Middle-low molecular weight brominated multi-block copolymer flame retardant and solution three-step preparation method thereof

A multi-block copolymer, low molecular weight technology, applied in the field of polymer flame retardants, can solve the problems of no multi-block structure, single structure, low bromine content, etc., to achieve easy uniform dispersion, less dosage, bromine The effect of high content

Active Publication Date: 2018-06-08
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] These high-molecular-weight brominated PS and brominated SBS have low bromine content, while the low- and medium-molecular-weight brominated PS has a single molecular chain structure and does not have a multi-block structure

Method used

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  • Middle-low molecular weight brominated multi-block copolymer flame retardant and solution three-step preparation method thereof
  • Middle-low molecular weight brominated multi-block copolymer flame retardant and solution three-step preparation method thereof
  • Middle-low molecular weight brominated multi-block copolymer flame retardant and solution three-step preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] Embodiment 1, a kind of preparation method of medium and low molecular weight brominated polymer flame retardant:

[0044] 1. Using 2,4,6-tribromostyrene, 1,4-butadiene, and pentabromostyrene as polymerization monomers, azobisisobutyronitrile (AIBN) as an initiator, and 4-cyano-4 -(thiobenzoyl) valeric acid is a chain transfer agent, and obtains medium and low molecular weight brominated styrene-butadiene-brominated styrene triblock copolymers by three-step polymerization, and the steps are as follows:

[0045] (1), 80 grams of 2,4,6-tribromostyrene, 0.05 grams of azobisisobutyronitrile (AIBN), 5 grams of 4-cyano-4-(thiobenzoyl) valeric acid, 200ml as Tetrahydrofuran (THF) as a solvent was added to the reactor, and reacted at 60°C for 8 hours under the protection of nitrogen to obtain a brominated styrene homopolymer with a degree of polymerization of 12 and a molecular weight of 4092=12*341;

[0046] Remarks: The molecular weight is measured by GPC, and then the degre...

Embodiment 2

[0051] Embodiment 2, a kind of preparation method of medium and low molecular weight brominated polymer flame retardant:

[0052] 1. With pentabromobenzyl acrylate and isoprene as polymerized monomers, azobisisobutylamidine hydrochloride (AIBA) as initiator, and S-(thiobenzoyl) mercaptoacetic acid as chain transfer agent, Obtain medium and low molecular weight brominated acrylate-isoprene-brominated acrylate triblock copolymer by three-step polymerization, the steps are as follows:

[0053] (1), 52 grams of pentabromobenzyl acrylate, 0.06 grams of azobisisobutylamidine hydrochloride (AIBA), 6 grams of S-(thiobenzoyl) mercaptoacetic acid, and 200 ml of toluene as a solvent are added to the reaction kettle , under the protection of nitrogen, react at 65°C for 7 hours to obtain a brominated acrylate homopolymer with a degree of polymerization of 4, and a molecular weight of 2228=4*557;

[0054] (2), 95 grams of isoprene was added to the above-mentioned reaction kettle under the ...

Embodiment 3

[0058] Embodiment 3, a kind of preparation method of medium and low molecular weight brominated polymer flame retardant:

[0059] 1. Using pentabromobenzyl acrylate, 1,4-butadiene and pentabromostyrene as polymerization monomers, azobisisobutylimidazoline hydrochloride (AIBI) as initiator, phenyldithioacetic acid- 1-Phenylethyl ester is a chain transfer agent, and the medium and low molecular weight brominated styrene-butadiene-brominated acrylate triblock copolymer is obtained by three-step polymerization, and the steps are as follows:

[0060] (1), 40 grams of pentabromostyrene, 0.065 grams of azobisisobutylimidazoline hydrochloride (AIBI), 6.5 grams of phenyldithioacetic acid-1-phenylethyl ester, and 200ml of solvent xylene are added to the reactor , under the protection of nitrogen, react at 70°C for 5 hours to obtain a brominated styrene homopolymer with a degree of polymerization of 3, and a molecular weight of 1497=3*499;

[0061] (2) Add 45 grams of 1,4-butadiene into...

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Abstract

The invention discloses a solution three-step preparation method of a middle-low molecular weight brominated multi-block copolymer flame retardant. The preparation method comprises that brominated styrene and/or brominated acrylate and diolefin as polymerization monomers, an azo-compound or organic peroxide as an initiator and a dithioester derivative as a chain transfer agent undergo a polymerization reaction in a solvent to produce a middle-low molecular weight brominated styrene/acrylate-diolefin-styrene/acrylate triblock copolymer through a three step method, and the copolymer is brominated through a brominating agent to produce the middle-low molecular weight brominated multi-block copolymer flame retardant which is a middle-low molecular weight brominated styrene/acrylate-diolefin-styrene/acrylate triblock copolymer. The flame retardant has the characteristics of medium and low molecular weight, high bromine content and multi-block structure.

Description

technical field [0001] The invention relates to the field of polymer flame retardants, in particular to a brominated medium and low molecular weight styrene / acrylate-diene-styrene / acrylate triblock copolymer flame retardant and a preparation method thereof. Background technique [0002] Brominated flame retardants have the advantages of high efficiency and good thermal stability, and can meet the flame retardant requirements of various polymer materials, and their raw materials are abundant and cheap. They are currently the largest and most widely used in the market. One of the flame retardants. However, the currently commonly used small molecule brominated flame retardants (molecular weight less than 500, such as polybrominated diphenyl ethers, etc.) usually have the disadvantage of being easily precipitated from the polymer material matrix, and they will produce carcinogens such as dioxins when burned, resulting in Environmental problems, and the long-chain structure of p...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F293/00C08F236/06C08F236/08C08F220/30C08F212/14C08F8/20C08F2/38C08L77/00C08L25/06C08L67/00C08L53/02C08L55/02
CPCC08F2/38C08F8/20C08F293/005C08L55/02C08L77/00C08F2438/03C08L2201/02C08L2205/03C08L25/06C08L67/00C08L53/025C08F220/301C08F212/14
Inventor 曹堃杨文龙姚臻
Owner ZHEJIANG UNIV
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