has characteristics of good performance and high yield.

Description

technical field [0001] The invention relates to a method for preparing dialkyl phosphinate with a redox initiation system. Background technique [0002] Organic phosphinate is a new type of organic phosphorus flame retardant. The flame retardant products produced by it have the advantages of low product density, less flame retardant addition, good mechanical properties, good color and low smoke density, and are widely used. for attention. It is widely used in connectors and switch components made of PA and PBT, rigid and flexible printed circuit boards, solder masks, solder masking coatings, automotive and electronic industry components, etc. It has broad application prospects in the electrical and electronic industry. And it is especially suitable for thin-walled electronic components, transparent sheets and films. [0003] In the prior art, the methods for preparing dialkylphosphinates include the use of azo compounds to generate alkenes in situ, and the addition reactio...

Claims

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Application Information

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IPC IPC(8): C07F9/30
Inventor 刘永亮陈志钊周侃
Owner PRESAFER QINGYUAN PHOSPHOR CHEM