Unlock instant, AI-driven research and patent intelligence for your innovation.

Production method of thermostable high-vinyl butadiene rubber

A high-vinyl butadiene, heat-stabilized technology, applied in the field of high polymer synthesis, can solve the problems of high viscosity of glue and difficulty in dispersing rubber, etc., to improve anti-aging effect, reduce Mooney appreciation, and gel content little effect

Active Publication Date: 2017-01-11
CHINA PETROLEUM & CHEM CORP
View PDF4 Cites 5 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In addition, due to the high viscosity of the glue after the polymerization, the added terminators and anti-aging agents are generally polar, making it difficult for them to disperse into the rubber

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] 1. Preparation of molybdenum catalyst

[0022] For the preparation of the main catalyst, under the protection of nitrogen, add a certain amount of molybdenum pentachloride and oxygen-containing phenol ligand 1076 (β-( 3,5-di-tert-butyl-4 hydroxyphenyl)propionic acid n-octadecyl alcohol ester) (the molar ratio of 1076 to Mo is 3:1), n-hexane solution, and the catalyst reacted at room temperature for 12 hours.

[0023] Under the protection of nitrogen, for the preparation of co-catalyst, cresol and triisobutyl aluminum were reacted for 6 hours at a molar ratio of 2:1.

[0024] 2. Preparation of high vinyl polybutadiene

[0025] The experiment was carried out in a sealed 30 ml polymerization tube. Bake the polymerization tube in a heating mantle at 120℃ for 2h, and replace it with nitrogen several times. Add butadiene n-hexane solution in sequence, the concentration is 0.14g / mL, the cresol-substituted triisobutylaluminum is 4.66× 10 -4 mol, oxygen-containing phenolic ligand 10...

example 1

[0032] Instance 10~14 , The molar ratio of cresol to triisobutyl aluminum in the co-catalyst is 6:1, the amount of molybdenum trichloride substituted by the main catalyst 1076 is shown in Table 3, and the others are the same as in Example 1.

[0033] Table Three

[0034] .

[0035] Bd is butadiene monomer

Embodiment 15

[0037] 1. Preparation of molybdenum catalyst

[0038] For the preparation of the main catalyst, under the protection of nitrogen, in the reaction flask after deoxygenation and water removal treatment, add molybdenum dichloride, oxygen-containing phenol ligand 2246 (2,2'-methylene bis (4 -Methyl 6-tert-butylphenol)) (2246 / Mo molar ratio is 3), n-hexane solution, and the catalyst reacts at room temperature for 24 hours.

[0039] For the preparation of the co-catalyst, m-cresol and tri-n-butyl aluminum were reacted for 6 hours at a molar ratio of 1:1.

[0040] 2. Preparation of high vinyl polybutadiene

[0041] The experiment was performed in a 30 ml polymer tube sealed with a rubber stopper. Bake the polymerization tube in a heating mantle at 120℃ for 2h, and replace it with nitrogen several times. Add butadiene n-hexane solution successively, the concentration is 0.14g / mL, and the triisobutylaluminum substituted by cresol is 3.12× 10 -4 mol, oxygen-containing phenolic ligand 2246 s...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

No PUM Login to View More

Abstract

A production method of thermostable high-vinyl butadiene rubber comprises the following steps: adding an n-hexane polymerization solution of a butadiene monomer into a waterless oxygen-free polymerization tank under the protection of nitrogen, sequentially adding an oxygen-containing ligand Mo system main catalyst and an aluminum alkyl cocatalyst according to a molar ratio of the oxygen-containing ligand Mo system main catalyst to the butadiene monomer of (0.2-10)*10<-4>:1 and a molar ratio of the aluminum alkyl cocatalyst to the oxygen-containing ligand Mo system main catalyst of (5-40):1, and carrying out a polymerization reaction at 30-80 DEG C for 3-10 h; and terminating the polymerization reaction by anhydrous ethanol after the reaction ends. A catalysis system formed by blending the oxygen-containing ligand Mo system main catalyst with the aluminum alkyl cocatalyst allows the 1,2 structure content of polybutadiene to be 80% or above, the gel content of a polymerization content to be small and be 0.1% or less, and reduces the Mooney increase phenomenon in the post-treatment process of raw rubber.

Description

Technical field [0001] A method for preparing thermally stable high vinyl butadiene rubber belongs to the technical field of polymer synthesis. Background technique [0002] 1,2-Polybutadiene is one of the main varieties of butadiene rubber. Its molecular chain structure contains vinyl side chains. By adjusting the content of vinyl groups, molecular design can be achieved and a polymer with good comprehensive properties can be obtained. Random medium and high vinyl 1,2-polybutadiene (1,2-PB) can be used as rubber materials. Molybdenum-based catalysts are one of the main coordination catalysts for the synthesis of high vinyl 1,2-PB rubber. The 1,2-structure content of polybutadiene prepared by this type of catalyst can reach more than 80%, which is high ethylene -Based polybutadiene, no need to add structure modifier, 1,2-structure presents random distribution, no gel. [0003] The research on the synthesis of 1,2-PB with molybdenum catalysts began at the same time that Ziegler-Na...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
IPC IPC(8): C08F136/06C08F4/69
Inventor 耿洁婷华静李迎徐玲艾学芹焦胜成史先鑫赵吉红贾凤玲庞先明
Owner CHINA PETROLEUM & CHEM CORP