A kind of method of synthesizing brominated polystyrene

A technology of brominated polystyrene and polystyrene, which is applied in the field of synthesizing brominated polystyrene, can solve the problems of polystyrene molecular weight reduction, long production cycle, and rising product cost, so as to improve thermal stability, molecular weight, etc. The effect of narrow distribution and low chroma value

Active Publication Date: 2022-04-19
TAIZHOU BAILLY CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] However, the disadvantages of the above synthesis route are: (1) the synthesis route is too long, the synthesis process is complicated, and the requirements for production equipment are high, resulting in an increase in product cost and a long production cycle, which reduces its market competitiveness; (2) tribromine The reactivity of styrene monomer is very high, which makes the polymerization reaction difficult to control. Therefore, dibromostyrene is generally used for polymerization, resulting in a low bromine content of the product after polymerization, which is about 60%. To achieve the same flame retardant effect, it needs Adding more amounts will have a greater impact on the original properties of the flame retardant material, and also increase the flame retardant cost
[0004] In addition, in the existing synthetic method of brominated polystyrene, the reaction of polystyrene and bromine is adopted. In addition to the bromine substitution reaction on the benzene ring, the substitution reaction may also occur with the active hydrogen on the tertiary carbon atom on the main chain. Due to the low bond energy, this by-product is prone to chain scission in a slightly higher temperature environment, resulting in a smaller molecular weight and wider distribution of brominated polystyrene

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Add 200g of dichloroethane and 10g of polystyrene in a 500mL four-neck flask with a water content of less than 100ppm, connect the tail gas system, and use dry nitrogen to replace the air in the system 3 times; cool down to -5~0°C and add 0.2g of trichloride Aluminum, add 0.03g BHT at the same time; add 43g bromine dropwise, and nitrogen gas continues to flow in while dropping, and the dropping time is 2 hours. deal with.

[0026] Post-processing method: Slowly pour the above solution into 200g of 0.1% sodium sulfite solution, use potassium iodide test paper to detect whether the water layer has changed color; leave the oil-water mixture to separate layers, and add the oil layer to 200g of 1% sodium hydroxide solution Stir and wash for 30 minutes, then stand to separate the layers again, add 200g water to the oil layer and wash for 30 minutes, let stand to separate the layers; add the oil layer dropwise into boiling water at 100°C, remove dichloroethane by flash evapora...

Embodiment 2

[0028] Add 200g of dichloroethane and 10g of polystyrene in a 500mL four-neck flask with a water content of less than 100ppm, connect the tail gas system, and use dry nitrogen to replace the air in the system 3 times; cool down to -5~0°C and add 0.2g of trichloride Aluminum, add 0.03g TEMPO at the same time; then add 43g bromine dropwise, and nitrogen gas continues to flow in while dropping, the dropping time is 2 hours, after the dropping is completed, the temperature is raised to 0~10°C and kept for 2 hours; Processing, aftertreatment mode is the same as embodiment 1. 31.2 g of brominated polystyrene finished product was obtained. The yellow index of the product is 13, the bromine content is 68.7%, and the temperature of 1% TGA is 358°C.

Embodiment 3

[0030] Add 200g of dichloroethane with a water content of 100~200ppm and 10g of polystyrene into a 500mL four-neck flask, connect the tail gas system, and use dry nitrogen to replace the air in the system 3 times; cool down to -5~0°C and add 0.2g of trichloro Aluminum chloride, add 0.03g BHT at the same time; add 43g of bromine dropwise, and continue to feed nitrogen gas during the dropwise addition. The dropwise addition time is 2 hours. Post-processing, post-processing mode is the same as embodiment 1. 32.2 g of brominated polystyrene finished product was obtained. The yellow index is 13, the bromine content is 68.6%, and the temperature of 1% TGA is 351°C.

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Abstract

The invention relates to a method for synthesizing brominated polystyrene. Under the condition of nitrogen protection, polystyrene dichloroethane solution is uniformly mixed with a certain amount of catalyst and free radical inhibitor, and then bromine is added dropwise to control its Dropping time, temperature after dropping, and then heat preservation reaction. After heat preservation reaction, post-treatment is carried out to obtain a crude product. The crude product is dried to constant weight to obtain the product brominated polystyrene. The method for synthesizing brominated polystyrene has the advantages of simple process and easy control, and the synthesized brominated polystyrene has high stability, high bromine content, low chroma and narrow molecular weight distribution.

Description

technical field [0001] The invention belongs to the technical field of preparation of macromolecule brominated flame retardants, and in particular relates to a method for synthesizing brominated polystyrene. Background technique [0002] The research and application of brominated polystyrene in foreign countries is relatively early, and the synthesis process is relatively mature. In the 1980s, Ferro Company and Great Lake Company of the United States took the lead in realizing the industrial production of brominated polystyrene. Great Lake company uses styrene as raw material, brominated it to obtain brominated styrene monomer, and then polymerized the monomer to obtain polybrominated styrene (PBS). US patent 5369202 provides its polybrominated styrene Synthetic method of ethylene commodity PDBS-80. The synthesis route of Great Lake Company is to brominate first and then polymerize, which avoids the halogenation reaction of the brominated agent on the main chain, so the the...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F12/08C08F8/22
CPCC08F8/22C08F12/08
Inventor 汪静莉潘兵波谢滋东袁东华耿飞陈健夏震宇
Owner TAIZHOU BAILLY CHEM CO LTD
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