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, poor solubility, and high gel content of the catalytic system, and achieve the effects of easy control of the reaction, small temperature fluctuations, and low gel content

Active Publication Date: 2009-11-18
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 an inert gas, boron trifluoride complexes are configured by boron trifluoride and complex ligands in n-hexane solvent at room temperature. The complex ligands are octanol and methyl butyl ketone, wherein octanol and methyl butyl The molar ratio of ketones is 1.

[0037] in N 2 Under protection, add 40mL n-hexane solution with a butadiene concentration of 2.5mol / L in a 150mL polymerization reactor, and add 3.9×10 -6 mol of nickel naphthenate and 2.4×10 -5 mol of the aging solution of triisobutylaluminum, and then add 3.9×10 -5 mol of boron trifluoride complex, polymerized for 18 hours, and terminated the reaction. The conversion rate is 74%, the intrinsic viscosity ([η]) of the polybutadiene product is 5.61dL / g, the gel cannot be detected, the cis-1, 4 content is 98.2%, and the trans-1, 4 content is 1.1%, 1,2-structure content is 0.7%.

Embodiment 2

[0039] Using 2-heptanone and hexanol at a molar ratio of 1 as a ligand, a boron trifluoride complex is prepared.

[0040] in N 2 Under protection, add 40mL n-hexane solution with a butadiene concentration of 2.5mol / L in a 150mL polymerization reactor, and add 9.8×10 -5 mol of nickel naphthenate and 5.9×10 -4 mol of the aging solution of triisobutylaluminum, and then add 9.8×10 -4 mol of boron trifluoride complexes, the reaction was terminated after 18 hours of polymerization. Conversion rate is 94%, and the [η] of polybutadiene product is 3.35dL / g, and gel can't be detected, M w 6.5×10 5 g / mol, M w / M n 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] The boron trifluoride complex is formulated with methyl isobutyl ketone and decyl alcohol at a molar ratio of 1 as ligands.

[0043] in N 2 Under protection, add 40mL n-hexane solution with a butadiene concentration of 2.5mol / L in a 150mL polymerization reactor, and add 9.8×10 -6 mol of nickel naphthenate and 5.9×10 -5 mol of the aging solution of triisobutylaluminum, and then add 2.0×10 -5 mol of boron trifluoride complexes, the reaction was terminated after 18 hours of polymerization. Conversion rate is 20%, and the [η] of polybutadiene product is 4.32dL / g, and gel can't be detected, M w 7.4×10 5 g / mol, M w / M n 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 catalyze the 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-content of 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 kettle and pipes and convenient operation.

Description

Technical field: [0001] The invention relates to a catalyst system and a method for preparing high cis-polybutadiene through butadiene polymerization using the catalyst system. Background technique: [0002] As an important supporting industry and an internationally recognized strategic material, automobile 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 in the automotive tire industry. Rubber includes natural rubber and synthetic rubber. At present, natural rubber is used together with butadiene rubber and styrene-butadiene rubber to prepare 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 type of rubber after styrene-butadiene rubber in the world, accounting for about 20% of the world's total synth...

Claims

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Application Information

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Patent Type & Authority Applications(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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