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Preparation method of brominated polystyrene

A technology of brominated polystyrene and polystyrene, which is applied in the field of polymer brominated flame retardant preparation, can solve problems such as poor dispersion, and achieve the effect of improving whiteness, fine and uniform particles, and good color of the product

Active Publication Date: 2010-05-05
TIANJIN SEA WATER DESALINATION & COMPLEX UTILIZATION INST STATE OCEANOGRAPHI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Aiming at the defects of poor dispersion of the reaction completion liquid in the separating agent and entrained solvent in the existing brominated polystyrene preparation method in the prior art, the present invention provides a new preparation method of brominated polystyrene, that is, the application produces The high-shear high-speed stirring equipment can quickly disperse the bromination reaction liquid, increase the contact area between the solvent and the separating agent, remove the solvent entrained in the brominated polystyrene product by a combination of physical and chemical methods, and improve the bromination rate. Product quality of polystyrene

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Take 10.4g of polystyrene and dissolve in 125mL of dichloroethane solvent. After the dissolution is complete, add 0.9g of antimony trichloride and stir to dissolve it. Cool the polystyrene solution to 12°C, add 41.4g of bromine chloride dropwise, keep the temperature at 12°C to 15°C during the dropwise addition, and complete the dropwise addition in 2.5 hours. Keep the temperature of the reaction solution at 15°C and continue stirring for 3 hours. Add 54mL of 5wt% sodium bisulfite to stop the reaction, remove excess bromine chloride, add 15mL of 5wt% sodium hydroxide solution for neutralization, and wash with water twice. After the water and oil are separated, add the lower oil phase to an emulsification homogenizer (a kind of homogeneous emulsification equipment) filled with 350mL ethanol at a rate of 20mL / min, turn on high-speed stirring, adjust the speed at 2000 rpm, wait until Add the oil phase into the homogenizer completely, and continue stirring at the rotating ...

Embodiment 2

[0018] Dissolve 10.4g polystyrene in 128mL dichloroethane solvent, add 1.0g antimony trichloride after dissolving, after the catalyst is dissolved, cool the polystyrene solution to 16°C, add 43.3g bromine chloride dropwise, add dropwise During the process, the reaction temperature was kept at 14°C to 16°C, and the dropwise addition was completed within 2 hours. Keep the temperature of the reaction solution at 14° C. to 16° C. and continue stirring for 3 hours. Add 110mL of 5wt% sodium sulfite to remove excess bromine chloride, add 38mL of 5wt% sodium hydroxide solution for neutralization, and wash with water twice. After the water and oil are separated, add the oil phase to an emulsification homogenizer (a kind of homogeneous emulsification equipment) filled with 350mL ethanol at a speed of 5mL / min, and adjust the high-speed stirring to 3000 rpm. After all the addition, keep the stirring speed and continue stirring for 2 minutes. The precipitated brominated polystyrene was w...

Embodiment 3

[0020] Take 21.0g of polystyrene and dissolve in 158mL of dichloroethane solvent, after the dissolution is complete, add 1.8g of antimony trichloride. After the catalyst was dissolved, the polystyrene solution was cooled to 15°C, and 86.3g of bromine chloride was added dropwise. The temperature during the dropwise addition was between 12°C and 15°C, and the dropwise addition was completed in 3 hours. Keep the temperature of the reaction solution at 12° C. to 15° C. and continue stirring for 4 hours. Add 142 mL of 5 wt % sodium bisulfite to terminate the reaction, remove excess bromine chloride, add 65 mL of 5 wt % sodium hydroxide solution for neutralization, and wash with water twice. Add the lower organic phase into the emulsification homogenizer at a rate of 15 mL / min, adjust the high-speed stirring speed to 2500 rpm, and add 320 mL of ethanol into the homogenizer. The bromine content of the precipitated brominated polystyrene is 68.0%, the product particles are fine and u...

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Abstract

The invention relates to a preparation method of brominated polystyrene, comprising three steps of catalyzing and brominating, neutralizing washing, and solidifying and separating. The step of catalyzing and brominating comprises the following steps: dissolving polystyrene into dichloroethane solvent, adding antimony trichloride catalyst into the solution, dropwise adding bromine chloride into the solution which is added with antimony trichloride catalyst, wherein the mole ratio of bromine chloride to polystyrene monomer is 3.8:1-3.5:1, keeping the temperature at 10-25 DEG C and reacting for 3-4 hours; the step of neutralizing washing comprises the following steps: adding 5wt% of sodium sulfite or sodium bisulfite aqueous solution into the polystyrene reaction liquid after catalyzing and brominating to terminate the reaction, then adding 5wt% of sodium hydroxide solution to be in neutrality, and then washing with water; and the step of solidifying and separating comprises the following steps: adding the brominated polystyrene solution after neutralizing washing into a high-speed stirring device with high shearing force at a speed of 5mL / min-20mL / min, wherein the high-speed stirring device is filled with alcohol separating agent; regulating the rotating speed to be in a range of 2000-3000 r.p.m.; scattering the brominated polystyrene product in the alcohol to cure into small particles; separating solid products, washing with alcohol, then filtering and drying to obtain brominated polystyrene products.

Description

technical field [0001] The invention belongs to the preparation technology of macromolecule brominated flame retardants, in particular to methods for preparing brominated polystyrene flame retardants and solidifying and separating them. Background technique [0002] As a flame retardant, brominated polystyrene has the advantages of high flame retardancy and good fluidity, and is widely used in engineering plastics such as PBT and PET. [0003] In the prior art, brominated polystyrene is prepared by reacting polystyrene with a brominating agent, and the preparation method includes bromination, washing and separation processes. The separation process adopts water distillation separation or organic solvent separation, and the brominated polystyrene is solidified and separated from the bromination reaction completion liquid. When the water is distilled and separated, near-boiling water is used as the separating agent, and the solvent is evaporated by high temperature, so that t...

Claims

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Application Information

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IPC IPC(8): C08F12/08C08F8/20C08L25/04
Inventor 蔡荣华姚颖张慧峰高书宝张淑芬黄西平张雨山王国强
Owner TIANJIN SEA WATER DESALINATION & COMPLEX UTILIZATION INST STATE OCEANOGRAPHI
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