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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: 2016-08-17
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 nitrogen protection, 562g of hexane and 102g of isoprene were added to the 2L reactor. After stirring and mixing uniformly, 1.9 mL (0.1467 mol / L) of neodymium neodecanoate hexane solution and 2.6 mL (1.865 mol / L) isobutyl aluminum hexane solution were added. After stirring for 20min and preheating to 40°C, 2mL (0.4096mol / L) monochlorodiisobutylaluminum hexane solution was added to initiate the polymerization reaction. The polymerization reaction temperature was controlled between 40°C and 50°C, and the reaction pressure was 0.2Mpa. After 3.5 hours of reaction, ethanol was added to terminate the reaction, and the yield was 78%.

[0044] Product structure analysis: the mass percentage of cis-1,4-polyisoprene content is 96.3%, the mass percentage of 3,4-polyisoprene content is 3.7%; the 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 nitrogen protection, 562g of hexane and 102g of isoprene were added to the 2L reactor. After stirring and mixing uniformly, 1.9 mL (0.1467 mol / L) of neodymium neodecanoate in hexane solution and 2.6 mL (1.865 mol / L) of isobutylaluminum and diisobutylaluminum hydride 1:1 hexane solution were added. After stirring for 30 min and preheating to 40 °C, 2 mL (0.4096 mol / L) monochlorodiisobutylaluminum hexane solution was added to initiate the polymerization reaction. The polymerization reaction temperature was controlled between 60 °C and 70 °C, and the reaction pressure was 0.2 MPa. After 3 hours of reaction, ethanol was added to terminate the reaction, and the yield was 72%.

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

Embodiment 3

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

[0050] Product structure analysis: the mass percentage of cis-1,4-polyisoprene content is 96.6%, the mass percentage of 3,4-polyisoprene content is 3.4%; the 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 comprises the steps: under the protection of nitrogen, adding isoprene and hexane into a reaction kettle according to a certain mass ratio, preheating, and then adding a certain amount of a catalyst A and a certain amount of a catalyst B, wherein the amount of the catalyst A is calculated according to Nd, the molar ratio of Nd to the isoprene monomer is 3.0*10<-5>-5.0*10<-3>, and the molar ratio of the catalyst A to the catalyst B is 1 to (10-30); and after mixing, adding a certain amount of a catalyst C, triggering a polymerization reaction with the molar ratio of the catalyst A to the catalyst C of 1 to (1-5), at the temperature of 40 DEG C-70 DEG C and at the pressure of 0 MPa-0.4 MPa, continuing to carry out a reaction for 3-5 hours, and carrying out condensation to obtain the product rare earth isoprene rubber. The catalyst A is a rare earth neodymium organic compound; the catalyst B is alkyl aluminum; the catalyst C is a 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. Replacing natural rubber for tire manufacturing and medicine. At present, the world's isoprene rubber production capacity is about 624,000 tons / year, which is 5% of the world's synthetic rubber (SR) production capacity. Titanium catalytic system isoprene rubber production technology is currently the most mature isoprene rubber production technology in the world with the largest production capacity. The content is higher, the material requirements for equipment are high, the three wastes treatment method is complicated and the processing capacity is large, while the rare earth isoprene rubber produ...

Claims

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Application Information

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Patent Type & Authority Applications(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