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Polybutylene thermoplastic elastomer and preparation method thereof

A thermoplastic elastomer and polybutene technology, applied in the field of polybutene thermoplastic elastomer, can solve the problems of sharp increase in system viscosity, inability of conversion rate to be too high, and complicated separation of post-processing procedures.

Active Publication Date: 2017-07-04
QINGDAO UNIV OF SCI & TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] One of the purposes of the present invention is to solve the defects that present medium and low isotactic polybutenes exist in the polymerization process, such as the sharp increase of the system viscosity in the later stage of bulk polymerization, resulting in a conversion rate that cannot be too high, and the post-treatment process of the solvent in the solution polymerization method (solvent Separation, recovery and refining, etc.) and other complicated problems, providing a new green polymerization process

Method used

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  • Polybutylene thermoplastic elastomer and preparation method thereof

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Effect test

Embodiment 1

[0038] 3L full-sealed magnetic stirring stainless steel pressure polymerization kettle, pumped out and replaced with high-purity nitrogen several times, then metered and added triethylaluminum (Al), external electron donor diphenyldimethoxysilane (Si ), hydrogen and MgCl 2 Loaded TiCl 4 Catalyst (Ti content 2.5wt%) 0.25g, add butene 0.4Kg, wherein Al / Ti=60 (molar ratio), Si / Ti=6 (molar ratio), H 2 1.5g. Stir and polymerize at 30°C for 5 hours, remove unreacted monomers and hydrogen under reduced pressure, then add 0.4Kg of 1-pentene, 0.4Kg of butene, and 3g of hydrogen into the reactor, react at 30°C for 8 hours, and obtain powder directly after drying. Shaped polymer 757g. The properties of the alloy are shown in Table 1.

Embodiment 2

[0040] 3L full-sealed magnetic stirring stainless steel pressure polymerization kettle, pumped and replaced with high-purity nitrogen for several times, then metered and added triethylaluminum (Al), external electron donor cyclohexyltrimethoxysilane (Si), Hydrogen and MgCl 2 Loaded TiCl 4 Catalyst (Ti content 2.5wt%) 0.25g, add butene 0.4Kg, wherein Al / Ti=80 (molar ratio), Si / Ti=10 (molar ratio). Stir and polymerize at 30°C for 2 hours, separate and recover unreacted monomers and hydrogen, then add 0.1Kg of 1-hexene, 1Kg of butene, 2g of hydrogen into the reactor, react at 40°C for 6 hours, stop drying and directly obtain powdery polymerization Material 803g. The properties of the alloy are shown in Table 1.

Embodiment 3

[0042] Two 3L fully-sealed magnetic stirring stainless steel pressure polymerization kettles were drained and replaced with high-purity nitrogen for several times, then metered and added triethylaluminum (Al) and external electron donor diphenyldimethoxy into No. 1 reactor Silane (Si) and MgCl 2 Loaded TiCl 4 Catalyst (Ti content 2.5wt%) 0.30g, add butene 0.4Kg, wherein Al / Ti=120 (molar ratio), Si / Ti=10 (molar ratio). Add 10mL of hydrogen, stir and polymerize at 0°C for 5h, then recover the unreacted monomer and hydrogen through the separation device, transfer the material to the No. 2 reactor, add 0.05Kg of 1-octene, 0.5Kg of butene, 10mL of hydrogen, The reaction was carried out at ℃ for 4 hours, the recovery of unreacted monomers was terminated, and 526 g of powdery polymers were directly obtained after drying. The properties of the alloy are shown in Table 1.

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Abstract

The invention discloses a polybutylene thermoplastic elastomer and a preparation method thereof. The polybutylene thermoplastic elastomer comprises: 10%-50% by mass of isotactic polybutylene, 45%-89.9% by mass of a block copolymerized elastomer, and 0.1%-5% by mass of atactic polybutene. The block copolymerized elastomer is a copolymer of butene and high-grade aliphatic alpha-olefin of 5-10 carbon atoms or aromatic olefin of 8-12 carbon atoms, and is a high isotactic polybutylene long block composed copolymer. According to the preparation method of the polybutylene thermoplastic elastomer, first a two-stage polymerization method is employed, butene firstly undergoes homopolymerization under the action of a loaded titanium catalyst, then butene and a comonomer copolymerize so as to obtain the polybutylene thermoplastic elastomer; and second, a multi-stage sequential polymerization method is employed, butene firstly undergoes homopolymerization under the action of the loaded titanium catalyst, then butene and the comonomer copolymerize, and homopolymerization and copolymerization are carried out in multiple cycles so as to obtain the polybutylene thermoplastic elastomer finally.

Description

technical field [0001] The invention relates to a novel polyolefin thermoplastic elastomer material, in particular to a preparation method of polybutene thermoplastic elastomer and the polybutene thermoplastic elastomer prepared by the method. Background technique [0002] Butene polymerization can prepare isotactic polybutene (isotacticity greater than 85%), polybutene thermoplastic elastomer (isotacticity 40%-85%) and random polybutene according to the catalytic characteristics of the catalyst. In 1981, U.S. Patent No. 4,298,722 reported a method of blending two polybutenes with different identical contents to prepare a polybutene thermoplastic elastic material that can be used for pipes, films, fibers, and cable sheathing materials. Body materials, opened up a new field of polybutylene thermoplastic elastomers. In 1982, Shell's European patent EP 0081787A1 reported a polybutene material with thermoplastic elastomer properties synthesized by a supported titanium catalyst ...

Claims

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Application Information

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IPC IPC(8): C08L53/00C08L23/20C08F110/08C08F293/00C08F4/646
CPCC08F4/6465C08F110/08C08F293/00C08L53/00C08L2205/03C08L2205/025C08L2207/10C08L2207/04C08L23/20
Inventor 邵华锋马韵升贺爱华栾波王日国姚刚
Owner QINGDAO UNIV OF SCI & TECH
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