A kind of preparation method of controllable molecular weight polyacrylate pentabromobenzyl ester

A technology of poly(pentabromobenzyl acrylate and molecular weight) is applied in the field of preparation of controllable molecular weight poly(pentabromobenzyl acrylate), which can solve the problems of uneven molecular weight distribution, imperfect purification process, low heat resistance and the like, and achieves the The effect of stable product quality, low cost and easy control

Active Publication Date: 2022-07-26
WEIFANG XINYANG CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, in the prior art, since there are many intermediate reaction steps in the synthesis process of pentabromobenzyl polyacrylate, the product quality is mainly affected by the purity and color of each step of the product, especially that pentabromotoluene is synthesized by high temperature reaction. , coupled with the imperfection of the existing purification process, the yield of the final product is low, the molecular weight distribution is uneven, and the heat resistance is not high

Method used

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  • A kind of preparation method of controllable molecular weight polyacrylate pentabromobenzyl ester
  • A kind of preparation method of controllable molecular weight polyacrylate pentabromobenzyl ester
  • A kind of preparation method of controllable molecular weight polyacrylate pentabromobenzyl ester

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Effect test

Embodiment 1

[0029] (1) electrophilic substitution reaction: add 640g anhydrous bromine, 0.5g catalyst aluminum trichloride, 250g dichloroethane in the reaction kettle, be cooled to 10 DEG C, slowly drop 100g benzyl chloride into the reaction kettle, drip The temperature in the reaction kettle was controlled at 10°C during the addition process, the tail gas was absorbed with water, and kept for 1 hour after the dropwise addition was completed, and an electrophilic substitution reaction occurred to obtain pentabromobenzyl chloride with a yield of 98.2% and a purity of over 99%.

[0030] (2) Nucleophilic substitution reaction: 75g acrylic acid and 550g 20% ​​sodium carbonate solution are reacted at room temperature to obtain sodium acrylate solution, and the pH value is adjusted to 7-9; pentabromobenzyl chloride is prepared in step (1). The solution was heated up, the excess bromine and residual hydrobromic acid were evaporated, then the temperature was lowered to below 50 °C, 1 g of tetrabut...

Embodiment 2

[0034] (1) electrophilic substitution reaction: add 640g anhydrous bromine, 0.5g catalyst aluminum trichloride, 250g dichloroethane in the reaction kettle, be cooled to 10 DEG C, slowly drop 100g benzyl chloride into the reaction kettle, drip The temperature in the reaction kettle was controlled at 20°C during the addition process, the tail gas was absorbed by water, and the temperature was kept for 1.5h after the dropwise addition was completed, and an electrophilic substitution reaction occurred to obtain pentabromobenzyl chloride with a yield of 98.79%.

[0035] (2) Nucleophilic substitution reaction: 75g of acrylic acid and 565g of 20% sodium carbonate solution were reacted at room temperature to obtain sodium acrylate solution, and the pH value was adjusted to 7-9; pentabromobenzyl chloride was prepared in step (1). The solution was heated up, the excess bromine and residual hydrobromic acid were evaporated, then the temperature was lowered to below 50 °C, 1 g of tetrabuty...

Embodiment 3

[0039] (1) electrophilic substitution reaction: add 700g anhydrous bromine, 5g catalyst aluminum trichloride, 550g dichloroethane in the reactor, be cooled to 10 ℃, slowly drop 100g benzyl chloride in the reactor, dropwise The temperature in the reaction kettle was controlled at 30° C., the tail gas was absorbed with water, and after the dropwise addition was completed, the temperature was kept for 2 hours, and an electrophilic substitution reaction occurred to obtain pentabromobenzyl chloride with a yield of 98.12%.

[0040](2) Nucleophilic substitution reaction: 75g acrylic acid and 580g 20% ​​sodium carbonate solution are reacted at room temperature to obtain sodium acrylate solution, and the pH value is adjusted to 7-9; pentabromobenzyl chloride is prepared in step (1). The solution was heated up, the excess bromine and residual hydrobromic acid were evaporated, and then the temperature was lowered to below 50 °C, 1 g of tetrabutylammonium bromide was added to the reaction ...

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Abstract

The invention provides a preparation method of poly(pentabromobenzyl acrylate) with controllable molecular weight, which solves the complicated reaction steps of the existing preparation method of polypropylene pentabromobenzyl ester, the rare and high price of raw materials, and the high input yield. The technical problem of low molecular weight distribution and unsuitable for industrialized production is that the present invention takes benzyl chloride and anhydrous bromine as raw materials, and successively generates electrophilic substitution reaction, nucleophilic substitution reaction and polymerization reaction to obtain polymer. Pentabromobenzyl acrylate. The invention can be widely used in the technical field of flame retardant preparation.

Description

technical field [0001] The present application belongs to the technical field of flame retardant preparation, and more specifically, relates to a preparation method of poly(pentabromobenzyl acrylate) with controllable molecular weight. Background technique [0002] Polypentabromobenzyl acrylate is a polymer type brominated flame retardant, the flame retardant has a pentabromobenzyl branched chain, its bromine content is higher than 70%, and the acrylic part has many advantages: The flame retardant material has good compatibility and good processability, and acts as a processing aid to enhance the weather resistance and thermal stability of the flame retardant material, so that the flame retardant material has fatigue resistance, bending resistance and anti-whitening effect, and can be Improve the impact strength of the material; make the material have excellent chemical resistance and electrical properties, and it is not easy to frost during use. Polypentabromobenzyl acryla...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F120/22
CPCC08F120/22
Inventor 崔文文徐金伟袁西强任伟民
Owner WEIFANG XINYANG CHEM CO LTD
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