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A kind of cobalt series catalyst and its application in 1,3-butadiene polymerization reaction

A polymerization reaction and catalyst technology, which is applied to cobalt-based catalysts and its application in 1,3-butadiene polymerization, can solve the problems of polybutadiene molecular weight and molecular weight distribution that are not easy to control, and achieve excellent catalytic performance. Active, low price, low environmental requirements

Active Publication Date: 2016-07-13
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But since these traditional Ziegler-Natta catalysts contain multiple active sites, the molecular weight and molecular weight distribution of the produced polybutadienes (PBDs) are not easy to control

Method used

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  • A kind of cobalt series catalyst and its application in 1,3-butadiene polymerization reaction
  • A kind of cobalt series catalyst and its application in 1,3-butadiene polymerization reaction
  • A kind of cobalt series catalyst and its application in 1,3-butadiene polymerization reaction

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0050] 1. The preparation of 2-(2-nitrophenyl)benzimidazole: Add o-nitrobenzaldehyde (3.045g, 20.1mmol), potassium hydrogen persulfate (3.381g, 11.0mmol), o-benzene Diamine (1.984g, 18.4mmol) and solvent 50ml DMF gave a yellow transparent liquid, and the reaction mixture was stirred at room temperature for 2h. Then add K dropwise 2 CO 3 (1M, 25mL) and distilled water (250mL), a milky white solid precipitated. Then, it was extracted three times with ethyl acetate (3 x 50 mL), and the organic layer was separated. They were then washed once with distilled water and twice with saturated saline. After drying with anhydrous sodium sulfate, filter and remove the solvent to obtain a brown solid crude product, wash it on a silica gel column with chloroform, collect and remove the solvent to obtain a light brown solid, which is 2-(2-nitrophenyl) Benzimidazole (3.266 g), 72.4% yield.

[0051] 1 HNMR (400MHz, CDCl 3 ):δ8.16(dd,J 1 =7.6Hz,J 2 =1.2Hz,1H,Ar-H),7.97(dd,J 1 =7.6Hz,J ...

Embodiment 2

[0063] 1. The preparation of complex 1 is the same as in Example 1.

[0064] 2. Polymerization of butadiene solution: under the protection of nitrogen, take complex 1 (2.2 mg, 5.0 μmol) in a polymerization reaction bottle, seal it with a rubber stopper, vacuumize and vent nitrogen for three times, and add 3.4 ml of purified toluene solvent . Then, add cocatalyst sesquiethylaluminum chloride (EASC, 0.4mol / L normal hexane solution) 1.0ml with syringe, make [Al] / [Co] be 160, this catalyst composition is stirred at 30 ℃ for two Minutes, then add 5.6ml of butadiene solution (1.85mol / L toluene solution) with a syringe, make [BD] / [Co] be 2000 (molar ratio, the same below), and the polymerization reaction starts. Unless otherwise stated, the total volume of the polymerization reaction was controlled at 10 ml by adjusting the amount of solvent toluene. Two hours later, the reaction solution was poured into 200ml of terminator to terminate the polymerization, and the terminator was 5%...

Embodiment 3

[0066] 1. The preparation of complex 1 is the same as in Example 1.

[0067] 2. Polymerization of butadiene solution: under the protection of nitrogen, take complex 1 (2.2 mg, 5.0 μmol) in a polymerization reaction bottle, seal it with a rubber stopper, vacuumize and vent nitrogen for three times, and add 3.9 ml of purified toluene solvent . Then, add cocatalyst sesquiethylaluminum chloride (EASC, 0.4mol / L normal hexane solution) 0.5ml with syringe, make [Al] / [Co] be 80, this catalyst composition is stirred at 30 ℃ for two Minutes, then add 5.6ml of butadiene solution (1.85mol / L toluene solution) with a syringe, make [BD] / [Co] be 2000 (molar ratio, the same below), and the polymerization reaction starts. Unless otherwise stated, the total volume of the polymerization reaction was controlled at 10 ml by adjusting the amount of solvent toluene. Two hours later, the reaction solution was poured into 200ml of terminator to terminate the polymerization, and the terminator was 5% ...

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Abstract

The invention discloses a cobalt-based catalyst and its application in 1,3-butadiene polymerization. The cobalt-based catalyst of the present invention is composed of a main catalyst and a co-catalyst; the molar ratio of the metal aluminum in the co-catalyst to the metal cobalt of the main catalyst is 10-2000:1. The main catalyst is a cobalt complex containing NNO ligand, and the cocatalyst is composed of one or two of aluminoxane and alkyl aluminum chloride compound. The main catalyst and cocatalyst of the cobalt-based catalyst are mixed in a solvent, and after aging for 2-10 minutes, the polymerization reaction can be carried out by adding monomer butadiene; the cobalt-based catalyst of the present invention is used to catalyze 1,3-butadiene olefin polymerization, exhibiting excellent catalytic activity and high product cis-selectivity, and has broad industrial application prospects.

Description

technical field [0001] The invention belongs to the technical field of chemical industry, and relates to a cobalt-based catalyst and its application in 1,3-butadiene polymerization. Background technique [0002] 1,3-butadiene can be polymerized in 1,4-polymerization and 1,2-polymerization. According to different catalyst types and polymerization conditions, cis-1,4 (cis-1,4) and trans - 1,4 (trans-1,4) or 1,2-vinyl (1,2-vinyl) polybutadiene. The difference in microstructure determines that polybutadiene has different properties. Among these different isomers, high-cis 1,4-polybutadiene has become an important industrial product with its excellent rubber properties, that is, butadiene rubber , is the second largest general-purpose synthetic rubber in the world after styrene-butadiene rubber, and is widely used in the production of rubber products such as tires, impact-resistant modifiers, tapes, hoses, and rubber shoes. [0003] So far, industrially synthesized butadiene ru...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F36/06C08F4/70
Inventor 介素云吕帅周勤灼李伯耿
Owner ZHEJIANG UNIV
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