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Method for producing poly(pentabromobenzyl acrylate)

A technology of polypentabromobenzyl acrylate and pentabromobenzyl acrylate, which is applied in the field of flame retardants, can solve problems such as poor thermal stability, color change, and poor UV stability, and achieve UV resistance Good light stability, little impact on material properties, and superior product performance

Active Publication Date: 2011-08-31
SHANDONG RUNKE CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, our domestic annual output of brominated flame retardants is about 11,000 tons, which needs to be imported in large quantities from abroad every year, and the flame retardants currently used are easy to bloom and migrate, and the color will change after a period of use. The stability to ultraviolet light is not very good, and the thermal stability is not good
[0012] General flame retardants, after being added to the material, the impact resistance will decrease, causing the material to be broken by external force, and will have a certain impact on the crystallization temperature, melting temperature and latent heat of the material, and will also change the crystallinity of the material. Changes in these factors will lead to changes in the physical properties of the material.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Make pentabromobenzyl bromide in the reactor of 5000L, add 437kg pentabromotoluene, 4285kg carbon tetrachloride, the hydrogen peroxide of 35kg benzoyl peroxide and 80kg30% concentration, will contain 0.32kg / L quality of 110kg bromine concentration of carbon tetrachloride bromine solution, at a temperature of 60 ° C, the bromine solution was added dropwise to the reaction solution, and then kept for 3 hours, the reaction product was filtered to obtain a solid product, and the product was washed with carbon tetrachloride until the washing liquid was It is a colorless transparent liquid, and after drying under vacuum at 35°C, pentabromobenzyl bromide is obtained.

[0028]To prepare pentabromobenzyl acrylate, add 550kg of ethylene glycol methyl ether, 41.5kg of acrylic acid, 0.75kg of hydroquinone, and 26.8kg of anhydrous sodium carbonate into a 3000L reactor. React at 35°C until the liquid no longer produces bubbles, then rapidly heat up to 100°C, add 289.6 kg of pentabrom...

Embodiment 2

[0031] Prepare pentabromobenzyl bromide in a 5000L reaction kettle, add 487kg pentabromotoluene, 3000L carbon tetrachloride, 40kg benzoyl peroxide and 130kg30% concentration of hydrogen peroxide, and dissolve 160kg bromine in 500L tetrachloride Make a solution with carbon, add the bromine solution dropwise to the reaction solution at a temperature of 65°C, then keep it warm for 4 hours, filter the reaction product to obtain a solid product, wash the product with carbon tetrachloride until the washing liquid is a colorless transparent liquid , and dried under vacuum at 40°C to obtain pentabromobenzyl bromide.

[0032] To prepare pentabromobenzyl acrylate, add 600kg of ethylene glycol methyl ether, 46.5kg of acrylic acid, 0.8kg of hydroquinone, and 31.8kg of anhydrous sodium carbonate into a 3000L reactor. React at 40°C until the liquid no longer produces bubbles, then rapidly heat up to 110°C, add 339.6 kg of pentabromobenzyl bromide, react at 110°C for 5 hours, and directly fi...

Embodiment 3

[0035] Make pentabromobenzyl bromide in the reactor of 5000L, add 537kg pentabromotoluene, 5285kg carbon tetrachloride, the hydrogen peroxide of 45kg benzoyl peroxide and 180kg30% concentration, will contain the 0.32kg / L quality of 210kg bromine concentration of carbon tetrachloride bromine solution, at a temperature of 70 ° C, the bromine solution was added dropwise to the reaction solution, and then incubated for 5 hours, the reaction product was filtered to obtain a solid product, and the product was washed with carbon tetrachloride until the washing liquid was It is a colorless transparent liquid, and after drying under vacuum at 45°C, pentabromobenzyl bromide is obtained.

[0036] To prepare pentabromobenzyl acrylate, add 650kg of ethylene glycol methyl ether, 51.5kg of acrylic acid, 0.85kg of hydroquinone, and 36.8kg of anhydrous sodium carbonate into a 3000L reactor. React at 45°C until the liquid no longer produces bubbles, then rapidly heat up to 120°C, add 389.6 kg o...

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PUM

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Abstract

The invention discloses a method for producing poly(pentabromobenzyl acrylate). The method comprises the following steps of: adding ethylene glycol monomethyl ether, acrylic acid, hydroquinone and anhydrous sodium carbonate into a reaction kettle; reacting at the temperature of between 35 DEG C and 45 DEG C until no bubbles are produced; heating to reach the temperature of between 100 DEG C and 120 DEG C; adding pentabromobenzyl bromide to react to obtain pentabromobenzyl acrylate; adding the ethylene glycol monomethyl ether and the prepared pentabromobenzyl acrylate into the reaction kettle; introducing nitrogen gas and stirring; heating to reach the temperature of between 90 DEG C and 110 DEG C; adding a mixed solution of dicumyl peroxide and glycol ether; polymerizing for 1.5 to 2.5 hours and then heating to reach the temperature of between 110 DEG C and 126 DEG C; and continuously reacting for 2 to 5 hours to prepare the poly(pentabromobenzyl acrylate). A product prepared by the method has the advantages of superior performance, no separation, no migration, extremely low influence on properties of materials, capability of increasing productivity, high mechanical property, high anti-ultraviolet stability and high thermal stability.

Description

technical field [0001] The invention relates to the technical field of flame retardants, in particular to a method for producing polypentabromobenzyl acrylate. Background technique [0002] At present, the total output of the world's six major general-purpose polymers has reached 180 million tons per year, of which 8-9%, or 14 million to 15 million tons per year, are flame-retardant, and its proportion will continue to increase, especially About 18% of the plastics used in the electronics and electrical industries are flame retardant, and it is expected to reach 23-25% in the next five years. [0003] In addition, the flame-retardant ratio of engineering plastics is higher than that of general-purpose plastics. From 2007 to 2008, the total output of engineering plastics in the world was 6 million tons per year, of which 35% were flame-retardant products, and they were used in engineering in the electronic-electrical industry. Plastics have a higher percentage of flame retar...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F120/22C08L67/02C08L77/00C08L33/16
Inventor 宗先庆崔明亮吴多坤
Owner SHANDONG RUNKE CHEM
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