Preparation method for dialkyl phosphinates

A technology of dialkyl phosphinate and dialkyl phosphinic acid, which is applied in the field of preparation of dialkyl phosphinate, can solve the problem of unwanted telomer formation, decreased product yield, low product purity, etc. problems, to avoid the reduction of yield and purity, avoid the formation of telomers, and reduce the effect of reaction temperature

Active Publication Date: 2013-02-13
ZHEJIANG XINHUA CHEM
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AI Technical Summary

Problems solved by technology

The reaction of this method is complicated, and the product obtained is a mixture with complex components, which is difficult to purify, and the product purity is very low, and the productive rate of dialkylphosphinic acid is only 16%.
[0004] CN98811626, CN98811627, etc. disclose to use phosphinate and olefins as raw materials, react to prepare dialkyl phosphinate under the action of initiator, the advantage of this reaction is that can obtain dialkyl phosphinate in high yield products, but must be recovered through complex processes due to the use of organic solvents in the reaction, and undesired formation of telomers due to the high solubility of olefins in organic solvents
Moreover, the presence of telomers and traces of organic solvents in the product can have undesirable side effects on plastics
CN200410104692 etc. disclose the method for preparing dialkyl hypophosphite under the condition of not using organic solvent, but need higher reaction temperature and longer reaction time, and product yield obviously drops

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  • Preparation method for dialkyl phosphinates

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Experimental program
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Effect test

Embodiment 1

[0031] Dissolve 300g of sodium hypophosphite monohydrate and 12g of sodium bisulfite in 1500g of water, then add it to the autoclave, replace it with nitrogen three times, start stirring, raise the temperature to 100°C, pass ethylene into the reactor, pass through the pressure reducing valve The pressure in the control kettle is about 0.6MPa. Dissolve 10g of 2,2'-azobis(2-amidinopropane) dihydrochloride in 100g of water, and continuously and evenly add it to the reactor within 6 hours. After the addition, the reaction was carried out at constant temperature and pressure for 1 hour to obtain sodium dialkylphosphinate.

[0032] Transfer the mixed solution of sodium dialkylphosphinate obtained above into a reactor equipped with a thermometer, stirring, condensing reflux pipe and dripping device, heat to 100°C, and then dissolve 350g of hexadecanohydrate sulfuric acid in 600g of water Aluminum was evenly added through the dropping funnel within 2 hours, refluxed for about 2 hours...

Embodiment 2

[0035] Dissolve 300g of sodium hypophosphite monohydrate and 20g of potassium bisulfite in 1000g of water, then add it to the autoclave, replace it with nitrogen three times, start stirring, raise the temperature to 120°C, pass ethylene into the reactor, pass through the pressure reducing valve The pressure in the control kettle is about 0.8MPa. Dissolve 12g of dibenzoyl peroxide in 100g of water, and continuously and evenly add it to the reaction kettle within 5 hours. After the addition, the reaction was carried out at constant temperature and pressure for 1 hour to obtain sodium dialkylphosphinate.

[0036] Transfer the mixed solution of sodium dialkylphosphinate obtained above into a reactor equipped with a thermometer, stirring, condensing reflux tube and dripping device, heat to 90°C, and then dissolve 350g of hexadecanohydrate sulfuric acid in 600g of water Aluminum was evenly added through the dropping funnel within 2 hours, refluxed for about 2 hours, cooled and filt...

Embodiment 3

[0040]Dissolve 350g of sodium hypophosphite monohydrate and 18g of sodium sulfite in 1000g of water, then add it to the autoclave, replace it with nitrogen three times, start stirring, raise the temperature to 120°C, feed ethylene into the reactor, and control the pressure inside the autoclave through a pressure reducing valve. The pressure is about 0.7MPa. Dissolve 12g of potassium persulfate in 100g of water, and continuously and evenly add to the reaction kettle within 5 hours. After the addition, the reaction was carried out at constant temperature and pressure for 1 hour to obtain sodium dialkylphosphinate.

[0041] Transfer the mixed solution of sodium dialkylphosphinate obtained above into a reactor equipped with a thermometer, stirring, condensing reflux pipe and dripping device, heat to 100°C, and then dissolve 420g of hexadecanohydrate sulfuric acid in 700g of water Aluminum was evenly added through the dropping funnel within 2 hours, refluxed for about 2 hours, coo...

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Abstract

The invention relates to a preparation method for dialkyl phosphinates, and belongs to the field of green and environment-friendly fire retardant. The preparation method for dialkyl phosphinates comprises the following technical steps: (1) preparing dialkyl phosphinic acid and / or alkali metal salt of dialkyl phosphinic acid; and (2) preparing dialkyl phosphinates. The preparation method adopts the water as the reaction solvent, so that the organic solvent residual in a product can be avoided, and the generation of telomere can be obviously reduced and even avoided, and as a result, the purity of the product can be ensured. Special assistant is added in the preparation method, so that the reaction temperature is reduced, the reaction time is reduced, and the energy consumption is also reduced while the yield and purity of dialkyl phosphinic acid and / or the alkali metal salt of dialkyl phosphinic acid are ensured.

Description

technical field [0001] The invention relates to a preparation method of dialkyl phosphinate, which belongs to the field of green and environment-friendly flame retardants. technical background [0002] With people's increasing awareness of environmental protection, safety and health, countries around the world have begun to focus on the research, development and application of environmentally friendly flame retardants. has been widely used. [0003] Dialkylphosphinates as flame retardants can be prepared by various methods. For example, US601172 and CN1280581 disclose taking yellow phosphorus and alkyl halide as raw materials, reacting in the mixed system of aqueous solution of alkali metal hydroxide or alkaline earth metal hydroxide and organic solvent, prepare alkyl phosphinic acid and alkyl phosphinic acid . The reaction of this method is complicated, and the product obtained is a mixture with complex components, which is difficult to purify, the product purity is very...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/30C09K21/12
Inventor 刘承伟谢自强王卫明李道权祝航黄斌钟启刚邵卫平王爱民
Owner ZHEJIANG XINHUA CHEM
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