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A kind of styrenic block copolymer and preparation method thereof

A technology of block copolymers and styrenes, applied in the field of styrenic block copolymers and their preparation, can solve the problems of difficult control of sulfonation reaction process, complex monomer structure, cumbersome steps of hydroxyl functionalized polymers, etc.

Active Publication Date: 2022-02-11
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the monomer structure of the former is complicated, and the preparation process is cumbersome. The monomers used are non-commercial products, which require special synthesis and refining, and the steps to obtain hydroxyl-functionalized polymers are also cumbersome. The sulfonation reaction process of the latter is usually difficult to control and prone to occur. side effects

Method used

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  • A kind of styrenic block copolymer and preparation method thereof
  • A kind of styrenic block copolymer and preparation method thereof
  • A kind of styrenic block copolymer and preparation method thereof

Examples

Experimental program
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preparation example Construction

[0027] The preparation method of the styrenic block copolymer provided by the invention comprises the following steps:

[0028] S1, isobutylene, styrene and p-methylstyrene are obtained through sequential living cationic copolymerization in the presence of an initiating system to obtain a polyisobutylene segment with a structure shown in formula (1) and styrene with a structure shown in formula (5) Block copolymers (SMB) of random copolymerized segments with p-methylstyrene structural units;

[0029]

[0030] Wherein, n is 200~1800, the total number (m) of styrene structural units accounts for 0.5~29% of the total moles of all structural units, and the total number (g) of p-methylstyrene structural units accounts for 0.5~29% of the total moles of all structural units. 1.05-43%.

[0031] S2, carry out bromination reaction / chlorination reaction in organic solvent with the block copolymer obtained in step S1 and bromination / chlorination reagent, obtain bromination / chlorinatio...

Embodiment 1

[0078] This example serves to illustrate the azonia-ionized poly[(p-methylstyrene-co-styrene)-b-isobutylene-b-(styrene-co-p-methylstyrene)] block copolymer (FSMB -1) Preparation and properties.

[0079] Preparation of S1 and SMB-1

[0080] Under the protection of high-purity nitrogen at -78°C, 110 mL of dichloromethane, 164 mL of n-hexane, 0.3 mol of isobutene (IB) and 0.845 mmol of bifunctional initiator 1,4-bis(2-chloro-2 -Propyl)benzene (DCC), add 7.0mL containing co-initiator FeCl 3 With the additive isopropanol (POH) solution (of which: FeCl 3 :POH=1:1.4), so that the concentration of IB in the reaction system is 1.0mol / L, DCC:FeCl 3 : IB=1:3.6:355 (molar ratio), reaction 15min, IB monomer is fully converted, obtains polyisobutylene double-end active chain; Add 100mL containing styrene (St, 68.7mmol) and p-methylstyrene (pMS, 34.4mmol) in dichloromethane / normal hexane (4 / 6, v / v) mixed solution, further carry out active cationic block copolymerization reaction, the rea...

Embodiment 2

[0088] The preparation method of S1 and SMB-2 is the same as step S1 in Example 1. Under the protection of high-purity nitrogen at -80°C, add 220mL of dichloromethane, 328mL of n-hexane, 0.6mol of isobutene and 3.38mmol of DCC into the polymerization reactor and mix well, add 14mL of FeCl containing co-initiator 3 With POH solution (where: FeCl 3 :POH=1:1.4), so that the concentration of IB in the reaction system is 1.0mol / L, DCC:FeCl 3 : IB=1:3.6:178 (molar ratio), polymerization reaction 15min, IB monomer is fully transformed, obtains polyisobutylene double-end active chain; Only the feeding amount of St and pMS mixed solution is reduced, add 120mL containing 82.4mmol styrene and 41.2mmol methylene chloride / n-hexane (4 / 6, v / v) mixed solution of p-methylstyrene, obtain poly(styrene-co-p-methylstyrene)-b-polyisobutylene-b-poly( Styrene-co-p-methylstyrene) triblock copolymer SMB-2.

[0089] S2, BSMB-2 preparation method is the same as step S2 in embodiment 1, just Br2 The am...

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Abstract

The invention belongs to the field of elastomers, and discloses a styrenic block copolymer and a preparation method thereof. The preparation method of the styrenic block copolymer comprises: S1, obtaining a block copolymer through sequential living cationic copolymerization reactions of isobutylene, styrene and p-methylstyrene in the presence of a cationic initiator; S2, making the block copolymer Segment copolymer and bromination / chlorination reagent carry out bromination / chlorination reaction, obtain bromination / chlorination block copolymer; S3, carry out side group nitrogenium / phosphonium ion to bromination / chlorination block copolymer functionalization, amine functionalization or hydroxyl functionalization. The interaction between the side group functional groups of the styrene block copolymer provided by the present invention can form thermally reversible physical cross-linking points and three-dimensional network structure, endow the material with excellent self-repairing performance at a certain temperature, and is beneficial to improve the durability of the material. Using temperature and heat stability and hydrophilicity, improves mechanical properties, both strengthens and toughens.

Description

technical field [0001] The invention belongs to the field of elastomers, and in particular relates to a styrenic block copolymer and a preparation method thereof. Background technique [0002] Thermoplastic elastomer (TPE) is a type of elastomer that has rubber elasticity at room temperature and can be plasticized and processed at high temperature. The structural characteristics of thermoplastic elastomers are different resin segments and rubber segments composed of chemical bonds. The resin segments form physical cross-linking points by virtue of inter-chain forces, and the rubber segments are highly elastic segments that contribute to elasticity. Therefore, thermoplastic elastomers have the physical and mechanical properties of vulcanized rubber and the processing properties of thermoplastics, and are widely used in wire and cable, automobile manufacturing, household appliances, medical equipment and other fields. There are many types of thermoplastic elastomers, which ar...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F8/44C08F8/40C08F8/12C08F8/30C08F8/22C08F293/00
CPCC08F8/44C08F8/40C08F8/12C08F8/30C08F8/22C08F293/005
Inventor 吴一弦魏志涛张航天
Owner BEIJING UNIV OF CHEM TECH
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