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Neodymium-based homogeneous phase rare earth catalyst and preparation method and application thereof

A rare-earth catalyst and catalyst technology, applied in the field of its preparation, neodymium-based homogeneous rare-earth catalyst, and polyconjugated diene elastomer, can solve the problems of cumbersome preparation process, difficult industrial application, and high catalyst cost, and achieve easy preparation method, The effect of good stability and excellent processability

Active Publication Date: 2012-07-04
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

CN 1484657A and CN 1479754A disclose a catalytic system composed of rare earth phosphate, alkylaluminum, alkylaluminum halide and conjugated diene monomer, which can obtain higher monomer conversion at a lower Al / Nd ratio For example, when the Al / Nd ratio is around 2, the monomer conversion rate can reach 100%, but the heterogeneous characteristics of the catalytic system make it difficult to apply in actual production
CN101260164A discloses a novel rare earth catalytic system composed of a pincer type rare earth complex and an alkyl aluminum two-component, when the Al / Nd ratio is 10, the monomer conversion rate can reach 100%, when the Al / Nd ratio is reduced to 2, a conversion rate of 63% can still be obtained, but the structure of this pincer-type rare earth complex is relatively complex, the preparation process is relatively cumbersome, and the cost of the catalyst is relatively high, making it difficult to further industrialize the application

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] Under the protection of nitrogen, add 8.5kg hexane, 304ml concentration of 0.141mol / L neodecanoate / hexane solution, 127ml isoprene and 277ml concentration of 0.469mol / L monochlorine into the dry aging kettle Diethylaluminum / hexane solution, stir and react at 8°C for 15 minutes, then add 371ml of triisobutylaluminum / hexane solution with a concentration of 1.141mol / L, continue to age for 12 hours, set aside, the catalyst is in a homogeneous state . The catalyst concentration was 3.1×10 -3 mol / L.

[0037] Under the protection of nitrogen, 1800g of hexane, 350g of isoprene and the above-mentioned 200ml catalyst were sequentially added to the polymerization kettle at 5°C, and reacted for 2 hours under stirring, and the polymer solution was released from the kettle and added 2,6-di-tert Butylhydroquinone ethanol solution terminated the reaction. The solvent was evaporated and then dried to obtain 332 g of polyisoprene with a conversion rate of 94.9%. The cis 1,4-structure...

Embodiment 2

[0039] Under the protection of nitrogen, add 6.5kg hexane, 1000ml concentration of 0.0369mol / L neodecanoate / hexane solution, 74ml isoprene and 55ml concentration of 2mol / L monochloride Ethylaluminum / hexane solution, stirred and reacted at 6°C for 17 minutes, then added 577ml of triisobutylaluminum / hexane solution with a concentration of 0.576mol / L, continued to age for 18 hours, set aside, the catalyst was in a homogeneous state. The catalyst concentration was 3.2×10 -3 mol / L.

[0040] Under the protection of nitrogen, 2000g of hexane, 300g of isoprene and the above 207ml of catalyst were successively added to the polymerization kettle at 20°C, and the reaction was carried out under stirring for 2.5 hours, and the polymer solution was released from the kettle and added 2,6-di-tert Butylhydroquinone ethanol solution terminated the reaction. The solvent was evaporated and then dried to obtain 275 g of polyisoprene with a conversion rate of 91.7%. The cis 1,4-structure content...

Embodiment 3

[0042] Under the protection of nitrogen, add 4.0kg hexane, 70ml concentration of 0.508mol / L neodecanoate / hexane solution, 200ml isoprene and 62ml concentration of 2mol / L to the dry aging kettle. Ethylaluminum / hexane solution, stirred and reacted at 10°C for 25 minutes, then added 265ml of triisobutylaluminum / hexane solution with a concentration of 0.741mol / L, continued to age for 48 hours, set aside, the catalyst was in a homogeneous state. The catalyst concentration is 5.4×10 -3 mol / L.

[0043] Under the protection of nitrogen, 1700g of hexane, 360g of isoprene and the above-mentioned 253ml of catalyst were sequentially added to the polymerization kettle at 50°C, and reacted for 3.5 hours under stirring, and the polymer solution was released from the kettle and added 2,6-di-tert Butylhydroquinone ethanol solution terminated the reaction. The solvent was evaporated and then dried to obtain 315 g of polyisoprene with a conversion rate of 87.5%. The cis 1,4-structure content ...

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Abstract

The invention relates to a rare earth catalyst used for conjugation alkadiene polymerization, a preparation method thereof and a method for combining a high cis-form gathering conjugate alkadiene elastic body. The rare earth catalyst is composed of carboxylic acid neodymium, alkyl aluminum, halogen-containing compound and conjugate alkadiene, can be prepared under the condition that the molar ratio of the alkyl aluminum and the carboxylic acid neodymium is smaller than or equal to 10, has relatively higher catalytic activity and enables polymerization conversion rate of the conjugate alkadiene to be larger than 80%. The catalyst has the advantages of homogeneous phase, good stability and high directionality. The catalyst is used for conjugate alkadiene polymerization and can prepare the gathering conjugate alkadiene elastic body with the cis-form structure content larger than 98%.

Description

Technical field: [0001] The invention relates to a rare earth catalyst, in particular to a novel neodymium homogeneous rare earth catalyst, its preparation method and its application. The neodymium-based homogeneous rare-earth catalyst of the invention is especially suitable as a catalyst for the polymerization of conjugated dienes to synthesize polyconjugated diene elastomers with high cis-structure content. Background technique: [0002] Compared with polyconjugated diene elastomers prepared by using rare earth catalysts, their macromolecular chains have higher regularity and perfect The linear structure has excellent raw rubber strength and vulcanized rubber performance, which meets the development needs of high-performance tires in terms of high speed, energy saving, safety, and environmental protection. In the composition of rare earth catalysts, alkylaluminum (including alkylaluminum hydride) is a necessary cocatalyst, and its amount is often measured by the molar rat...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F36/04C08F4/54C08F4/52C08F36/08
Inventor 张杰赵姜维李传清谭金枚杨亮亮欧阳素芳辛益双徐林于国柱梁爱民
Owner CHINA PETROLEUM & CHEM CORP
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