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Rare earth catalytic system based high-cis styrene/isoprene/butadiene ternary polymer and its preparation method

A technology of butadiene terpolymer and terpolymer, applied in the field of polymer materials, can solve the problems of high final product cost, unstable rare earth catalytic system activity and orientation ability, expensive organoaluminoxane, etc. , to achieve the effect of narrow molecular weight distribution index

Active Publication Date: 2012-11-21
DALIAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] Chinese invention patent ZL201010271998.0 discloses "rare earth catalyst system styrene / isoprene / butadiene ternary random copolymer and its preparation method", which is based on rare earth organic compound / organoaluminoxane / cyclopentadiene styrene / isoprene / butadiene ternary random copolymer was successfully prepared in cyclohexane or n-hexane as the catalytic system, but the rare earth catalyst disclosed in the invention The system must contain organoaluminoxane components, which brings the following disadvantages: (1) The price of organoaluminoxane is relatively expensive, resulting in higher cost of the final product; (2) Different batches of organoaluminoxane have different structures and compositions. difference, leading to unstable activity and orientation ability of the rare earth catalytic system; (3) Due to the use of organoaluminoxane (such as: methylaluminoxane MAO), the third component of the catalytic system must be a cyclopentadienyl derivative , resulting in insufficient ability of the catalytic system to orient the cis-1,4 structure of butadiene and isoprene

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] At room temperature, sequentially add 0.5mL NdV to the 20mL catalyst reactor 3 (0.167mol / L n-hexane solution), 1.3mLTIBA (25wt% n-hexane solution), 0.08mL isoprene, react at 30°C for 10min, then add 0.36mLCHCl 3 (0.68mol / L cyclohexane solution) for 40min, shake to mix evenly.

[0030] Using cyclohexane as a solvent, the monomer concentration is 39g / 100mL, add 1.0g of butadiene, 1.3g of isoprene, and 3.9g of styrene into a 60mL polymerization reactor according to the ratio; take 1.0mL of aged Catalyst (Nd / monomer molar ratio is 5.0×10 -4 ) into the polymerization bottle. Shake to make it evenly mixed, and react at 70°C for 6h. The reaction was terminated with an ethanol solution containing 1% 2,6-di-tert-butyl-p-methylphenol, and the polymer was precipitated in excess ethanol. After being washed with ethanol and extruded, it was vacuum-dried at 40°C for 24 hours.

[0031] The product structure analysis results are as follows: the content of styrene is 7.8wt%, the con...

Embodiment 2

[0033] At room temperature, sequentially add 0.5mL NdV to the 20mL catalyst reactor 3 (0.167mol / L n-hexane solution), 1.3mL DIBAH (1.0mol / L n-hexane solution), 0.08mL isoprene, react at 50°C for 10min, then add 0.36mL CHCl 3 (0.68mol / L cyclohexane solution) for 40min, shake to mix evenly.

[0034] Using cyclohexane as a solvent, the monomer concentration is 21g / 100mL, add 1.0g of butadiene, 1.3g of isoprene, and 3.9g of styrene into a 60mL polymerization reactor according to the ratio; take 0.4mL of aged Catalyst (Nd / monomer molar ratio is 2.0×10 -4 ) into the polymerization bottle. Shake to make it evenly mixed, and react at 70°C for 24h. The reaction was terminated with an ethanol solution containing 1% 2,6-di-tert-butyl-p-methylphenol, and the polymer was precipitated in excess ethanol. After being washed with ethanol and extruded, it was vacuum-dried at 40°C for 24 hours.

[0035] Product structure analysis result is as follows: the content of styrene is 8.5wt%, the co...

Embodiment 3

[0037] At room temperature, sequentially add 1.0mL NdV to the 20mL catalyst reactor 3 (0.167mol / L n-hexane solution), 2.5mL DIBAH (1.0mol / L n-hexane solution), 0.16mL isoprene, react at 10°C for 10min, then add 0.73mL CHCl 3 (0.68mol / L cyclohexane solution) for 40min, shake to mix evenly.

[0038] Using cyclohexane as a solvent, the monomer concentration is 39g / 100mL, add 2.0g of butadiene, 2.6g of isoprene, and 7.8g of styrene into a 60mL polymerization reactor according to the ratio; take 1.9mL of aged Catalyst (Nd / monomer molar ratio is 5.0×10 -4 ) into the polymerization bottle. Shake to make it evenly mixed, and react at 70°C for 12h. The reaction was terminated with an ethanol solution containing 1% 2,6-di-tert-butyl-p-methylphenol, and the polymer was precipitated in excess ethanol. After being washed with ethanol and extruded, it was vacuum-dried at 40°C for 24 hours.

[0039] Product structure analysis result is as follows: the content of styrene is 15.9wt%, the c...

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Abstract

The invention discloses a rare earth catalytic system based high-cis styrene / isoprene / butadiene ternary polymer and its preparation method. The polymer is characterized in that the polymer comprises 5-70wt% of styrene, 10-70wt% of butadiene, 10-70wt% of isoprene, 70-98wt% of 1,4-polyisoprene, 70-98wt% of 1,4-polybutadiene, and 35wt% or more of cis-1,4-polybutadiene; and the rare earth catalytic system does not contain organic aluminoxane, and comprises a rare earth neodymium carboxylate, alkyl aluminum, a chloralkane and a conjugated diolefin. The ternary polymer disclosed in the invention has the characteristics of high styrene content, high cis-structure content, high irregular distribution, narrow molecular weight distribution and the like.

Description

technical field [0001] The invention belongs to the technical field of polymer materials, and relates to a kind of high-cis-styrene / isoprene / butadiene terpolymer based on a rare earth catalyst system and a preparation method thereof. Background technique [0002] Styrene / isoprene / butadiene terpolymer (SIBR) is a polybutadiene rubber (BR), styrene-butadiene rubber (SBR), polyisoprene rubber (IR), butadiene rubber ( IBR) is an integrated rubber that combines the characteristics of four types of rubber into one body and has excellent comprehensive performance; there are segments that are as flexible as butadiene rubber, and segments that are less flexible such as styrene-butadiene rubber. Segments of different structures provide rubber with different properties. The flexible segment can make the rubber have excellent low-temperature performance, and can also reduce rolling resistance and improve the wear resistance of the rubber; the more rigid segment can increase the wear res...

Claims

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Application Information

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IPC IPC(8): C08F212/08C08F236/10C08F236/08C08F236/06C08F4/58C08F4/54C08F4/52
Inventor 李杨许蔷申凯华史正海王艳色王玉荣
Owner DALIAN UNIV OF TECH
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