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Preparation method of trimethylolpropane tri-(2-carboxyethyl phenyl phosphinate)

A technology of trimethylolpropane and trimethylolpropane, which is applied in the field of preparation of environmentally friendly flame retardant plasticizers, can solve the problems of limited use, low freezing point, and influence on material properties, and achieve easy control of the process and simple production process , the effect of good affinity

Active Publication Date: 2015-04-29
SHANDONG UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Tricresyl phosphate and chlorinated paraffin are commonly used flame retardant plasticizers, but there are still many problems in the process of processing and are limited in use
Although trihydrocarbyl phosphate esters have good flame retardant and smoke suppression effects and low volatility, due to their low freezing point, some small molecule phosphate esters will thermally decompose, volatilize or ooze out during mold processing at higher temperatures, which will affect material properties. , and pose a threat to the health of practitioners

Method used

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  • Preparation method of trimethylolpropane tri-(2-carboxyethyl phenyl phosphinate)

Examples

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Effect test

Embodiment 1

[0017] Add 140g of trimethylolpropane, 322g of 2-carboxyethylphenyl hypophosphorous acid and 5g of p-toluenesulfonic acid into a reactor equipped with mechanical stirring and a water separator, heat to 220°C, and react for 18 hours. 52g of water, after the reaction, the product in the reactor was poured into water for cooling to obtain 394g of colorless transparent massive solid, with a yield of 92.2%.

Embodiment 2

[0019] Add 140g trimethylolpropane, 322g 2-carboxyethylphenylphosphorous acid and 2.7g SnCl in the reactor equipped with mechanical stirring and water separator 2 2H 2 O, heated to 160° C., reacted for 20 h, and divided 48 g of water during the reaction. After the reaction, the product in the reactor was poured into water to cool to obtain 391 g of a colorless transparent block solid, with a yield of 91.5%.

Embodiment 3

[0021] Add 140g trimethylolpropane, 322g 2-carboxyethylphenylphosphorous acid and 3.2g MgCl in a reactor equipped with mechanical stirring and water separator 2 , heated to 220°C, and reacted for 18 hours. During the reaction, 53g of water was separated. After the reaction, the product in the reactor was poured into water to cool, and 400g of colorless or light yellow transparent block solid was obtained, with a yield of 93.5%.

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Abstract

The invention discloses a preparation method of trimethylolpropane tri-(2-carboxyethyl phenyl phosphinate). The preparation method comprises the following steps of: performing heating reaction on trimethylolpropane and 2-carboxyethyl phenyl hypophosphorous acid serving as raw materials in the presence of a catalyst, pouring the reaction product into water for cooling after the reaction is completed, and thus obtaining the product; the molar ratio of the trimethylolpropane to the 2-carboxyethyl phenyl hypophosphorous acid is 1: (2.5-3.5); the catalyst is one or more of FeCl3, SnCl2, SnCl4, Al2(SO4)3, MgCl2, CaCl2, Sb2O3, Sb(CH2COO)3, p-toluenesulfonic acid and concentrated sulfuric acid; the consumption of the catalyst is 0.5 to 4 percent of mass of the trimethylolpropane; and the reaction temperature is 80 to 260 DEG C, and the reaction time is 10 to 28 hours. The plasticizer is prepared by adopting a 'one-pot method', the production process is simple, the process is easily controlled, and the method is favorable for large-scale production; and an organic solvent is not used in the whole production process, so the method has obvious environmental friendliness.

Description

technical field [0001] The invention relates to a preparation method of an environment-friendly flame-retardant plasticizer, in particular to a preparation method of trimethylolpropane tris(2-carboxyethylphenylphosphinate). Background technique [0002] Plasticizers are currently the most widely used additives for plastics and rubber, and are widely used in industries such as rubber, plastics, packaging materials, medical materials, automobiles, and electronics. In 2007, the global output of plasticizers reached 8.9 million tons / year. The research report shows that in 2007 my country's plasticizer production capacity has reached 2.6 million tons per year, and in 2010 the production capacity will reach 3.5 million tons per year, and the average annual growth rate of market consumption will grow rapidly at a rate of 9%. The main reason is that high-value specialty plasticizer products continue to occupy a larger market share. At the same time, countries and regions such as th...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F9/30C08L27/06C08K5/5313
Inventor 王忠卫刘尚义张召举刘炳艳
Owner SHANDONG UNIV OF SCI & TECH