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Process for preparing brominated polystyrene

A technology for brominated polystyrene and polystyrene, which is applied in the field of preparing brominated polystyrene, can solve the problems of reduced use effect, inconvenient storage and use, etc., and achieves safe and efficient use, easy operation and control, and low price. Effect

Inactive Publication Date: 2009-08-05
HUAIHAI INST OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The chemical properties of phosphorus pentoxide are extremely active, and it is inconvenient to store and use. It is often pasted on the wall of the reactor, and the use effect is reduced.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] In the 1000 milliliter reaction flask of light-proof, add 400 milliliters of dichloroethanes, polystyrene 50 grams and sulfur 1.8 grams of mass-average molecular weight Mw=25000, stir and drop into bromine 10 grams, keep the material in the reaction flask at 30 around ℃ until the polystyrene melts. Lower the temperature of the material in the reaction flask to 0-2°C, add 2 grams of anhydrous aluminum trichloride powder, and drop in 230 grams of bromine dried by concentrated sulfuric acid within 2 hours. After bromine dripping was completed, the stirring reaction was continued for 2 hours at natural temperature. The reaction product system was washed with 3×300 ml of water, then neutralized with 20% caustic soda aqueous solution with a mass concentration of 20% to neutralize the pH value of the reaction product system to 7.0-7.5, and the water phase was separated. The organic phase was dropped into 1000 ml of methanol, the brominated polystyrene crystallized out was cen...

Embodiment 2

[0025] In a 1000 ml reaction flask protected from light, add 400 ml of dichloroethane and 52 grams of polystyrene with a mass average molecular weight Mw=25000, and keep the material in the reaction flask at around 30° C. until the polystyrene melts. Reduce the material temperature in the reaction flask to 0-2°C, add 1.6 grams of sulfur, 2.3 grams of anhydrous aluminum trichloride powder and 0.3 grams of zinc powder, and drop 235 grams of bromine dried in concentrated sulfuric acid within 2 hours. After bromine dripping was completed, the stirring reaction was continued for 2 hours at natural temperature. The reaction product system was washed with 3×300 ml of water, then neutralized with 20% caustic soda aqueous solution with a mass concentration of 20% to neutralize the pH value of the reaction product system to 7.0-7.5, and the water phase was separated. The organic phase was dropped into 1000 ml of methanol, the crystallized brominated polystyrene was centrifuged to remove...

Embodiment 3

[0027]In a 1000 ml reaction flask protected from light, add 400 ml of dichloroethane and 50 grams of polystyrene with a mass average molecular weight Mw=25000, and keep the material in the reaction flask at around 30° C. until the polystyrene melts. Lower the temperature of the materials in the reaction flask to 0-2°C, add 3.0 grams of sulfur, 3.0 grams of anhydrous aluminum trichloride powder and 0.5 grams of zinc powder, and drop in 250 grams of bromine dried by concentrated sulfuric acid within 2 hours. After bromine dripping was completed, the stirring reaction was continued for 2 hours at natural temperature. The reaction product system was washed with 3×300 ml of water, then neutralized with 20% caustic soda aqueous solution with a mass concentration of 20% to neutralize the pH value of the reaction product system to 7.0-7.5, and the water phase was separated. The organic phase was dropped into 1000 ml of methanol, the crystallized brominated polystyrene was centrifuged ...

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PUM

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Abstract

The invention provides a preparation method of bromized polystyrene. The method is characterized in that sulfur is taken as the scavenging agent of a small amount of water in the electrophilic bromination reaction of the polystyrene and as the quencher of free radical in the electrophilic bromination reaction of the polystyrene, and the mass of the sulfur is 0.1 to 12 percent of that of the polystyrene. In the organic solvent of dichloroethane, chloroform, bromochloromethane, carbon tetrachloride or tetrachloroethane, the anhydrous aluminium trichloride, the anhydrous ferric chloride, the titanium tetrachloride, the antimonous chloride, the aluminum powder, the zinc powder or the iron powder is taken as the catalyst, the sulfur is taken as the scavenging agent of the small amount of water and as the quencher of the free radical, and the bromized polystyrene is prepared by the electrophilic bromination reaction between the polystyrene and the bromine.

Description

technical field [0001] The invention relates to a preparation method of brominated polymer. It particularly relates to a method for preparing brominated polystyrene by using sulfur as a scavenger for trace moisture in a polystyrene electrophilic bromination reaction system and a free radical quencher in the polystyrene electrophilic bromination reaction. technical background [0002] Brominated polystyrene is polystyrene dispersed and dissolved in organic solvents such as dichloroethane, dichloromethane, bromochloromethane, chloroform, carbon tetrachloride or tetrachloroethane, using anhydrous aluminum trichloride, Anhydrous ferric trichloride, titanium tetrachloride, antimony trichloride, aluminum powder, zinc powder or iron powder, etc. are used as catalysts, and bromine is a brominated polymer prepared by the bromination reaction of benzene nuclei. As an organic polymer bromide flame retardant, brominated polystyrene has high flame retardancy, good thermal stability, goo...

Claims

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Application Information

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IPC IPC(8): C08F8/22C08F112/08
Inventor 张田林周杰兴姜培琴
Owner HUAIHAI INST OF TECH
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