Production of soft-segment total saturated block copolymer

A block copolymer and soft segment technology, which is applied in the field of block copolymer preparation, can solve the problems of inconvenient industrial application, high price, and increased cost, and achieve the effect of simple method, low cost, and environmental friendliness

Active Publication Date: 2007-06-20
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The preparation of the three-block copolymer disclosed in the above-mentioned patents is double-terminal initiation, and adopts an organic halide compound containing a tertiary (aryl) alkyl group connected to a functional group as an initiator with a special structure. This type of compound is a non-industrial product. It needs to be synthesized in the laboratory by itself, which will inevitably bring inconvenience to industrial applications
Need to consume a certain amount of initiator and / or proton-scavenging agent, as well as expensive end-capping agent, resulting in a significant increase in cost

Method used

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  • Production of soft-segment total saturated block copolymer

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031]At -60°C and under the protection of high-purity nitrogen, 9ml of dichloromethane (CH 2 Cl 2 ), 9ml n-hexane (n-Hex), 4.4×10 -3 mmol H 2 O, 24mmol isobutene and 0.132mmol N,N-dimethylacetamide were mixed evenly, and after precooling for half an hour, 2mmol TiCl was added 4 Initiate polymerization, after polymerization reaction 60 minutes, add the styrene solution (concentration is 1.0mol / L, CH 2 Cl 2 / n-Hex=1 / 1) to continue the polymerization. After 50 minutes, 10 mL of ethanol / water (V / V=50 / 50) mixed solution containing 1 wt% NaOH was added to terminate the polymerization. After removing the solvent and unreacted monomers, the polymerized product was washed and purified with water several times, and dried in vacuum at 40°C until constant weight. The conversion rate of isobutylene in the first stage is 99.2%, and the weight average molecular weight of the polyisobutylene segment is 8.1×10 4 ; The peak molecular weight is 8.7×10 4 ; Molecular weight distribution i...

Embodiment 2

[0033] Add 9ml of CH 2 Cl 2 , 9ml n-Hex, 2.0×10 -4 mmol H 2 O, 24 mmol isobutene, 0.10 mmol acetone and 0.03 mmol N, N-dimethylacetamide were mixed evenly, and after half an hour of pre-cooling, 2 mmol TiCl was added 4 Initiate polymerization, after polymerization reaction 60 minutes, add 24ml and contain 0.036mmol 2, the p-methylstyrene solution of 6-di-tert-butylpyridine, 0.12mmol acetone and 0.03mmol N, N-dimethylacetamide (concentration is 1.0mol / L, CH 2 Cl 2 / n-Hex=1 / 1) to continue the polymerization reaction. After 70 minutes, 10 mL of ethanol / water (V / V=50 / 50) mixed solution containing 1 wt% NaOH was added to terminate the polymerization. After removing the solvent and unreacted monomers, the polymerized product was washed and purified with water several times, and dried in vacuum at 40°C until constant weight. The conversion rate of isobutylene in the first stage is 99.7%, and the weight average molecular weight of the polyisobutylene segment is 7.18×10 4 ; The...

Embodiment 3

[0035] Add 26ml CH 2 Cl 2 , 26ml n-Hex, 3.74×10 -4 mmol H 2 O, 10.4mmol styrene and 0.40mmol N,N-dimethylacetamide were mixed evenly, and after precooling for half an hour, 6.4mmol TiCl was added 4 The polymerization was initiated, and after 70 minutes of polymerization, a small amount of sample was taken out to measure the molecular weight of polystyrene. Add 58mmol of isobutylene to continue the second stage of polymerization, react for 80 minutes, and take out a small amount of sample to measure the molecular weight of polystyrene-b-polyisobutylene copolymerization product. Then add 7ml of styrene solution containing 0.06mmol N,N-dimethylacetyl (concentration is 2.0mol / L, CH 2 Cl 2 / n-Hex=1 / 1) proceed to the third stage of polymerization. After 50 minutes, 20 mL of ethanol / water (V / V=50 / 50) mixed solution containing 1 wt % NaOH was added to terminate the polymerization. After removing the solvent and unreacted monomers, the polymerized product was washed and purified...

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Abstract

Production of soft-segment saturated block multi-polymer is carried out by taking styrene monomer or isoalkene as the first monomer under cation polymerization, taking water as initiating agent, taking Lewis acid as coinitiator in polymer system containing solvent and additive, controlling cation polymerization, adding into isoalkene containing additive or styrene the second kind monomer to two-block copolymer or adding into the first monomer containing additive and the third segment polymerizing to obtain the three-block copolymer. It's simple and cheap.

Description

technical field [0001] The invention relates to a method for preparing a block copolymer, more specifically, the invention relates to a method for preparing a soft-segment fully saturated block copolymer by cationic polymerization. Background technique [0002] Synthetic thermoplastic elastomers (TPE) generally involve the preparation of triblock copolymers with rubbery soft segments and plastic hard segments. The plastic hard segment is usually a vinyl aromatic compound such as polystyrene, while the rubbery soft segment is usually polybutadiene or polyisoprene. The most important styrenic TPE material is the ABA type thermoplastic elastomer polystyrene-b-polybutadiene-b-polystyrene triblock copolymer (SBS), and the preparation of SBS by living anionic polymerization method is industrially , both commercially and practically. However, the soft polybutadiene segment in the molecular structure of SBS contains highly unsaturated double bonds, and its chemical properties are ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F297/00
Inventor 吴一弦邱迎昕张成龙冉奋武冠英
Owner BEIJING UNIV OF CHEM TECH
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