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Segmented copolymer with fully-saturated soft segment and crystallizable hard segment and preparation method of segmented copolymer

A technology of block copolymer and soft segment, applied in the field of block copolymer and its preparation, can solve the problems of limiting the application range and field of TPE, the destruction of physical cross-linking points, the limited range of Tg increase, etc., and achieve dimensional stability of the material. Improve the physical and mechanical properties, stabilize the physical cross-linking point, and simplify the process and process.

Active Publication Date: 2013-05-29
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, when the use temperature is higher than the softening temperature of the polystyrene segment (60-80°C), the physical crosslinking point will be destroyed, resulting in a low use temperature of the block copolymer and a significant decrease in mechanical properties. The above even lost the mechanical properties and could not be used normally as a material, which limited the application range and field of this type of TPE.
In order to improve the service temperature and material properties of this thermoplastic elastomer, styrene derivatives, such as methyl styrene or tert-butyl styrene, can be used to increase the T of the hard segment g Increase to 100-120°C or 130°C (see: Polymer: 2004, 45: 4719-4730; J.Polym.Sci.PartA: Polym.Chem., 1992, 30: 41-48), although this can be done to a certain extent Increase the use temperature, but the range of Tg increase is limited

Method used

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  • Segmented copolymer with fully-saturated soft segment and crystallizable hard segment and preparation method of segmented copolymer

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Embodiment 1

[0034] A. Under the protection of nitrogen at -80°C, add dichloromethane, n-hexane, 2,4,4-trimethyl-2-chloropentane (TMPCl), isobutylene (IB), N , N-dimethylacetamide (DMA) and TiCl 4 , making [IB]=1.8mol / L, TMPCl:TiCl 4 :DMA:IB=1:2:0.47:40 (molar ratio). After 60 minutes of polymerization reaction, add 1wt% NaOH mixed solution of ethanol and water (the volume ratio of ethanol and water is 1:1) to terminate the reaction, purify by dissolving and precipitating, vacuum dry at 40°C to constant weight, and obtain Based polyisobutylene macroinitiator, weight average molecular weight (M w ) is 6.3×10 3 , molecular weight distribution index (M w / M n ) is 2.1;

[0035] B. At -80°C and under the protection of nitrogen, add dichloromethane, n-hexane, triphenylamine (TPA), the above-mentioned 0.08mmol polyisobutylene macroinitiator, styrene (St) and AlCl to the polymerization reactor 3 , making [St]=0.63mol / L, polyisobutylene chain: AlCl 3 :TPA:St=1:1:0.2:150 (molar ratio). Aft...

Embodiment 2

[0037] A, the preparation method of double-ended tertiary chloropolyisobutylene macroinitiator are the same as embodiment 1 step A, just replace TMPC1 with 1,4-bis(2-chloro-2-propyl)benzene (DCC), and [IB ]=1.1mol / L, DCC:TiCl 4 :DMA:IB=1:10.2:1:308 (molar ratio). The M of the prepared double-ended tertiary chloropolyisobutylene macroinitiator w 1.2×10 4 ,M w / M n is 1.5;

[0038] B, the method for preparing block copolymer with above-mentioned polyisobutylene macroinitiator is the same as embodiment 1 step B, just polyisobutylene chain: AlCl 3 :TPA:isoprene:St=1:2:0.24:3:300 (molar ratio). The M of the gained polystyrene-b-polyisobutylene-b-polystyrene triblock copolymer w 2.4×10 5 ,M w / M n It is 5.1, the mass content of polystyrene is 79%, and the crystallization melting temperature range of polystyrene segment is 160°C-187°C.

Embodiment 3

[0040] The preparation method of A, tertiary chloropolyisobutylene macroinitiator is the same as embodiment 1 step 1, just [IB]=1.7mol / L, TMPCl: TiCl 4 :DMA:IB=1:5:0.5:200 (molar ratio). The M of the prepared tertiary chloropolyisobutylene macroinitiator w 2.6×10 4 ,M w / M n is 2.4;

[0041] B, the method for preparing block copolymer is the same as embodiment 1 step B, just replace TPA with triphenylphosphine (TPP), AlCl 3 Replaced by TiCl 4 , and the polyisobutylene chain: TiCl 4 :TPP:St=1:40:16:300 (molar ratio). The M of the gained polyisobutylene-b-polystyrene block copolymer w 4.9×10 4 ,M w / M n It is 1.4, the mass content of polystyrene is 73%, and the melting temperature of polystyrene segment crystallization is in the range of 150°C to 175°C.

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Abstract

The invention relates to a segmented copolymer with a fully-saturated soft segment and a crystallizable hard segment and a preparation method of the segmented copolymer. A segmented copolymer with a fully-saturated polyisobutene segment as the soft segment and a crystallizable polystyrene or polyalkyl substituted styrene segment as the hard segment is synthesized by combining cationic polymerization of isobutene with cationic steric polymerization of styrene or alkyl substituted styrene cations, wherein as the hard segment has the crystallizability, physical crosslinking points are more stable, not only is a self-enhancement role achieved, but also the softening temperature of the segmented copolymer is effectively improved, and the melting point ranges from 150 DEG C to 210 DEG C; and according to the segmented copolymer, the use temperature is improved by 50-110 DEG C, and the heat resistance, the material size stability and the physical and mechanical properties are also improved.

Description

Technical field: [0001] The present invention relates to a crystallizable block copolymer with fully saturated soft segment and hard segment and a preparation method thereof. Block copolymers of substituted styrenes, and methods of preparing such block copolymers by cationic polymerization. Background technique: [0002] Styrene-containing thermoplastic elastomers (TPE) are block 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, such as polystyrene-b-polybutadiene-b-poly Styrene (SBS), polystyrene-b-polybutadiene-b-polystyrene (SIS) or polystyrene-b-polyisobutylene-b-polystyrene (SIBS), is an important class of high molecular material. Among them, the polystyrene segment usually does not produce crystallization phenomenon. SBS and SIS are prepared by anionic polymerization method, and SIBS is usually ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F293/00C08F210/10C08F212/06C08F212/12C08F2/44
Inventor 吴一弦邹宇田程虹李贝特
Owner BEIJING UNIV OF CHEM TECH
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