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Catalyst system and method for polymerizing butadiene

A catalyst and butadiene technology, applied in the field of catalyst systems, can solve the problems of poor stability of the catalytic system, high gel content, poor dispersion, etc., and achieve the effects of easy control of the reaction, low gel content, and high catalytic activity

Active Publication Date: 2011-05-04
CHINA PETROLEUM & CHEM CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0015] Due to the poor solubility and poor dispersibility of the boron trifluoride ether complex in the nickel-based catalytic system in the prior art, the utilization rate of boron is low, and the gel content is high, and Al / B can The adjustment range is narrow, the stability of the catalytic system is poor, the product quality often fluctuates, and the molecular weight of polybutadiene is difficult to effectively control. At present, my country only produces medium Mooney butadiene rubber with a Mooney viscosity of about 45, resulting in the grade of nickel-based butadiene rubber. Single, while polybutadiene has a higher gel content

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] Under the protection of inert gas, the boron trifluoride complex is prepared by boron trifluoride and complex ligand in n-hexane solvent at room temperature. The complex ligand is octanol and methyl butyl ketone, wherein octanol and methyl butyl ketone The molar ratio of ketones is 1.

[0037] in N 2 Under the protection, 40 mL of n-hexane solution with a butadiene concentration of 2.5 mol / L was added to a 150 mL polymerization reactor, and at 30 °C, a solution containing 3.9 × 10 -6 mol of nickel naphthenate and 2.4 x 10 -5 mol of triisobutylaluminum aging solution, then add 3.9×10 -5 mol of boron trifluoride complex, polymerized for 18 hours to terminate the reaction. The conversion rate was 74%, the intrinsic viscosity ([η]) of the polybutadiene product was 5.61 dL / g, the gel was undetectable, the cis-1,4 content was 98.2%, and the trans-1,4 content was 1.1%, 1,2-structure content of 0.7%.

Embodiment 2

[0039] A boron trifluoride complex is prepared by using 2-heptanone and hexanol with a molar ratio of 1 as a ligand.

[0040] in N 2 Under the protection, 40 mL of n-hexane solution with a butadiene concentration of 2.5 mol / L was added to a 150 mL polymerization reactor, and at 30 °C, a solution containing 9.8 × 10 -5 mol of nickel naphthenate and 5.9 x 10 -4 mol of triisobutylaluminum aging solution, then add 9.8×10 -4 mol of boron trifluoride complex, the reaction was terminated after 18 hours of polymerization. The conversion was 94%, the [η] of the polybutadiene product was 3.35 dL / g, the gel was not detectable, M w 6.5×10 5 g / mol, M w / M n It is 3.3, the content of cis-1,4 is 97.7%, the content of trans-1,4 is 1.3%, and the content of 1,2-structure is 1.0%.

Embodiment 3

[0042] Using methyl isobutyl ketone and decanol with a molar ratio of 1 as ligands, a boron trifluoride complex is prepared.

[0043] in N 2 Under the protection, 40 mL of n-hexane solution with a butadiene concentration of 2.5 mol / L was added to a 150 mL polymerization reactor, and at 30 °C, a solution containing 9.8 × 10 -6 mol of nickel naphthenate and 5.9 x 10 -5 mol of triisobutylaluminum aging solution, then add 2.0×10 -5 mol of boron trifluoride complex, the reaction was terminated after 18 hours of polymerization. The conversion was 20%, the [η] of the polybutadiene product was 4.32 dL / g, the gel was not detectable, M w 7.4×10 5 g / mol, M w / M n It is 2.4, the content of cis-1,4 is 98.1%, the content of trans-1,4 is 1.1%, and the content of 1,2-structure is 0.8%.

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Abstract

The invention relates to a catalyst system and a method for polymerizing butadiene by using the catalyst system. The catalyst system comprises soluble nickel compounds, organic aluminum compounds and boron triflouride complexes, wherein ligands are mixtures of any two compounds of oxide compounds including alcohols, esters, ketones and ethers. The catalytic system is high in activity, can catalyzethe polymerization of 1,3-butadiene in an alkaline solvent at a temperature of between 20 DEG C below zero and 90 DEC G to synthesize cis-rich polybutadiene rubber having little gel but a cis-contentof over 97 percent, even up to 99 percent. The system and the method can realize stable production with low energy consumption in a polymerization process, light rubber sticking in a polymeric kettleand pipes and convenient operation.

Description

Technical field: [0001] The present invention relates to a catalyst system and a method for preparing high-cis polybutadiene by butadiene polymerization using the catalyst system. Background technique: [0002] As an important supporting industry and an internationally recognized strategic material, automotive tires have always been highly valued by world powers such as the United States and Europe for their technological and industrial development. Rubber is a necessity for the automotive tire industry. Rubber includes natural rubber and synthetic rubber. At present, natural rubber is used in combination with cis-butadiene rubber and styrene-butadiene rubber to make car tire casings. The development trend of the tire industry is high performance, safety, energy saving, consumption reduction and durability. [0003] Polybutadiene rubber (BR) is currently the second largest rubber species in the world after styrene-butadiene rubber, accounting for about 20% of the world's ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F4/70C08F136/06
Inventor 吴一弦李德高赵姜维乔雨露
Owner CHINA PETROLEUM & CHEM CORP
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