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Nitrogen-containing functional rare-earth isoprene rubber and preparation method thereof

A rare earth isoprene rubber, functionalization technology, applied in the field of polymer materials, can solve the problem of low polymerization activity

Active Publication Date: 2013-02-27
DALIAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] As mentioned above, functionalized polymers in the chain have been mainly prepared by living anionic polymerization. Since the rare earth catalyst system usually used for the synthesis of rare earth isoprene rubber has relatively low polymerization activity compared with styrene monomer, the rare earth based There is no report on the catalytic system and the preparation of functionalized rare earth isoprene rubber with styrene derivatives as functionalized comonomers

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] At room temperature, sequentially add 0.5mL NdV to the 20mL catalyst reactor 3 (0.167mol / L n-hexane solution), 1.3mL TIBA (25% n-hexane solution), 0.08mL isoprene, react at 30°C for 10min, then add 0.36mL CHCl 3 (0.68mol / L cyclohexane solution) for 40min, shake to mix evenly.

[0021] Using cyclohexane as the solvent, the monomer concentration is 39g / 100mL, add 2.3g of isoprene and 3.9g of p-N,N-dimethylaminostyrene into a 60mL polymerization reactor according to the ratio; take 1.0mL Aged catalyst (Nd / monomer molar ratio is 5.0×10 -4) into the polymerization bottle. Shake to make it evenly mixed, and react at 70°C for 6h. The reaction was terminated with an ethanol solution containing 1% 2,6-di-tert-butyl-p-methylphenol, and the polymer was precipitated in excess ethanol. After being washed with ethanol and extruded, it was vacuum-dried at 40°C for 24 hours.

[0022] The product structure analysis results are as follows: the content of p-N,N-dimethylaminostyrene is...

Embodiment 2

[0024] At room temperature, sequentially add 1.0mL NdV to the 20mL catalyst reactor 3 (0.167mol / L n-hexane solution), 2.5mL DIBAH (1.0mol / L n-hexane solution), 0.16mL isoprene, react at 10°C for 10min, then add 0.73mL CHCl 3 (0.68mol / L cyclohexane solution) for 40min, shake to mix evenly.

[0025] Using cyclohexane as the solvent, the monomer concentration is 39g / 100mL, add 4.6g of isoprene and 7.8g of p-N,N-dimethylaminostyrene into a 60mL polymerization reactor according to the ratio; take 1.9mL Aged catalyst (Nd / monomer molar ratio is 5.0×10 -4 ) into the polymerization bottle. Shake to make it evenly mixed, and react at 70°C for 12h. The reaction was terminated with an ethanol solution containing 1% 2,6-di-tert-butyl-p-methylphenol, and the polymer was precipitated in excess ethanol. After being washed with ethanol and extruded, it was vacuum-dried at 40°C for 24 hours.

[0026] The product structure analysis results are as follows: the content of p-N,N-dimethylaminost...

Embodiment 3

[0028] At room temperature, sequentially add 1.0mL NdV to the 20mL catalyst reactor 3 (0.167mol / L n-hexane solution), 0.8mL DIBAH (1.0mol / L n-hexane solution), 0.19mL piperylene, react at 30°C for 10min, then add 0.73mL CHCl 3 (0.68mol / L cyclohexane solution) for 40min, shake to mix evenly.

[0029] Using cyclohexane as the solvent, the monomer concentration is 21g / 100mL, add 4.1g of isoprene and 6.9g of p-N,N-diethylaminostyrene into a 60mL polymerization reactor according to the ratio; take 0.6mL Aged catalyst (Nd / monomer molar ratio is 3.0×10 -4 ) into the polymerization bottle. Shake to make it evenly mixed, and react at 50°C for 12h. The reaction was terminated with an ethanol solution containing 1% 2,6-di-tert-butyl-p-methylphenol, and the polymer was precipitated in excess ethanol. After being washed with ethanol and extruded, it was vacuum-dried at 40°C for 24 hours.

[0030] The product structure analysis results are as follows: the content of p-N,N-diethylaminost...

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Abstract

The invention discloses a rare earth catalyst system, i.e., nitrogen-containing functional rare-earth isoprene rubber, characterized in that: the weight-average molecular weight is 1*10<4>-120*10<4>; measured as 100% of total amount of polymer, the mass percentage of combined styrene derivative is 1-50%, and the mass percentage of isoprene is 50-99%; measured as 100% of total amount of polyisoprene, the mass percentage of 1,4-polyisoprene is 70-98%; the styrene derivative is selected from nitrogen atom-substituted styrene and at least comprises a tertiary amine group substituent; the substituent can be directly conjugated to the ortho-position, the meta-position or para-position of styrene, and can be conjugated to the alkyl group at the ortho-position, the meta-position or para-position of styrene; and the styrene derivative can comprise mono substituent, dual substituents or three substituents, wherein the substituents can be same or different.

Description

technical field [0001] The invention belongs to the technical field of polymer materials, and relates to a kind of nitrogen-containing functionalized rare earth isoprene rubber based on a rare earth catalytic system and a preparation method thereof. Background technique [0002] Polymer functionalization has become an important way to achieve high-performance polymer materials. The functionalization of polymer materials based on living anionic polymerization has developed from terminal functionalization to chain functionalization. Chain-functionalized synthetic rubber has become a new generation of functional synthetic rubber, and functionalized polymers have developed from the realization of chain-end functionalization to the regulation of chain-functionalization. At present, the research on the synthesis method of terminal-functionalized polymers has become mature, but due to the limited number of polymer terminal groups, the structure and performance of functionalized pol...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F236/10C08F236/08C08F212/14C08F4/54C08F4/52
Inventor 李杨史正海许蔷申凯华郭芳王玉荣王艳色
Owner DALIAN UNIV OF TECH
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