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Preparation method of dialkyl phosphinate with high thermal stability

A technology of dialkyl phosphinate and alkyl phosphinate, applied in the field of preparation of dialkyl phosphinate, can solve problems such as poor thermal stability, achieve good thermal stability, high weight loss temperature, Solve the effect of easy fading

Inactive Publication Date: 2013-06-26
ZHUHAI WANTONG CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] In order to overcome the problem of poor thermal stability of existing dialkyl phosphinates, the object of the present invention is to provide a method for preparing dialkyl phosphinates with high thermal stability

Method used

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  • Preparation method of dialkyl phosphinate with high thermal stability
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  • Preparation method of dialkyl phosphinate with high thermal stability

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0045] 1.1 Preparation of aluminum diethyl hypophosphite

[0046] Dilute 183g (1.2mol) 80% diethylphosphinic acid solution with water to 418.3g 35% diethylphosphinic acid solution, heat to 85°C, add 3mol 30% sulfuric acid solution to make the solution pH<1, Add 444g of a mixture of 30% by mass aluminum sulfate (M=666) and water dropwise within 45min, stir and react for 45min, a white solid is formed, cool and filter to obtain 129g of filter cake, the water content of the filter cake is 40%, and 1713g of filtrate is obtained , The filtrate is recycled. The precipitate was washed with 3L of deionized water, and dried at 200°C for 10 hours to obtain 78.0 g of aluminum diethylphosphinate, with a yield of 50.0% and a moisture content of 0.6%.

[0047] Tap density (g / L): 602; TG: 1% weight loss temperature 368°C, 5% weight loss temperature 423°C.

[0048] IR: 779cm -1 , 1077 cm -1 , 1152cm -1 , 2881 cm -1 , 2959 cm -1

[0049] 1.2 Example 1.1 Filtrate recovery and prepar...

Embodiment 2

[0058] Prepare aluminum diethylphosphinate as in Example 1, heat 610g (1.5mol) of 30% diethylphosphinic acid solution to 70°C, add 1.875mol of 99% sulfuric acid solution to make the solution pH<1, within 30min Add dropwise 333g of a mixture of 50% by mass aluminum sulfate (M=666) and water, stir for 50 minutes to generate a white solid, cool, filter, and recycle the filtrate, wash the precipitate with 4L of deionized water, and dry at 200°C for 10 hours , to obtain 114.3 g of aluminum diethylphosphinate, with a yield of 58.6% and a moisture content of 0.4%.

[0059] Tap density (g / L): 601; TG: 1% weight loss temperature 378°C, 5% weight loss temperature 428°C.

Embodiment 3

[0061] Prepare aluminum diethylphosphinate as in Example 1, heat 732g (0.6mol) of 10% diethylphosphinic acid solution to 100°C, add 0.3mol of 60% sulfuric acid solution to make the solution pH<1, within 30min Add dropwise 333g of a mixture of 20% by mass aluminum sulfate (M=666) and water, stir for 0.1h to generate a white solid, cool, filter, and recycle the filtrate, wash the precipitate with 3L of deionized water, and dry at 200°C After 10 hours, 48.4 g of aluminum diethylphosphinate was obtained, with a yield of 62.0% and a moisture content of 0.3%.

[0062] All the other steps are the same as 1.2 and 1.3 in Example 1, and the final product total yield is 96.3%.

[0063] Tap density (g / L): 660; TG: 1% weight loss temperature 390°C, 5% weight loss temperature 440°C.

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Abstract

The invention discloses a preparation method of dialkyl phosphinate with high thermal stability. The preparation method comprises the following steps of: (a), adding strong acid to dialkyl phosphinic acid and / or a dialkyl phosphinic acid alkali metal salt aqueous solution to obtain dialkyl phosphinic acid and / or the dialkyl phosphinic acid alkali metal salt aqueous solution with pH lower than 1; (b), reacting a mixture of a metal compound and water with the dialkyl phosphinic acid and / or the dialkyl phosphinic acid alkali metal salt aqueous solution with the pH lower than 1 to generate dialkyl phosphinic acid metal salt, wherein the pH of the solution after the reaction is lower than 1; and (c), filtering, recycling the filtrate, washing and drying the filter cake to obtain the corresponding dialkyl phosphinate. The product prepared by the preparation method disclosed by the invention has a high TG1% weight loss temperature and a high TG5% weight loss temperature and good thermal stability, and is heated up for 8 hours at 250 DEG C without changing color and carbonizing, so that the problems that the flame retardant is easy to fade and easy to decompose in a resin processing process are radically solved.

Description

technical field [0001] The invention belongs to the technical field of flame retardant synthesis, and in particular relates to a preparation method of a dialkyl phosphinate with high thermal stability. Background technique [0002] Polymer materials (plastic, rubber, chemical fiber, etc.) are widely used in the construction industry, automobile industry, medical and health care and household appliances. However, 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 and meet the requirements of environmental protection, the most effective method is to add halogen-free flame retardants to synthetic materials. [0003] Since Hoechst AG of Germany reported in European patent EP0699708 in 1995 that aluminum dialkylphosphinate and calcium dialkylphosphinate were used as flame retardants in polyester molding compositions ,...

Claims

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Application Information

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IPC IPC(8): C07F9/30C08K5/5313C08K7/14C08L67/02C08L77/06
Inventor 卢昌利柴生勇李积德孔蕾陈林
Owner ZHUHAI WANTONG CHEM
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