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Method for preparing low molecular weight narrow distribution brominated polystyrene by active/controllable polymerization

A brominated polystyrene, low molecular weight technology, used in fire-resistant coatings, etc., can solve the problems of high molecular weight, unstable product quality, and poor compatibility with matrix resins

Inactive Publication Date: 2008-08-13
TONGJI UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The current domestic brominated polystyrene products are made by direct bromination of polystyrene with high molecular weight (molecular weight above 200,000), so the molecular weight of the obtained product is also very high, and the processing temperature is too high, which is different from the flame-retardant matrix resin. The compatibility is not good, which greatly affects the mechanical properties of the resin, and the product quality is also unstable

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  • Method for preparing low molecular weight narrow distribution brominated polystyrene by active/controllable polymerization
  • Method for preparing low molecular weight narrow distribution brominated polystyrene by active/controllable polymerization
  • Method for preparing low molecular weight narrow distribution brominated polystyrene by active/controllable polymerization

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Embodiment 1

[0038] Styrene is used as a monomer, organic halides containing halogen atoms are used as initiators, low-valent metal halides are used as catalysts and ligands, and low-molecular-weight polystyrene is obtained by performing atom transfer free radical polymerization. Low-molecular-weight polystyrene uses alkyl halide as a solvent and alkylaluminum halide as a catalyst. In the presence of a dehydrating agent, low-molecular-weight polystyrene is brominated with bromine to obtain low-molecular-weight brominated polystyrene.

[0039] Step (a): Add refined 50g styrene, 0.05g α-methyl bromoacrylate, 0.05g cuprous chloride and 0.1g bipyridine in a 250mL three-necked flask equipped with a magnetic stirrer, and react The system was evacuated and filled with nitrogen, heated to 80°C, stirred by magnetic force and reacted under reflux for 20h. After the obtained product was dissolved in tetrahydrofuran, it was added dropwise to a precipitant with a ratio of 1:10 of methanol and distilled...

Embodiment 2

[0043] Styrene is used as a monomer, organic halides and azos containing halogen atoms are used as initiators, high-valent metal halides are used as catalysts and ligands, and low molecular weight polystyrene is obtained by reverse atom transfer radical polymerization. Low-molecular-weight polystyrene uses alkyl halide as a solvent and alkylaluminum halide as a catalyst. In the presence of a dehydrating agent, low-molecular-weight polystyrene is brominated with bromine to obtain low-molecular-weight brominated polystyrene.

[0044] Step (a): Add refined 40g styrene, 0.05g benzyl chloride, 0.02g azobisisobutyronitrile, 0.08g ferric chloride and 0.05g triphenyl to a 250mL three-necked flask equipped with a magnetic stirrer Based phosphine, the reaction system was evacuated and filled with nitrogen, heated to 120 ° C, magnetically stirred and refluxed for 30 h. After the obtained product was dissolved in tetrahydrofuran, it was added dropwise to a precipitant with a ratio of meth...

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Abstract

A method of preparation of brominated polystyrene combustion inhibitor with low molecular weight by active / controllable polymerization. Brominated polystyrene with controllabel low molecular weight is prepared by atom transfer radical polymerization (ATRP) or reverse atom transfer radical polymerization (FATRP), comprising using organic halogen as initiator, adding azo-initiator, catalyst of low valent metal halogen and ligand into FATRP, then obtaining narrow distributed brominated polystyrene with low molecular weight by bulk polymerization, suspension polymerization, emulsion polymerization. The polystyrene is mixed with alkyl halide, alkyl aluminium halide, dehydrant, brominated by bromine to get narrow distributed brominated polystyrene with low molecular weight. Polystyrene or brominated polystyrene of different molecular weight can be respectively obtained by controlling weight of added monomer or bromine. The obtained brominated polystyrene combustion inhibitor with low molecular weight has high content of bromine, good compatibility with matrix, great heat durability and ageing resistance, little influence on impact resistance of basic resin.

Description

technical field [0001] The invention belongs to the field of chemical industry and relates to a flame retardant, in particular to a method for preparing low molecular weight brominated polystyrene by active / controllable polymerization. Background technique [0002] Atom transfer radical polymerization (ATRP) is a kind of living / controllable polymerization, and it is a new type of polymer synthesis method. Different from traditional free radical polymerization, ATRP is the most ideal method to control the molecular weight of polymers. Accurate control of molecular weight and molecular weight can be achieved to obtain a narrow distribution of polymer molecular weight. [0003] Low molecular weight brominated polystyrene is mainly used for flame retardancy of engineering plastics polyamide (PA), polyester (PBT, PET) and polystyrene (PS). It can be used alone or with antimony trioxide (Sb 2 o 3 ) are used together for synergistic flame retardancy. [0004] The molecular wei...

Claims

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Application Information

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IPC IPC(8): C08F8/22C08F112/08C08F4/04C08F2/06C09K21/14
Inventor 刘琳刘洋王国建李胜利
Owner TONGJI UNIV
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