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Highly-active high vinyl butadiene rubber catalyst as well as preparation and application thereof

A high vinyl butadiene, high activity technology, applied in the field of polymer synthesis, can solve the problems of easy heterogeneity, affecting catalyst activity pipeline transportation, Mooney appreciation and other problems, achieving high catalytic activity and small performance change rate , Mooney viscosity and low density effect

Inactive Publication Date: 2017-05-24
CHINA PETROLEUM & CHEM CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, during the storage of the polymerization product and the coagulation and drying of the rubber, there will be a phenomenon of Mooney appreciation.
At present, Qilu Petrochemical uses oxygen-containing phenolic compounds to react with Mo compounds to prepare the main catalyst, which improves the Mooney appreciation phenomenon and improves the thermal stability of the polymer. However, the above Mo-based main catalysts are prone to unevenness during the configuration and placement process. phase, which affects the activity of the catalyst and its transport in the pipeline

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Embodiments 1 to 9 are specific embodiments of a high-activity high-vinyl butadiene rubber catalyst of the present invention and its preparation and application. Wherein embodiment 1 is the best embodiment. Comparative examples 1 to 4 are comparative examples designed by the applicant.

[0024] Example 1

[0025] The preparation method of catalyst is as follows:

[0026] Preparation of the main catalyst: under the protection of nitrogen, add 0.24g molybdenum pentachloride, 2,2'-methylene bis(4-methyl 6-tert-butyl phenol) 0.3ml, isopropanol 0.1ml, and n-hexane solution, stirred and mixed; after mixing, reacted at room temperature for 48 hours, and the resulting mixture was the main catalyst; wherein, molybdenum pentachloride, 2,2' -Methylene bis(4-methyl 6-tert-butylphenol) and isopropanol are added in a molar ratio of 1:(1~6):0.3;

[0027] Preparation of co-catalyst: under the protection of nitrogen, 15.0 ml cresol and 45.0 g triisobutylaluminum were added to the ...

Embodiment 2

[0029] The preparation method of catalyst is as follows:

[0030] Preparation of the main catalyst: under the protection of nitrogen, add 0.23g molybdenum pentachloride, 2,2'-methylene bis(4-methyl 6-tert-butyl phenol) 0.50ml, isopropanol 0.3ml, and n-hexane solution, stirred and mixed; after mixing, reacted at room temperature for 48 hours, and the resulting mixture was the main catalyst; wherein, molybdenum pentachloride, 2,2' -Methylene bis(4-methyl 6-tert-butylphenol) and isopropanol are added in a molar ratio of 1:(1~6):0.6;

[0031] The preparation of co-catalyst is the same as in Example 1.

Embodiment 3

[0033] The preparation method of catalyst is as follows:

[0034] Preparation of the main catalyst: under the protection of nitrogen, add 0.25g molybdenum pentachloride, 2,2'-methylene bis(4-methyl 6-tert-butyl base phenol) 1.2ml, isopropanol 0.8ml, and n-hexane solution, stirred and mixed; reacted at room temperature for 48 hours after mixing, and the resulting mixture was the main catalyst; wherein molybdenum pentachloride, 2,2' -Methylene bis(4-methyl 6-tert-butylphenol) and isopropanol are added in a molar ratio of 1:(1~6):0.9;

[0035] The preparation of co-catalyst is the same as in Example 1.

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PUM

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Abstract

The invention discloses a highly-active high vinyl butadiene rubber catalyst, as well as a preparation and application of the highly-active high vinyl butadiene rubber catalyst, and belongs to technical field of high polymer synthesis. The highly-active high vinyl butadiene rubber catalyst comprises a main catalyst and a cocatalyst; the main catalyst is a mixture obtained by mixing and reacting molybdenum chloride or / and a molybdenum oxide, an anti-oxidant with an antioxidant function, a compound with active hydrogen and a solvent oil at room temperature; the molybdenum chloride or / and molybdenum oxide, the anti-oxidant with the antioxidant function and the compound with the active hydrogen are added in a molar ratio of 1:(0.5-10):(0.3-5); the compound with the active hydrogen is one or a mixture selected from the group of alcohol ROH, water and carboxylic acid RCOOH; the cocatalyst is a product obtained by a reaction of cresol or m-cresol and an organic aluminum compound in a molar ratio of (1-6):1 at the room temperature. The highly-active high vinyl butadiene rubber catalyst disclosed by the invention has relatively high polymerization activity, and further improves physical and mechanical properties of aging resistance and the like of butadiene rubber.

Description

technical field [0001] The invention belongs to the technical field of high polymer synthesis, and in particular relates to a high-activity high-vinyl butadiene rubber catalyst and its preparation and application. Background technique [0002] High-vinyl polybutadiene is one of the main varieties of polybutadiene rubber. Its molecular chain structure contains vinyl side chains. By adjusting the content of vinyl groups, molecular design can be realized, and polymers with good comprehensive properties can be obtained. Random medium and high vinyl polybutadiene can be used as rubber material. Molybdenum-based catalysts are one of the main coordination catalysts for the synthesis of high-vinyl butadiene rubber. The 1,2-structure content of polybutadiene produced by such catalysts can reach more than 80%, which belongs to high-vinyl polybutadiene. Butadiene, no need to add structure regulator, 1,2-structure presents random distribution, no gel. [0003] The research on the synt...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F136/06C08F4/69C08L9/00
Inventor 艾学芹华静焦胜成贾凤玲耿洁婷庞先明李迎赵吉红徐玲刘金慧
Owner CHINA PETROLEUM & CHEM CORP
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