Polyethylene/polybutene thermoplastic elastomer alloy material and preparation method thereof

A thermoplastic elastomer and alloy material technology, applied in the preparation of polyethylene/polybutene thermoplastic elastomer alloy materials, polyethylene/polybutene thermoplastic elastomer alloy materials, can solve the problem of inability to achieve high conversion rate, identical Low content, low crystallinity and other problems, to achieve the effect of good hydrogen adjustment sensitivity, high polymerization activity, strong crystallization ability

Active Publication Date: 2015-07-15
QINGDAO UNIV OF SCI & TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

A series of studies subsequently reported polybutene-1 with low identical content (Chinese invention patent CN 101039967A (2007), US patent US 4,058,654, Chinese invention patent 201010139360). However, polybutene and butylene with low and medium identical content Owing to the low isotactic content and low crystallinity of ene-1 copolymer, it is very easy to dissolve in monomers or solvents, so the viscosity of the polymerization system is high. It is well known that the bulk method cannot achieve a high conversion rate due to the high viscosity in the later stage of polymerization, while The solution method requires a large amount of solvent and there are processes such as solvent recovery and polymer post-treatment

Method used

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  • Polyethylene/polybutene thermoplastic elastomer alloy material and preparation method thereof

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Experimental program
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Effect test

Embodiment 1

[0033]1L fully enclosed magnetic stirring stainless steel pressure polymerization kettle, pumped and replaced several times with high-purity nitrogen, then metered and added n-heptane, triethylaluminum (Al), MgCl2 supported TiCl4 catalyst (Ti content 2.5wt. %) 0.25g, add ethylene 0.05Kg, wherein Al / Ti=50 (molar ratio). Stir and polymerize at 0°C for 5 minutes, then heat up and depressurize to evacuate ethylene and n-heptane, flush it into a new reactor with inert gas, replace the inert gas with ethylene to a pressure of 0.2MPa, and then add 0.02MPa of hydrogen at 60 React at ℃ for 6 minutes, then evacuate ethylene and hydrogen, add 0.3Kg butene-1, react at 50℃ for 1 hour, evacuate butene-1, further feed ethylene to a pressure of 0.2MPa, maintain 6 minutes, then evacuate ethylene, add 0.3Kg of butene-1 and 0.01MPa hydrogen, reacted for 1h, and circulated twice like this. At the same time, the pre-polymerization of ethylene was continuously carried out in the pre-polymerization ...

Embodiment 2

[0035] 1L fully-sealed magnetic stirring gas-phase stainless steel pressure polymerization kettle, pumped and replaced several times with high-purity nitrogen, then metered 150ml of hexane, external electron donor, triethylaluminum (Al) and MgCl2 loaded tetrachloride into the reaction kettle Titanium oxide catalyst (titanium content 4wt%) 0.25g, add 0.03Kg of ethylene, wherein Al / Ti=80 (molar ratio), 0 ℃ of stirring polymerization 5min, then raise the temperature and depressurize to empty ethylene and hexane, use inert gas Pour it into a new reactor, replace the inert gas with ethylene to a pressure of 0.1MPa, then add 0.02MPa hydrogen to react at 50°C for 6 minutes, then empty the ethylene and hydrogen, add 0.3Kg butene-1, and react at 50°C for 1h , evacuate butene-1, further feed ethylene to a pressure of 0.1MPa, and maintain for 6min, then evacuate ethylene, add 0.3Kg of butene-1 and 0.01MPa hydrogen, react for 1h, and cycle like this for 3 times, after the drying is termina...

Embodiment 3

[0037] 10L fully-closed loop reactor, after pumping and replacing several times with high-purity nitrogen, metered and added heptane 150ml, triethylaluminum (Al) and MgBr successively in the reactor ) 1.0g, add ethylene 0.3Kg, wherein Al / Ti=50 (molar ratio). Stir and polymerize at 0°C for 5 minutes, then heat up and depressurize to evacuate ethylene and n-heptane, flush it into a new reactor with inert gas, replace the inert gas with ethylene to a pressure of 0.1MPa, and then add 0.02MPa of hydrogen at 40 React at ℃ for 8 minutes, then evacuate ethylene and hydrogen, add 3Kg of butene-1, react at 50℃ for 1 hour, evacuate butene-1, further feed ethylene to a pressure of 0.1MPa, and maintain it for 8 minutes, then evacuate ethylene, add 3Kg Butene-1 and 0.01MPa hydrogen, reacted for 1h, and circulated like this for 5 times, and obtained 4.2kg of powdery polymer directly after the drying was terminated. The properties of the alloy are shown in Table 1.

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Abstract

The invention discloses a polyethylene / polybutene thermoplastic elastomer alloy material and a preparation method thereof. The material contains, by mass, 5 to 98.9 parts of polybutene, 1 to 80 parts of polyethylene and 0.1 to 20 parts of an ethylene-butylene copolymer. According to the invention, the polyethylene / polybutene thermoplastic elastomer alloy material is synthesized through multi-stage sequential polymerization in virtue of a titanium and / or vanadium-loaded catalyst; after prepolymerization of ethylene, a section of bulk polymerization is carried out to produce a polyethylene particle with activity so as to continue initiation of polymerization of butylene-1, and a polyethylene shell can prevent adhesion of polymer particles in the process of polymerization of butylene-1; then bulk polymerization of ethylene and butylene-1 are further and successively carried out; and the above-mentioned operations are cyclically carried out. Cyclic operations of sequential polymerization enable good porosity of particles to be maintained, thereby allowing high polymerization activity to be maintained, and the cyclic operations also allow the content of the ethylene-butylene copolymer to be increased; and the prepared polyethylene / polybutene thermoplastic elastomer alloy material inherits the advantages of excellent shock resistance, heat resistance and creep properties of polybutene and high modulus and the like of polyethylene.

Description

technical field [0001] The invention relates to the field of a novel polyolefin thermoplastic elastomer material, in particular to a preparation method of a polyethylene / polybutene thermoplastic elastomer alloy material and a polyethylene / polybutene thermoplastic elastomer alloy material prepared by the method . Background technique [0002] Butene polymerization can prepare isotactic polybutene (isotacticity greater than 85%), polybutene thermoplastic elastomer (isotacticity 30-85%) and random polybutene according to the catalytic characteristics of the catalyst. Two polybutenes with different identical contents are blended to obtain a polybutene thermoplastic elastomer (PB-TPE), which can be used for pipes, films, fibers, and cable sheathing materials (US Patent No. 4,298,722). A series of studies subsequently reported polybutene-1 with low identical content (Chinese invention patent CN 101039967A (2007), US patent US 4,058,654, Chinese invention patent 201010139360). How...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08L23/06C08L23/20C08F110/02C08F110/08C08F4/646C08F4/68C08F4/685
CPCY02P20/52C08L23/06C08F110/02C08F110/08C08F210/16C08L23/20C08L2201/08C08L2205/03C08L2207/04C08L2308/00
Inventor 贺爱华姜秀波刘晨光邵华锋
Owner QINGDAO UNIV OF SCI & TECH
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