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Process for brominating butadiene polymers

A technology of brominated butadiene and polymer, which is applied in the field of random or graft copolymers and blocks, can solve the problems of cost and other problems, and achieve the effect of simple recycling and simplified product recycling

Inactive Publication Date: 2013-02-20
DOW GLOBAL TECH LLC
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This means further expense in handling the aqueous phase and removing water from the brominated polymer

Method used

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  • Process for brominating butadiene polymers

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Embodiment

[0038] A styrene-butadiene-styrene triblock rubber with a molecular weight of 86,000 having 46 wt% of styrene units and 54 wt% of butadiene units (of which 83% is in the form of 1,2-isomer units) was Bromide. The starting material contained 9.5 mmol of double bonds per gram. A solution of 13.0 g of the triblock rubber in 130 g of dichloromethane (DCM) was heated to reflux while adding bromine (20.7 g, 0.130 mol) and tetraethylammonium bromide (32.7 g, 0.156 mol) during 10 minutes. ) in 63 g of DCM. The resulting mixture was heated to reflux with mechanical stirring (250 rpm) for 2 hours, at which point stirring was stopped and the reaction mixture was allowed to separate into layers. The upper layer is orange and constitutes 75% by mass of the reaction mixture. The lower layer is pale yellow. The lower layer is viscous and contains brominated rubber. Partially brominated rubber was separated from part of the lower layer by casting a film and allowing the solvent to evapor...

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Abstract

Butadiene polymers are brominated using tetraethylammonium tribromide as the brominating agent. The bromination is performed in a solvent for the starting polymer and for the tetraethylammonium bromide that is formed as a reaction byproduct. The process proceeds easily under mild conditions. In some cases, a solution of the brominated polymer and the tetraethylammonium monobromide is produced; this solution separates into a layer that contains the brominated polymer and another layer that contains most or all of the tetraethylammonium monobromide salt. In other cases, the brominated polymer precipitates from the reaction mixture and is separated from the tetraethylammonium monobromide salt in that manner. This process therefore permits the tetraethylammonium monobromide reaction by-product to be separated easily from the brominated product, and allows aqueous washing steps to be reduced or eliminated.

Description

technical field [0001] This application claims priority to US Provisional Patent Application No. 61 / 354,335, filed June 14, 2010. [0002] The present invention relates to a process for brominated butadiene homopolymers or copolymers, such as block, random or graft copolymers of brominated styrene and butadiene. Background technique [0003] WO 2008 / 021417 describes a process for the bromination of butadiene polymers. The brominating agent is phenyltrialkylammonium tribromide, benzyltrialkylammonium tribromide, or tetraalkylammonium tribromide. The process is carried out in solution with the starting polymers. Achieves highly selective bromination of aliphatic carbon-carbon double bonds, leaving aromatic rings largely unaffected. [0004] A potential application of brominated polymers is as a flame retardant additive for thermoplastic polymers such as polystyrene. In this application, the thermal properties of the brominated polymer are important. Thermoplastic polymers...

Claims

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Application Information

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IPC IPC(8): C08C19/18C08F36/16
CPCC08C19/12C08F8/20C08C19/14
Inventor B·A·金J·W·赫尔D·B·戈尔曼
Owner DOW GLOBAL TECH LLC
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