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Industrial preparation method for polypentabrombenzamide acrylate with high purity and high stability

A technology of polypentabromobenzyl acrylate and pentabromobenzyl acrylate, which is applied in the field of industrial preparation of high-purity and high-stability polypentabromobenzyl acrylate, can solve the problem of deep color, low purity and problems of pentabromobenzyl bromide Problems such as deep color to achieve the effect of ensuring chroma and improving purity

Inactive Publication Date: 2016-06-15
SHOUGUANG TAIYUAN CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] However, in the prior art, since there are many intermediate reaction steps in the synthesis process of pentabromobenzyl polyacrylate, the main influence on its product quality is the purity and color of each step of the product, especially the synthesis of pentabromotoluene by high temperature reaction. , coupled with the imperfection of the existing purification process, resulting in a darker color of the subsequent synthesis of pentabromobenzyl bromide, making the final product darker in color and lower in purity, which also affects the overall stability of the product

Method used

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  • Industrial preparation method for polypentabrombenzamide acrylate with high purity and high stability

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Embodiment 1

[0029] A method for industrialized preparation of high-purity and high-stability polypentabromobenzyl acrylate, comprising the following steps:

[0030] (1) Synthesize light-colored pentabromotoluene by controlling the low-temperature reaction, as follows: put bromine into the reaction kettle, control the reaction temperature at -5°C, control the weight ratio of toluene to bromine to 1:19, and control the toluene at After 6 hours, the dropwise addition was completed, and then the heat preservation reaction was carried out. After the reaction was completed, excess bromine was evaporated, centrifuged, and the material was washed with water until neutral to obtain pentabromotoluene;

[0031] (2) Purify the pentabromotoluene obtained in step (1), as follows: heat pentabromotoluene and solvent to 40°C, stir for 2 hours, then crystallize at 0°C, and centrifuge the product to obtain pure white pentabromotoluene It can reach 99.5%. Among them, dichloroethane is used as solvent, and th...

Embodiment 2

[0037] A method for industrialized preparation of high-purity and high-stability polypentabromobenzyl acrylate, comprising the following steps:

[0038](1) Synthesize light-colored pentabromotoluene by controlling the low-temperature reaction, as follows: put bromine into the reaction kettle, control the reaction temperature at 10°C, control the weight ratio of toluene and bromine to 1:25, and control the toluene at 10h The dropwise addition is completed, and then the heat preservation reaction is carried out. After the reaction is completed, excess bromine is evaporated, centrifuged, and the material is washed to neutrality to obtain pentabromotoluene;

[0039] (2) Purify the pentabromotoluene obtained in step (1), as follows: heat pentabromotoluene and solvent to 50°C, stir for 2 hours, then crystallize at a low temperature at 5°C, and centrifuge the product to obtain pure white pentabromotoluene It can reach 99.5%. Among them, carbon tetrachloride is used as solvent, and th...

Embodiment 3

[0045] A method for industrialized preparation of high-purity and high-stability polypentabromobenzyl acrylate, comprising the following steps:

[0046] (1) Synthesize light-colored pentabromotoluene by controlling the low-temperature reaction, as follows: put bromine into the reaction kettle, control the reaction temperature at 5°C, control the weight ratio of toluene and bromine to 1:21, and control the toluene at 8h The dropwise addition is completed, and then the heat preservation reaction is carried out. After the reaction is completed, excess bromine is evaporated, centrifuged, and the material is washed to neutrality to obtain pentabromotoluene;

[0047] (2) Purify the pentabromotoluene obtained in step (1), as follows: heat pentabromotoluene and solvent to 45°C, stir for 2 hours, then crystallize at a low temperature at 3°C, and centrifuge the product to obtain pure white pentabromotoluene It can reach 99.5%. Among them, one or two of dichloroethane, dichloromethane, c...

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Abstract

An industrial preparation method for polypentabrombenzamide acrylate with high purity and high stability comprises the following steps: (1) pentabromotoluene with lighter color is synthesized by controlling a low-temperature reaction; (2) pentabromotoluene obtained in the step (1) is purified; (3) pentabromobenzyl bromide is synthesized from pentabromotoluene obtained in the step (2); (4) pentabromobenzyl bromide obtained in the step (3) is purified; (5) pentabromobenzyl acrylate is synthesized from pentabromobenzyl bromide obtained in the step (4); (6) pentabromobenzyl acrylate obtained in the step (5) is polymerized, and the molecular weight of a product is controlled precisely by adding a combined initiator step by step in a polymerization reaction process. The chromaticity is guaranteed, and the purity and the stability are improved.

Description

technical field [0001] The invention relates to the technical field of synthesis of pentabromobenzyl polyacrylate, in particular to a method for industrialized preparation of high-purity and high-stability pentabromobenzyl polyacrylate. Background technique [0002] At present, pentabromobenzyl polyacrylate belongs to polymerization Bromine series flame retardant , its bromine content can reach 71.7%. In addition to excellent flame retardant performance, it also has excellent thermochemical stability, good processing performance and electrical performance, good compatibility with resin, and basically does not affect the physical and chemical properties of the material. Machinability, and can improve the impact strength of flame retardant materials. When pentabromobenzyl polyacrylate is used for flame retardant PBT, it does not change the melting temperature, crystallization temperature and latent heat of the material, nor does it change the crystallinity of the material. ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F120/22C08F2/00C07C17/38C07C17/14C07C25/02C07C67/11C07C69/54
CPCC07C17/14C07C17/38C07C67/11C08F2/00C08F120/22C07C25/02C07C69/54
Inventor 任伟民李奎徐金伟马超王世海丁加中潘光辉崔文文
Owner SHOUGUANG TAIYUAN CHEM CO LTD
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