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Preparation method for preparing catalyst of rare earth butadiene rubber

A rare earth cis-butadiene and catalyst technology is applied in the field of catalysts for preparing cis-butadiene rubber to achieve the effects of good effect, good fluidity and high activity

Active Publication Date: 2017-12-29
PETROCHINA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] So far, the report on high Mooney rubber is that the patent of Sinopec Qilu Co., Ltd. with application number 200310114681.6 mentions the production process of nickel-based butadiene rubber with a Mooney viscosity of 25-100. The main catalyst mentioned in this process is Nickel, the product is nickel-based butadiene rubber, which is different from the rare earth butadiene rubber of this project; the U.S. patent with publication number US5616653 (A) mentions Mooney viscosity of 70-120 styrene-isoprene-butadiene coupling rubber The preparation method, the polymerization monomer used in this method is styrene-isoprene-butadiene, which is different from this project; for narrow molecular weight distribution (1.3~2.5) high Mooney (Mooney viscosity 55-100) Rare earth butadiene rubber technology research reports, no similar literature at home and abroad described

Method used

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  • Preparation method for preparing catalyst of rare earth butadiene rubber
  • Preparation method for preparing catalyst of rare earth butadiene rubber
  • Preparation method for preparing catalyst of rare earth butadiene rubber

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Catalysts for the preparation of rare earth butadiene rubber include neodymium phosphate (where the phosphate is bis(2-ethylhexyl) phosphate), diisobutylaluminum hydride and monochloro / dichloroethylaluminum, butadiene, molecular weight regulator Triisobutylaluminum (the ratio to diisobutylaluminum hydride is triisobutylaluminum / diisobutylaluminum hydride 50:1).

[0025] The mol ratio of described diisobutyl aluminum hydride and neodymium phosphate is 5:1; The mol ratio of monochloro / dichloroethylaluminum and neodymium phosphate is 2:1, the mol ratio of butadiene and neodymium phosphate is 2: 1.

[0026] The preparation method of the catalyst is as follows: under the protection of nitrogen, add neodymium phosphate 3.46×10 -4 mol, butadiene 6.92×10 -4 mol, diisobutylaluminum hydride 1.73×10 -3 mol, aged at 0°C for 30 minutes, then added monochloro / dichloroethylaluminum 6.92×10 -4 mol, aged at 0°C for 20 minutes, after forming a homogeneous transparent solution, add tr...

Embodiment 2

[0028] The catalysts for the preparation of rare earth butadiene rubber include neodymium phosphate (where the phosphate is 2-ethylhexyl phosphate), diisobutyl aluminum hydride and monochloro / dichloroethyl aluminum, butadiene, molecular weight Regulator triisobutylaluminum (the ratio to diisobutylaluminum hydride is triisobutylaluminum / diisobutylaluminum hydride 50:50). The mol ratio of described diisobutyl aluminum hydride and neodymium phosphate is 15:1; :1.

[0029] The preparation method of the catalyst is as follows: under the protection of nitrogen, add neodymium phosphate 3.46×10 -4 mol, butadiene 4.15×10 -3 mol, diisobutylaluminum hydride 5.19×10 -3 mol, aged at 30°C for 20 minutes, then added monochloro / dichloroethylaluminum 1.21×10 -3 mol, aged at 30°C for 10 minutes, after forming a homogeneous transparent solution, add triisobutylaluminum 5.19×10 -3 mol, aged at 30°C for 10 minutes to prepare a concentration of 2.5×10 -5 mol / ml of Catalyst B.

Embodiment 3

[0031] The catalysts for the preparation of rare earth butadiene rubber include neodymium phosphate (wherein the phosphoric acid ester is dimethylheptyl aluminum methyl phosphate), diisobutyl aluminum hydride and monochloro / dichloroethyl aluminum, butadiene, molecular weight regulator Triisobutylaluminum (the ratio to diisobutylaluminum hydride is triisobutylaluminum / diisobutylaluminum hydride 99:1). The mol ratio of described diisobutyl aluminum hydride and neodymium phosphate is 25:1; :1.

[0032] The preparation method of the catalyst is as follows: under the protection of nitrogen, add neodymium phosphate 3.46×10 -4 mol, butadiene 6.92×10 -3 mol, diisobutylaluminum hydride 8.65×10 -2 mol, aged at 60°C for 10 minutes, then added monochloro / dichloroethylaluminum 1.73×10 -4mol, aged at 60°C for 5 minutes to form a homogeneous transparent solution, then added 8.56mol of triisobutylaluminum, aged at 60°C for 30 minutes, and prepared a concentration of 5×10 -5 mol / ml of Cat...

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Abstract

The invention relates to a preparation method for preparing a catalyst of rare earth butadiene rubber. The preparation method comprises the following steps: under nitrogen protection, successively adding a solution of a phosphoric acid rare earth compound, alkadiene and hydrogenated aluminum alkyl into a catalyst ageing bottle which is dried; ageing the mixture for 10-30min at 0-60 DEG C; then adding an organic chloride; ageing the mixture for 5-20min at 0-60 DEG C to from a homogeneous transparent solution; and then adding aluminum alkyl to age for 1-30min at 0-60 DEG C to prepare the catalyst of rare earth butadiene rubber. The catalyst is used for evaluating activity of butadiene polymerization. The monomer conversion rate is greater than or equal to 90%, the Mooney point of a product is 55-100, the number-average molecular weight is greater than or equal to 180 thousand and the molecular weight distribution is 1.3-2.5.

Description

technical field [0001] The invention relates to the field of a catalyst for preparing butadiene rubber, in particular to a preparation method for a catalyst for preparing rare earth butadiene rubber with narrow molecular weight distribution and high Mooney. Background technique [0002] After the implementation of EU tire labeling regulations, high-performance tires and green tires with "high speed, environmental protection, safety and energy saving" have attracted worldwide attention. High-performance tires require rubber raw materials not only to meet the requirements of the tire manufacturing process, but also to meet the requirements of high speed, safety, energy saving and environmental protection. From the analysis of the existing butadiene rubber industrial products, rare earth butadiene rubber is the best rubber to meet the requirements. Rare earth butadiene rubber has the characteristics of high molecular chain structure regularity, low long chain branching degree, ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F136/06C08F4/54
CPCC08F4/545C08F136/06
Inventor 周鹏松张志强张玉东王中平郭中台李潇王晓冰
Owner PETROCHINA CO LTD
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