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Poly(pentabromobenzyl acrylate) synthesizing method

A technology of polypentabromobenzyl acrylate and synthesis method, which is applied in the field of synthesis of polypentabromobenzyl acrylate to achieve the effects of quality improvement, mild reaction conditions, and product quality improvement

Active Publication Date: 2017-12-08
WEIFANG RIXING CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, the synthesis of pentabromobenzyl polyacrylate is mainly synthesized by the solvent method, and there are few reports on the synthesis of the emulsion polymerization method. The advantage of the emulsion polymerization is that it is ecological and environmentally friendly, and at the same time, the product yield and purity have been improved.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] A synthetic method of pentabromobenzyl polyacrylate, comprising the following steps:

[0022] (1) Add 1.5g of emulsifier OP-10 to a solution of 300g of water and 100g of acrylic acid, stir well to make it evenly miscible, add dropwise methanol solution of sodium methoxide (75g of sodium methoxide) at 80°C, and adjust the pH to 9-10 , add 1.5g phase transfer catalyst chain polyethylene glycol and 0.3g polymerization inhibitor p-benzoquinone after completion of the reaction, fully stir and then add dropwise the dichloropropane solution of pentabromobenzyl chloride (579g of pentabromobenzyl chloride) , reacting at a temperature of 80° C. for 3 hours, cooling down to room temperature after the reaction, static layering, washing the lower organic layer with water, and filtering the insoluble matter to obtain an intermediate solution;

[0023] (2) The temperature of the above intermediate solution was raised to 90°C, 0.3g of dispersant hydroxyethyl cellulose was added, and th...

Embodiment 2

[0025] A synthetic method of pentabromobenzyl polyacrylate, comprising the following steps:

[0026] (1) Add 2g of emulsifier lauryl alcohol polyoxyethylene ether to the solution of 400g of water and 100g of acrylic acid, stir well for uniform miscibility, add dropwise methanol solution of sodium methoxide (sodium methoxide 75g) at 80°C, adjust pH=9 -10, add 2g phase-transfer catalyst chain polyethylene glycol and 0.3g polymerization inhibitor methylhydroquinone after the completion of the reaction, fully stir and then add dropwise the dichloropropane solution of pentabromobenzyl chloride (pentabromobenzyl chloride 579 g), reacted at a temperature of 80° C. for 3 hours, cooled to room temperature after the reaction was completed, and statically separated layers. After the lower organic layer was washed with water, the insoluble matter was filtered to obtain an intermediate solution;

[0027] (2) above-mentioned intermediate solution is warmed up to 90 ℃, adds 0.3g dispersant h...

Embodiment 3

[0029] A synthetic method of pentabromobenzyl polyacrylate, comprising the following steps:

[0030] (1) Add 1.5g of emulsifier OP-10 to a solution of 300g of water and 100g of acrylic acid, stir well to make it evenly miscible, add dropwise methanol solution of sodium methoxide (75g of sodium methoxide) at 80°C, and adjust the pH to 9-10 After completion of the reaction, add 1.5g phase transfer catalyst chain polyethylene glycol dialkyl ether and 0.3g polymerization inhibitor p-benzoquinone, fully stir and then add dropwise the dichloropropane solution of pentabromobenzyl chloride (pentabromobenzyl chloride Benzyl chloride 579g), reacted at a temperature of 80° C. for 3 hours, cooled to room temperature after the reaction, and statically separated layers. After the lower organic layer was washed with water, the insolubles were filtered to obtain an intermediate solution;

[0031] (2) above-mentioned intermediate solution is warmed up to 90 ℃, adds 0.3g dispersant polyvinyl al...

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PUM

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Abstract

The invention discloses a poly(pentabromobenzyl acrylate) synthesizing method and belongs to the technical field of brominated flame retardant synthesis. The synthesizing method comprises the steps of adding acrylic acid and an emulsifier into a water phase, warming to 60 DEG C to 80 DEG C, gradually dropwise adding an alkali metal alkoxide solution, adjusting a pH to be equal to 9 to 10, fully stirring and evenly mixing, adding a phase transfer catalyst and a polymerization inhibitor, maintaining a temperature as 60 DEG C to 80 DEG C, adding a pentabromobenzyl chloride solution dissolved by dichloropropane, keeping the temperature for 1 to 5 hours after dropwise adding the pentabromobenzyl chloride solution, standing and layering, taking an organic layer to be washed by water, filtering to obtain an intermediate solution, warming the solution to 90 DEG C, adding a dispersant, an initiator and a molecular weight control agent to perform polymerization reaction, adding a stabilizer and a pH modifier in a center control process, programmably warming, finally curing in high temperature and filtering and drying to obtain a poly(pentabromobenzyl acrylate) product with even molecular weight distribution.

Description

technical field [0001] The invention relates to a synthesis method of pentabromobenzyl polyacrylate, belonging to the technical field of synthesis of brominated flame retardants. Background technique [0002] Pentabromobenzyl polyacrylate is a high molecular type brominated flame retardant with pentabromobenzyl branched chain and its bromine content is higher than 70%. 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, flex resistance and anti-whitening effect and can 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. Pentabromobenzyl polyacrylate is well compatible with polymers and reinforcing materials, and does not migr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F120/22C08F2/38C08F2/40C08F2/30
Inventor 宗先庆郭安昊孙美玲孙丹阳邱亮泽
Owner WEIFANG RIXING CHEM
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