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Preparation method of triblock acrylic acid ester thermoplastic elastomer

A thermoplastic elastomer and acrylate technology, which is applied in the field of three-block thermoplastic elastomers, can solve the problems of difficult removal and reuse of catalysts, difficulty in industrialization, and increased production costs, so as to improve heat aging resistance and chemical Responsiveness, low catalyst usage, and reduced sensitivity

Active Publication Date: 2013-10-30
CHANGZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The use of a large number of catalysts not only increases the production cost, but also the removal and reuse of catalysts is a problem that is not easy to solve, and the industrialization is difficult and difficult to carry out.

Method used

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  • Preparation method of triblock acrylic acid ester thermoplastic elastomer

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] (1) Preparation of bifunctional macroinitiator polybutylacrylate: preset molecular weight 60000 (initiator:monomer=1:600,

[0028] Conversion rate 80% stop reaction)

[0029] Add 76.90g (0.6mol) monomer BA, 0.3880g (1×10 -3 mol) difunctional initiator diα-bromoisobutyrate 1,4-butanediol, 0.02680g (1.2×10 -4 mol) Catalyst CuBr 2 , 0.3122g (1.8×10 - 3mol) ligand PMDETA, 0.9720g (2.4×10 -3mol) reducing agent Sn(EH)2, 15.23g toluene, 5g anisole, mix evenly, then vacuumize and fill with nitrogen, heat up and stir, and react at 75°C. Samples were taken every 30 minutes, and the monomer conversion rate was measured by gas chromatography and the molecular weight and molecular weight distribution were measured by gel permeation chromatography. After 12 hours of reaction, the conversion rate reached 79.5%, and the reaction ended. The solvent in the system was distilled off under reduced pressure to obtain a light yellow transparent viscous product. The product quality is 5...

Embodiment 2

[0036] (1) Use the same difunctional macromolecular initiator as in Example 1.

[0037] (2) Preparation of triblock copolymer poly(methyl methacrylate-b-butyl acrylate-b-methyl methacrylate): preset

[0038] Molecular weight 100000 (initiator:monomer=1:500, conversion rate 90% stop reaction)

[0039] In a 100mL four-neck flask with a thermometer, add 10.07g (0.1mol) monomeric methyl methacrylate (MMA), 10.65g (2×10 - 4mol) polybutylacrylate (PBA) macroinitiator, 0.002690g (2×10 -5 mol) Catalyst CuCl 2 , 0.3469g (3×10 -5 mol) Ligand PMDETA, 0.0081g (2×10 -5 mol) reducing agent Sn(EH)-2, 15.57g toluene, 5.13g anisole, mixed evenly, then evacuated and filled with nitrogen, heated and stirred, and reacted at 75°C. Samples were taken every 30 minutes, and the monomer conversion rate was measured by gas chromatography and the molecular weight and molecular weight distribution were measured by gel permeation chromatography. After 8.5 hours of reaction, the conversion rate reach...

Embodiment 3

[0043] (1) Preparation of bifunctional macromolecular initiator polybutylacrylate: preset molecular weight 2000 (initiator:monomer=1:20, conversion rate 80% stop reaction)

[0044] Add 76.78g (0.6mol) monomer BA, 10.8g (0.03mol) bifunctional initiator α-bromoisobutyrate 1,4-ethylene glycol, 0.04048g in a 250mL four-neck flask with a thermometer (3×10 -4 mol) catalyst CuCl2, 0.7005g (1.5×10 -3 mol) ligand tris-(N,N-dimethylaminoethyl)amine (Me 6 TREN), 0.2645g (1.5×10 -3 mol) ascorbic acid (AA), 15.15gs tetrahydrofuran, 3.20g toluene, mix evenly, then vacuumize and fill with argon, heat up and stir, and react at 60°C. Samples were taken every 30 minutes, and the monomer conversion rate was measured by gas chromatography and the molecular weight and molecular weight distribution were measured by gel permeation chromatography. After 6.5 hours of reaction, the conversion rate reached 85.2%, and the reaction ended. The solvent in the system was distilled off under reduced pres...

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Abstract

The invention relates to a preparation method of a triblock acrylic acid ester thermoplastic elastomer. The method is as below: first preparing poly butyl acrylate monomer; initiating polymerization of methyl methacrylate monomers by using the poly butyl acrylate monomer as a macro-molecular initiator to obtain poly(methyl methacrylate-b-butyl acrylate monomer-b-methyl methacrylate). The method can reduce the usage amount of a catalyst, reduce sensitivity to oxygen during a polymerization process; an environment-friendly reducing agent is employed; and the post-treatment is simple to reduce cost of industrial production.

Description

technical field [0001] The invention belongs to the field of chemical materials and relates to the synthesis of a three-block thermoplastic elastomer of methyl methacrylate and butyl acrylate. Background technique [0002] Thermoplastic elastomer (TPE) refers to a type of elastomer that has the elasticity of rubber at room temperature and can be plasticized at high temperature. Its products not only have the excellent properties of high elasticity, aging resistance and oil resistance of traditional cross-linked vulcanized rubber, but also have the characteristics of wider processing methods of ordinary plastics. Therefore, it is widely used in many fields such as automobiles, construction, household equipment, wires, cables, electronic products, food packaging, and medical equipment. [0003] The most widely used traditional thermoplastic elastomers are styrene-based thermoplastic elastomers, such as styrene-isoprene-styrene (SIS), styrene-butadiene-styrene (SBS) and their ...

Claims

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Application Information

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IPC IPC(8): C08F293/00C08F220/14C08F220/18C08F8/32C08F295/00
Inventor 任强张旸孙建平李坚汪称意
Owner CHANGZHOU UNIV
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