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Salts of dialkylphosphinic acid, preparation method and application

A technology of dialkyl phosphinate and dialkyl phosphinic acid, applied in the field of dialkyl phosphinate, can solve the problem of easy quenching and inactivation reaction yield of free radicals, environmental pollution by waste, and large input of raw materials. and other problems, to achieve the effect of novel synthetic route, high purity, and avoidance of danger

Active Publication Date: 2014-12-24
KINGFA SCI & TECH CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] However, the above method has the following defects: the addition of olefins with hypophosphorous acid will generate monoalkylphosphinate by-products while obtaining dialkylphosphinate; Low, resulting in large input of raw materials and low output, and produces a large amount of waste to pollute the environment

Method used

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  • Salts of dialkylphosphinic acid, preparation method and application
  • Salts of dialkylphosphinic acid, preparation method and application
  • Salts of dialkylphosphinic acid, preparation method and application

Examples

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preparation example Construction

[0037] The present invention discloses a preparation method of dialkyl phosphinate represented by formula (I), comprising the following steps:

[0038]

[0039] (I);

[0040] Wherein, R is an alkyl group with 1 to 12 carbon atoms; n=2 or 3; M is a metal ion;

[0041] (1) Preparation of dihydroxyalkyl hypophosphorous acid: reaction of hypophosphorous acid and aldehyde in water to obtain dihydroxyalkyl hypophosphorous acid;

[0042] (2) Preparation of dialkylphosphinic acid: the hydroxyl group of dihydroxyalkylphosphinic acid is reduced by reducing agent to obtain dialkylphosphinic acid solution;

[0043] (3) Preparation of dialkylphosphinic acid salt: react the dialkylphosphinic acid solution obtained in step (2) with an aqueous metal salt solution to obtain a solid, which is cooled, filtered, washed with water, and dried to obtain a dialkylphosphinic acid solution. Phosphonates.

[0044] Wherein, the preparation of step (1) dihydroxyalkyl hypophosphorous acid can also ob...

Embodiment 1

[0049] (1) Preparation of bishydroxymethylphosphinic acid

[0050] In a 500mL four-necked flask equipped with a stirrer and a reflux condenser, add 159g (1.5mol) sodium hypophosphite monohydrate, 100mL deionized water, 135mL (1.55mol) 36% hydrochloric acid and 93g (3.1mol) Paraformaldehyde was stirred and reacted at 60°C for 10 hours to obtain 487g of bismethylolphosphinic acid aqueous solution, which contained 36.4% of bismethylolphosphinic acid (M=126), and the yield was 93%.

[0051] After purification, the product is analyzed by infrared spectrum: there are absorptions at υ(cm- 1 ) = 475, 769, 856, 1035, 1091, 1151, 1310, 1422, 1635, 2900 and 3406.

[0052] (2) Preparation of dimethylphosphinic acid

[0053] Take 200ml of bishydroxymethylphosphinic acid (0.578mol) aqueous solution, concentrate under reduced pressure to 100ml, add 50ml of 57% hydroiodic acid (d=1.7), 60g of red phosphorus, and reflux at 126°C for 15 hours. Cool, extract 3 times with 50ml of chloroform, comb...

Embodiment 2

[0058] (1) Preparation of bishydroxymethylphosphinic acid

[0059] In a 500mL four-necked flask equipped with a stirrer and a reflux condenser, 198g (1.5mol) of 50% hypophosphorous acid, 120mL deionized water and 86g (3.1mol) of paraformaldehyde were added, and the reaction was stirred at 60°C for 10h to obtain 400 g of bismethylolphosphinic acid aqueous solution contained 42.5% of bismethylolphosphinic acid (M=126) according to liquid chromatography analysis, and the yield was 90%.

[0060] Infrared spectrum (IR) after purification of the product: there are absorptions at υ(cm-1) = 475, 769, 856, 1035, 1091, 1151, 1310, 1422, 1635, 2900, 3406.

[0061] (2) Preparation of dimethylphosphinic acid

[0062] Take 200ml of bishydroxymethylphosphinic acid (0.675mol) aqueous solution, concentrate under reduced pressure to 100ml, add 60ml of 57% hydroiodic acid (d=1.7), 70g of red phosphorus, and reflux at 126°C for 15 hours. Cooled, extracted 3 times with 50ml of chloroform, combin...

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Abstract

The invention discloses a preparation method and an application of salts of dialkylphosphinic acid, the salts of dialkylphosphinic acid has a structure shown in a formula (I). The preparation method of the salts of dialkylphosphinic acid comprises the following steps: hypophosphorous acid or hypophosphites are reacted with aldehyde in an aqueous solution to obtain di(alpha-hydroxy)alkyl hypophosphorous acid, hydroxy is reduced through HI / P to obtain an dialkylphosphinic acid solution, and the dialkylphosphinic acid solution and metal salt are reacted to obtain the corresponding salts of dialkylphosphinic acid. The preparation method of salts of dialkylphosphinic acid has the advantages of high yield, simple synthesis process and convenient operation, and substantially reduces production cost, simplifies production equipment and enhances the security of production process.

Description

technical field [0001] The invention relates to the field of organic synthesis, in particular to a dialkyl phosphinate, its preparation method and application. Background technique [0002] Polymer materials (plastic, rubber, chemical fiber, etc.) are widely used in construction industry, automobile industry, medical and health care, household appliances and other fields. Polymer materials are usually flammable or combustible, and the requirements for their flame retardancy are getting higher and higher in practical applications. In order to ensure the safety of synthetic materials, the most effective way is to add flame retardants. [0003] Dialkyl phosphinate is a commonly used flame retardant, the higher the content of phosphorus in dialkyl phosphinate, the better the flame retardant effect. In the prior art, for the synthesis of small molecular alkyl hypophosphite technology, free radicals are used to initiate the reaction with ethylene. For example, Hoechst AG of Germ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F9/30C08L67/02C08K13/04C08K7/14C08K5/5313
Inventor 柴生勇蔡彤旻曾祥斌叶南飚李积德孔蕾陈林
Owner KINGFA SCI & TECH CO LTD
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