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A kind of preparation method of phenoxytetrabromobisphenol A carbonate flame retardant

The technology of phenoxytetrabromobisphenol and tetrabromobisphenol is applied in the field of preparation of additive carbonate flame retardants, and can solve the problems of using additive flame retardants, general end-capping effect, and no end-capping, etc. To achieve the effect of sufficient reaction, shortened reaction time and good transparency

Active Publication Date: 2015-07-29
SHOUGUANG WEIDONG CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] Publication No. "CN101033291" titled "Super Molecular Weight Tetrabromobisphenol A Polycarbonate Preparation Method" Chinese Invention Patent, and Publication No. "CN1900140" Title" The Chinese invention patents of “Preparation of High Molecular Weight Bisphenol Polycarbonate by Interfacial Polymerization Method” all use the reaction of bis(trichloromethyl)carbonate and tetrabromobisphenol A to prepare high molecular weight polycarbonate, and neither Capped, and the molecular weight is above 150,000, it cannot be used alone as an additive flame retardant
[0004] and the Chinese patent with publication number "CN101177481" title "Preparation Method for Synthesizing Brominated Polycarbonate with Dual Catalysts" provides a kind of Synthetic Brominated Polycarbonate with Dual Catalysts The preparation method of the ester, by using a dual-catalyst system, first polymerizes bis(trichloromethyl)carbonate and tetrabromobisphenol A, and then uses monohydric phenol to block the end to obtain brominated For polycarbonate, because this method is to polymerize to form a high-chain polymer first, and then carry out end-capping, the reaction time is long, and the reaction is not sufficient, and the end-capping effect is general

Method used

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  • A kind of preparation method of phenoxytetrabromobisphenol A carbonate flame retardant
  • A kind of preparation method of phenoxytetrabromobisphenol A carbonate flame retardant

Examples

Experimental program
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Effect test

Embodiment 1

[0027] (1) Add 27.2 grams of tetrabromobisphenol A and 2.4 grams of phenol into 50 ml of dichloromethane, pass through cooling water, control the temperature at 20°C, and stir evenly to obtain a suspension or transparent liquid;

[0028] (2) Dissolve 7.0 grams of bis(trichloromethyl)carbonate in 20 milliliters of dichloromethane and stir evenly to obtain a chlorinated hydrocarbon solution of bis(trichloromethyl)carbonate for subsequent use;

[0029] (3) The temperature is controlled at normal temperature, and 0.9 g of triethylamine (3.3% of the mass of tetrabromobisphenol A) is added to the solution in step (2) under stirring;

[0030] (4) Add the solution obtained in step (1) to the solution obtained in step (2) at a constant speed. At the same time, add 5% sodium hydroxide solution dropwise to react until the reaction material is alkaline. After the addition is completed, keep warm for 2 hours ;

[0031] (5) After the heat preservation is over, stop stirring, let stand for ...

Embodiment 2

[0035] Under the same conditions as in Example 1, 1.0 g of pyridine (3.7% of tetrabromobisphenol A mass) was used instead of 0.9 g of triethylamine to obtain 30.5 g of phenoxytetrabromobisphenol A carbonate, and the technical detection indicators were as follows :

[0036] The number average molecular weight of the product is 2578, and the melting point is 190.8~197.2℃.

Embodiment 3

[0038] Under the same conditions as in Example 1, 0.9 gram of triethylamine was replaced with 1.3 gram of triethylbenzyl ammonium chloride (4.8% of tetrabromobisphenol A quality), and the obtained phenoxytetrabromobisphenol A carbonate 29.6 grams, the technical testing indicators are as follows:

[0039] The number average molecular weight of the product is 2498, and the melting point is 190.2~196.8℃.

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Abstract

The invention relates to the technical field of addition type carbonate flame retardants and provides a method for preparing a phenoxy tetrabromobisphenol A carbonate flame retardant. The method comprises the following steps: (1) dissolving phenol and tetrabromobisphenol A in a chloralkane solution, and uniformly stirring; (2) dissolving bi(trichloromethyl) carbonate in the chloralkane solution in a reaction container at room temperature; (3) adding a catalyst into the reaction container; (4) dropwise adding alkaline liquor and a mixture dissolving solution prepared in the step (1) into the reaction container at a constant speed, and reacting for 1-2 hours at room temperature; (5) washing the solution prepared in the step (4) until the solution does not contain chloridion, and splitting the organic layer; and (6) dropwise adding the organic layer into hot water at the temperature of 70-95 DEG C, and separating out the coarse product by crystallization. According to the method, the target product, namely phenoxy tetrabromobisphenol A carbonate is directly obtained, the molecular weight controllability of the product is improved, the operation process is simple, and the operability is high.

Description

technical field [0001] The invention relates to the technical field of preparation of additive-type carbonate flame retardants, in particular to a preparation method of phenoxytetrabromobisphenol A carbonate flame retardants. Background technique [0002] With the rapid rise of polymer material science, polymer materials are widely used in human production and life, and more and more fires are caused by them being ignited. Therefore, the flame retardancy of polymer materials has been widely recognized by people. focus on. Japan and Germany have conducted very in-depth research, and my country has also conducted extensive research in this field, and has also achieved some considerable results. In particular, flame retardants with low toxicity and less impact on the performance of polymer materials have gradually been recognized and used by people. [0003] Publication No. "CN101033291" titled "Preparation Method of Ultra-Molecular Weight Tetrabromobisphenol A Polycarbonate"...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C69/96C07C68/06C08K5/109
CPCC07C68/06C07C69/96
Inventor 刘瑞祥陈如林谢忠财曹永强朱之军
Owner SHOUGUANG WEIDONG CHEM
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