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A kind of rare earth isoprene rubber catalyst process method

A rare earth isoprene rubber and process method technology, applied in the field of synthetic rubber, can solve the problems of unstable quality of isoprene rubber products, difficult control of the reaction temperature and pressure of the first reaction kettle, blockage of the rubber conveying pipeline, and the like, so as to omit the catalyst The effect of preparation steps, saving equipment investment and stable product quality

Active Publication Date: 2018-07-13
PETROCHINA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

According to the current research results, the quality of the catalyst is seriously affected by factors such as the preparation environment temperature and aging time.
At the same time, due to the high activity of the catalyst, it is not easy to control the reaction temperature and pressure of the first reactor, and the rubber pipeline is blocked, which leads to a series of subsequent engineering control problems.
The direct consequence of these factors is the unstable quality of isoprene rubber products

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043]Under the protection of nitrogen, 562g of hexane and 102g of isoprene were added to a 2L reactor. After stirring and mixing evenly, 1.9 mL (0.1467 mol / L) neodymium neodecanoate hexane solution and 2.6 mL (1.865 mol / L) isobutylaluminum hexane solution were added. After stirring for 20 minutes and preheating to 40°C, add 2mL (0.4096mol / L) diisobutylaluminum hexane solution to initiate the polymerization reaction. The polymerization reaction temperature is controlled between 40°C-50°C and the reaction pressure is 0.2Mpa. After 3.5 hours of reaction, ethanol was added to terminate the reaction, and the yield was 78%.

[0044] Product structure analysis: cis-1,4-polyisoprene content mass percentage is 96.3%, 3,4-polyisoprene content mass percentage is 3.7%; weight average molecular weight is 88×10 4 , the molecular weight distribution is 2.4, and the Mooney viscosity is 90.

Embodiment 2

[0046] Under the protection of nitrogen, 562g of hexane and 102g of isoprene were added to a 2L reactor. After stirring and mixing evenly, add 1.9mL (0.1467mol / L) neodymium neodecanoate hexane solution and 2.6mL (1.865mol / L) isobutylaluminum and diisobutylaluminum hydride 1:1 hexane solution. After stirring for 30 minutes and preheating to 40°C, add 2mL (0.4096mol / L) diisobutylaluminum hexane solution to initiate the polymerization reaction. The polymerization reaction temperature is controlled between 60°C and 70°C, and the reaction pressure is 0.2MPa. After 3 hours of reaction, ethanol was added to terminate the reaction, and the yield was 72%.

[0047] Product structure analysis: cis-1,4-polyisoprene content mass percentage is 96.1%, 3,4-polyisoprene content mass percentage is 3.9%; weight average molecular weight is 52×10 4 , molecular weight distribution is 2.6, Mooney viscosity is 60.

Embodiment 3

[0049] Under the protection of nitrogen, 562g of hexane and 102g of isoprene were added to a 2L reactor. After stirring and mixing evenly, add 1.9mL (0.1467mol / L) neodymium naphthenate hexane solution and 2.6mL (1.865mol / L) 1:1 hexane solution of isobutylaluminum and diisobutylaluminum hydride. After stirring for 10 minutes and preheating to 30°C, add 2mL (0.4096mol / L) diisobutylaluminum hexane solution to initiate the polymerization reaction. The polymerization reaction temperature is controlled between 60°C-70°C, and the reaction pressure is 0.. 15MPa. After 3 hours of reaction, ethanol was added to terminate the reaction, and the yield was 72%.

[0050] Product structure analysis: cis-1,4-polyisoprene content mass percentage is 96.6%, 3,4-polyisoprene content mass percentage is 3.4%; weight average molecular weight is 55×10 4 , the molecular weight distribution is 3.0, and the Mooney viscosity is 63.

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Abstract

A rare earth isoprene rubber catalyst process method, under the protection of nitrogen, isoprene and hexane are added into the reaction kettle according to a certain mass ratio, and a certain amount of catalyst A and catalyst B are added after preheating, and the amount of catalyst A is represented by Nd Calculated, the molar ratio of Nd / isoprene monomer is 3.0×10-5-5.0×10-3, and the molar ratio of catalyst A to catalyst B is 1:10-30; after mixing, add a certain amount of catalyst C to initiate polymerization Reaction, the molar ratio of catalyst A and catalyst C is 1:1-5, at 40°C-70°C, 0MPa-0.4MPa, continue to react for 3-5 hours, and the product rare earth isoprene rubber is obtained through condensation; the catalyst A It is rare earth neodymium organic compound; catalyst B is alkyl aluminum; catalyst C is chloride.

Description

technical field [0001] The invention relates to the field of synthetic rubber, in particular to a rare earth isoprene rubber catalyst process method. Background technique [0002] Isoprene rubber is a high-cis (cis-1,4 content of 95% to 98%) synthetic rubber made from isoprene. Its structure and properties are similar to natural rubber. It is also called synthetic natural rubber. Instead of natural rubber, it is used in tire manufacturing and medical fields. At present, the production capacity of isoprene rubber in the world reaches about 624,000 tons per year, accounting for 5% of the production capacity of synthetic rubber (SR) in the world. Titanium catalyst system isoprene rubber production technology is currently the most mature isoprene rubber production technology with the largest production capacity in the world. The output of titanium-based isoprene rubber accounts for more than 95% of the world's total isoprene rubber production. The rare earth isoprene rubber pr...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F136/08C08F4/52
Inventor 侯军王硕郭睿达刘乃青张桂荣孙继德王刚王松芝
Owner PETROCHINA CO LTD