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Brominated multi-block copolymer flame retardant with medium-and-low molecular weight and three-step preparation method for solution thereof

A brominated multi-block and low-molecular-weight technology, applied in the field of polymer flame retardants, can solve the problems of low bromine content, no multi-block structure, single structure, etc. good burning effect

Inactive Publication Date: 2018-07-06
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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  • Brominated multi-block copolymer flame retardant with medium-and-low molecular weight and three-step preparation method for solution thereof
  • Brominated multi-block copolymer flame retardant with medium-and-low molecular weight and three-step preparation method for solution thereof
  • Brominated multi-block copolymer flame retardant with medium-and-low molecular weight and three-step preparation method for solution thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] Embodiment 1, a kind of preparation method of medium and low molecular weight brominated polymer flame retardant:

[0040] 1. Using styrene and 1,4-butadiene as polymerization monomers, azobisisobutyronitrile (AIBN) as initiator, and 4-cyano-4-(thiobenzoyl)valeric acid as chain transfer agent, obtain medium and low molecular weight styrene-butadiene-styrene triblock copolymers by three-step polymerization, and the steps are as follows:

[0041] (1), 80 grams of styrene, 0.05 grams of azobisisobutyronitrile (AIBN), 5 grams of 4-cyano-4-(thiobenzoyl) valeric acid, and 200 ml of solvent tetrahydrofuran (THF) were added to the reaction kettle , under the protection of nitrogen, react at 60°C for 8 hours to obtain a styrene homopolymer with a degree of polymerization of 40;

[0042] (2) Under the protection of nitrogen, add 100 grams of 1,4-butadiene into the above reaction kettle, and react at 60° C. for 8 hours to obtain a styrene-butadiene diblock copolymer with a degree...

Embodiment 2

[0046] Embodiment 2, a kind of preparation method of medium and low molecular weight brominated polymer flame retardant:

[0047] One, with styrene, isoprene as polymerization monomer, azobisisobutylamidine hydrochloride (AIBA) as initiator, S-(thiobenzoyl) mercaptoacetic acid as chain transfer agent, through three steps Method polymerization obtains medium and low molecular weight styrene-isoprene-styrene triblock copolymer, and the steps are as follows:

[0048] (1), 15 grams of styrene, 0.02 gram of azobisisobutylamidine hydrochloride (AIBA), 2 gram of S-(thiobenzoyl) mercaptoacetic acid, 200ml of solvent toluene are added to the reaction kettle, under nitrogen protection , and reacted at 65°C for 7 hours to obtain a styrene homopolymer with a degree of polymerization of 19;

[0049] (2) Under the protection of nitrogen, 35 grams of isoprene was added into the above reaction kettle, and reacted at 65° C. for 7 hours to obtain a styrene-isoprene diblock copolymer with a deg...

Embodiment 3

[0053] Embodiment 3, a kind of preparation method of medium and low molecular weight brominated polymer flame retardant:

[0054] 1. Using styrene and isoprene as polymerization monomers, azobisisobutylimidazoline hydrochloride (AIBI) as initiator, and 1-phenylethyl phenyldithioacetate as chain transfer agent, Obtain medium and low molecular weight styrene-isoprene-isoprene triblock copolymers by three-step polymerization, the steps are as follows:

[0055] (1), 20 gram styrenes, 0.08 gram azobisisobutylimidazoline hydrochloride (AIBI), 8 gram phenyldithioacetic acid-1-phenylethyl esters, 200ml solvent xylenes are added in the reactor, Under the protection of nitrogen, react at 70°C for 5 hours to obtain a styrene homopolymer with a degree of polymerization of 6;

[0056] (2) Under the protection of nitrogen, 100 grams of isoprene was added into the above reaction kettle, and reacted at 70° C. for 5 hours to obtain a styrene-isoprene diblock copolymer with a degree of polymer...

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Abstract

The invention discloses a three-step preparation method for a solution of a brominated multi-block copolymer flame retardant with medium-and-low molecular weight. According to the invention, a reversible addition-tragmentation chain transfer (RAFT) polymerization method is adopted for preparation, and a styrene-butadiene / isoprene-styrene triblock copolymer with medium-and-low molecular weight is obtained by polymerization through a three-step method in a solvent with styrene and 1,4-butadiene / isoprene as polymerization monomers, an azo compound or an organic peroxide as an initiator and a dithioester derivative as a chain transfer agent; and after the copolymer is brominated with a brominating agent, the brominated multi-block copolymer flame retardant with medium-and-low molecular weight(a polymerization degree of 16 to 156) is obtained, i.e., a brominated styrene-butadiene / isoprene-styrene triblock copolymer bromine-based flame retardant with medium-and-low molecular weight is obtained. The triblock copolymer flame retardant provided by the invention has the characteristics of medium 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-butadiene / isoprene-styrene triblock copolymer flame retardant and a preparation method thereof. Background technique [0002] Brominated flame retardants have the advantages of high flame retardant 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 str...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F293/00C08F236/06C08F212/08C08F236/08C08F2/38C08F4/04
CPCC08F8/20C08F2/38C08F4/04C08F293/005C08F236/06C08F212/08C08F236/08
Inventor 曹堃杨文龙姚臻
Owner ZHEJIANG UNIV
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