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Partially alkylated phosphinic acid nonalkali metal salt and preparing method and application thereof

A technology of alkylating phosphinic acid and alkali metal salt, applied to the application of partially alkylated phosphinic acid non-alkali metal salt in polymer flame retardancy, partially alkylated phosphinic acid non-alkali metal salt and its In the field of preparation, it can solve the problems of high requirements for reaction equipment and cumbersome steps, and achieve the effect of simple equipment requirements, simple process and few by-products

Inactive Publication Date: 2010-06-23
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method has the advantages of rich sources of raw materials, but also has the disadvantages of cumbersome steps and high requirements for reaction equipment.

Method used

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  • Partially alkylated phosphinic acid nonalkali metal salt and preparing method and application thereof
  • Partially alkylated phosphinic acid nonalkali metal salt and preparing method and application thereof
  • Partially alkylated phosphinic acid nonalkali metal salt and preparing method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Weigh 600g of aluminum hypophosphite into a 5L reactor filled with 2.5L of deionized water, stir and disperse evenly. Weigh 10g of ammonium persulfate and add water to configure an initiator solution with a mass percent solubility of 3%, and put the initiator solution on the reaction kettle. Heating so that the temperature rises to 105°C after 30 minutes, start filling isobutene gas, and start adding the initiator solution dropwise when the pressure is stabilized at 0.01 MPa, and add it uniformly within 8 hours. 10 minutes after the initiator was added dropwise, stop aerating and turn off the heating device, stop stirring after 30 minutes, open the reaction kettle, filter the obtained solid-liquid mixture, and dry in an oven at 105°C for 5 hours to obtain 1198.1g of white fluid powder. Molecular formula H 2 (C 4 h 9 ) 4 P 3 o 6 Al: phosphorus content is 20.8%; X-ray electron spectrum: phosphorus content is 20.6%.

Embodiment 2

[0036]Weigh 600g of aluminum hypophosphite into a 5L reactor filled with 2.5L of deionized water, stir and disperse evenly. Weigh 8g of ammonium persulfate and add water to configure an initiator solution with a mass percentage solubility of 3%, and put the initiator solution on the reaction kettle. Heating so that the temperature rises to 65°C after 30 minutes, start filling isobutylene gas, and start adding the initiator solution dropwise when the pressure is stabilized at 0.01 MPa, and add it uniformly within 8 hours. 10 minutes after the initiator was added dropwise, stop aerating and turn off the heating device, stop stirring after 30 minutes, open the reaction kettle, filter the obtained solid-liquid mixture, and dry in an oven at 105°C for 5 hours to obtain 902.3g of white fluid powder. Molecular formula H 4 (C 4 h 9 ) 2 P 3 o 6 Al: phosphorus content 27.8%; X-ray electron spectrum: phosphorus content 27.7%.

Embodiment 3

[0038] Weigh 600g of magnesium hypophosphite and add it into a 5L reaction kettle filled with 2.5L of deionized water, stir and disperse evenly. Weigh 0.6g of 2,2'-azobis(2-amidinopropane) dihydrochloride and add water to configure an initiator solution with a mass percent solubility of 3%, and put the initiator solution on the reaction kettle. Heat to make the temperature rise to 100°C after 30 minutes, start to fill with ethylene gas, and start dropping the initiator solution when the pressure is stabilized at 0.1 MPa, and add it uniformly within 8 hours. 10 minutes after the initiator was added dropwise, stop aerating and turn off the heating device, stop stirring after 30 minutes, open the reaction kettle, filter the obtained solid-liquid mixture, and dry in an oven at 105°C for 5 hours to obtain 930.5g of white fluid powder. Molecular formula H(C 2 h 5 ) 3 P 2 o 4 Mg: phosphorus content 26.1%; X-ray electron spectrum: phosphorus content 25.5%.

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Abstract

The invention provides a partially alkylated phosphinic acid nonalkali metal salt and a preparing method and application thereof. The preparing method comprises the following steps of: ensuring that radical addition occurs between a phosphinic acid nonalkali metal salt and compound containing double bonds in the presence of an initiator, and generating partially alkylated phosphinic acid nonalkali metal salt products. The application is as follows: a flame-retardant polymer comprises a thermoplastic polymer or thermosetting polymer, and more than one of the partially alkylated phosphinic acidnonalkali metal salt. The invention has the advantages of simple technical process, easy operation, less byproducts, low energy consumption and pollution and the like.

Description

technical field [0001] The invention relates to the technical field of plastic processing and application, in particular to a partially alkylated phosphinic acid non-alkali metal salt and a preparation method thereof, as well as the application of the partially alkylated phosphinic acid non-alkali metal salt in polymer flame retardancy. Background technique [0002] There are existing patent literatures reporting synthesis methods of alkyl phosphinates and flame retardant polymer materials prepared from them. [0003] CN 1660857A invented a dialkyl phosphinate with the following structure (3). It was found that a mixture of 25% by weight of aluminum diethylphosphinate and 75% by weight of polybutylene terephthalate was compounded in a twin-screw extruder at 230-260°C to obtain a flame-retardant polymer Object molding composition, the classification of the sample according to UL94 is V-0. [0004] [0005] The Chinese patent application whose publication number is CN 197...

Claims

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Application Information

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IPC IPC(8): C07F9/30C08K5/5313C08L63/00C08L75/04C08L67/06
Inventor 姜宏伟董亮亮
Owner SOUTH CHINA UNIV OF TECH
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