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Poly-1-butene elastomer material and preparation method thereof

An elastomeric material, elastomeric technology, applied in the field of organic polymers

Active Publication Date: 2011-09-21
QINGDAO UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] One of the purposes of the present invention is to use 1-butene to polymerize useful elastomeric materials, including PB-TPE, saturated and unsaturated elastomeric materials, and To overcome the above-mentioned shortage of performance and material variety of poly-1-butene thermoplastic elastomer materials, it can replace the existing ethylene-propylene copolymer and POE thermoplastic elastomers in some occasions, the new poly-1-butene elastomer material, It has excellent elasticity, the tensile strength can reach 14MPa and above, the elongation at break is greater than 300%, the tensile permanent deformation is less than 100%, and the 200% tensile permanent deformation is less than 50%.

Method used

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  • Poly-1-butene elastomer material and preparation method thereof

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Effect test

Embodiment 1

[0031] Example 1. Solution Polymerization Synthesis of Poly 1-Qualitative Thermoplastic Elastomers.

[0032] 10L fully enclosed magnetic stirring stainless steel pressure polymerization kettle (double-helical stirring paddle), pumping for 2 to 3 hours, during which it was replaced several times with high-purity nitrogen. Add the 1-butene / normal hexane solution that the monomer concentration is 40% in the polymerization kettle, with Ti / Bt=2×10 -5 (molar ratio, the same below), Al / Ti=300 (molar ratio, the same below), electron donor / Ti=5 (molar ratio), under stirring, add triisobutylaluminum (Al) and supported titanium catalyst successively (Ti) and ether electron donors were polymerized at 50° C. for 5 hours, and the polymer poly-1-butene was obtained directly after drying, with a monomer conversion rate of 76% and a catalytic efficiency of 148,000 g polymer / gTi. The content of isotactic pentads was determined by NMR to be 70%, that is, the content of isotactic poly-1-butene ...

Embodiment 2

[0033] Example 2. Synthesis of 1-butene / 1-hexene copolymer saturated elastomer by solution polymerization.

[0034] 10L fully enclosed magnetic stirring stainless steel pressure polymerization kettle (double-helical stirring paddle), pumping for 2 to 3 hours, during which it was replaced several times with high-purity nitrogen. Adding monomer volume concentration in the polymerization kettle is 1-butene and 1-hexene / normal hexane solution of 30%, wherein 1-hexene content is 10% (molar ratio) of monomer total amount, with Ti / monomer =4×10 -5 , Al / Ti=300, under stirring, add triisobutylaluminum (Al) and supported titanium catalyst (Ti) sequentially, polymerize at 40° C. for 8 hours, and obtain a polymer directly after drying, with a monomer conversion rate of 65%. The glass transition temperature of the polymer as determined by DSC is -23.5 degrees, the melting point is 80.8 degrees, and the crystallinity is 9.5%. The content of the 1-hexene structural unit in the polymer was...

Embodiment 3

[0035] Example 3. Synthesis of 1-butene / non-conjugated diene copolymer unsaturated elastomer by solution polymerization.

[0036] 10L fully enclosed magnetic stirring stainless steel pressure polymerization kettle (double-helical stirring paddle), pumping for 2 to 3 hours, during which it was replaced several times with high-purity nitrogen. Adding monomer volume concentration in the polymerization kettle is 1-butene and ethylidene norbornene (ENB) / normal hexane solution of 35%, wherein ENB content is 5% of monomer total amount, with Ti / monomer=6× 10 -5 , Al / Ti=400, under stirring, triisobutylaluminum (Al) and supported titanium catalyst (Ti) were metered in sequence, polymerized at 40° C. for 8 hours, and the polymer was obtained directly after drying, and the monomer conversion rate was 42%. The ENB structural unit content in the polymer was determined to be 3% by NMR.

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Abstract

The invention discloses a poly-1-butene elastomer material and a preparation method thereof. The elastomer material is 1-butene homopolymer which has the isotactic structure content represented by mmmm percent (detected by a nuclear magnetic resonance method) of 55-70 percent, the crystallinity of 10-25 percent and typical properties of a thermoplastic elastomer, or a saturated elastomer preparedby copolymerizing 1-butene and other alpha-olefins, or an unsaturated elastomer prepared by copolymerizing 1-butene and other unconjugated dialkene. In one preparation method, a bulk reaction extrusion polymerization process is adopted, and consists of three steps of prepolymerization, screw reaction extrusion polymerization, and double screw devolatilization and extrusion granulation; and in theother preparation method, the traditional solution or bulk polymerization process in a stirred tank reactor. The polymerization process is carried out segmentally at the temperature of between 0 and 100DEG C by using a catalyst system consisting of a titanium-supported catalyst and an organic aluminum compound. Ether, ester and silane nucleophilic reagents can serve as reagents for regulating regularity of polymer. Hydrogen is a molecular weight regulator for polymer. The elastomer material is similar to polyolefin elastomer (POE), ethylene-propylene rubber (EPR) and ethylene-propylene-diene monomer (EPDM) in the aspect of properties, and can be applied to the similar fields.

Description

technical field [0001] The invention belongs to the technical field of organic macromolecular polymers, and more specifically relates to the polymerization of 1-butene, an elastomer material formed therefrom, and a synthesis process and equipment thereof. Background technique [0002] 1-butene is a monoolefin second only to ethylene and propylene, and its polymer poly1-butene is the same as all materials polyethylene (HDPE, LDPE, LLDPE, POE) and polypropylene (iPP, PPR, sPP, aPP) According to the regularity and crystallinity of the chain structure, the properties are very different, including plastics, thermoplastic elastomers, elastomers and other materials. At present, the PB-1 industry is still blank in our country. [0003] High isotactic poly-1-butene, that is, high stereoregular poly-1-butene (identical content > 80%, also known as iPB), easy to crystallize, is a kind of high flexibility, high strength, high hardness Plastic, due to its outstanding creep resistance...

Claims

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Application Information

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IPC IPC(8): C08L23/20C08F10/08C08F2/02C08F2/06B29C47/92B29C48/92
CPCB29C48/92B29C2948/92704B29C48/04B29C2948/9259B29C2948/92885B29C2948/92895B29B7/487B29B7/603B29B7/726B29B7/728B29B7/845B29B7/86
Inventor 姚薇黄宝琛邵华锋贺爱华赵永仙刘晨光
Owner QINGDAO UNIV OF SCI & TECH
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