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Preparation method of structure-modified 1,2-polybutadiene rubber

A polybutadiene rubber and structure modifier technology, which is applied in the field of butadiene homopolymer preparation, can solve the problems of widening and reducing the molecular weight distribution, and the molecular weight of phosphorus-containing ligand products has not been seen, and achieve low viscosity , excellent performance

Active Publication Date: 2012-03-14
CHINA PETROLEUM & CHEM CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] So far, there have been no literature reports about phosphorus-containing ligands that can not only improve the polymerization activity of Mo series, but also reduce the molecular weight of the product and broaden the molecular weight distribution.

Method used

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  • Preparation method of structure-modified 1,2-polybutadiene rubber
  • Preparation method of structure-modified 1,2-polybutadiene rubber
  • Preparation method of structure-modified 1,2-polybutadiene rubber

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0067] Add the hydrogenated gasoline solution of butadiene in the stirred reactor that has been evacuated and filled with nitrogen, and then add the stoichiometric structural modifier liquid polybutadiene (molecular weight is 2×10 3 ) TBP substituted MoCl 5 (Mo / TBP=1:2 molar ratio), m-cresol substituted triisobutylaluminum Al(OPhCH 3 )(i-Bu) 2 . Heating in a water bath, the constant temperature is 60°C, the reaction time is 6h, the reaction is terminated with ethanol, the polymer is precipitated, washed and dried. However, Al / Mo=20 (molar ratio). The amount of structural modifier is 3% (mass ratio) of the amount of butadiene monomer.

[0068] Monomer conversion rate, polymer intrinsic viscosity, microstructure content, gel content, etc. are listed in Table 1.

[0069] Table 1 Butadiene monomer conversion rate, polymer structure

[0070] Monomer Conversion % [η] Mη×10 5 Mn×10 5 Mw / Mn l，2％ Transl, 4% Gel% 87.9 4.53 7.38 3.68 2.3...

Embodiment 2

[0075] Add the hydrogenated gasoline solution of butadiene into the stirred reactor that has been evacuated and filled with nitrogen, and then add the polybutadiene of the stoichiometric structure modifier liquid hydroxyl end with a syringe; MoCl 3 (OC8H17) 2 (or TBP substituted MoCl 5 , Mo / TBP=1:2 molar ratio), m-cresol substituted triisobutylaluminum Al(OPhCH3)(i-Bu)2. Heating in a water bath, the constant temperature is 60°C, the reaction time is 6h, the reaction is terminated with ethanol, the polymer is precipitated, washed and dried. Among them, Al / Mo=30, Mo / Bd=4.0×10-4 (molar ratio). The amount of structural modifier is 3% (mass ratio) of the amount of butadiene monomer.

[0076] The monomer conversion, polymer intrinsic viscosity, gel content and microstructure of the two catalysts are listed in Table 2.

[0077] Table 2 Butadiene monomer conversion rate, polymer structure

[0078] sample number Molybdenum catalyst Monomer Conversion % [η] Mn×10 ...

Embodiment 3～ Embodiment 7

[0082] Add PB structural modifiers with different molecular weights of 3% mass of butadiene monomer mass to TBP-substituted MoCl 5 (Mo / TBP=1:2 molar ratio), m-cresol substituted triisobutylaluminum Al(OPhCH 3 )(i-Bu) 2 Catalyzed butadiene monomer polymerization system, where Mo / Bd=2×10 -4; Al / Mo=20; TBP / Mo=2 (the above are molar ratios); [Bd]=0.14g / ml, reacted at 60°C for 6h, and the conversion rate of the obtained product was greater than 95%. The molecular weight of gained polymer and its distribution, gel content and its cyclohexane solution (3g / 100ml) viscosity that measure solution at 25 ± 0.2 ℃ with the rotational viscometer of NXS-11A are as shown in table 3:

[0083] Table 3 Mo-based 1,2-PB molecular weight and its distribution and solution viscosity prepared by structural modifiers with different molecular weights

[0084]

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Abstract

The invention relates to a preparation method of structure-modified 1,2-polybutadiene rubber, belongs to a macromolecular compound obtained by carbon-carbon unsaturated bond reaction, relates to a preparation method of butadiene homopolymers, and is characterized by comprising (1) raw materials used; (2) the preparation method of the structure-modified 1,2-polybutadiene rubber; (3) a preparation method of mixed stock of the structure-modified 1,2-polybutadiene rubber. The invention provides a molybdenum catalyst system which can substantially raise the activity of the catalysis system, reduce the molecular weight of a polymerization product, widen molecular weight distribution and decrease the polymerization glue solution viscosity, and simultaneously also provides a structure modifier for improving cold-flow performance and processability of a polymer and wet traction and aging resistance of vulcanized rubber and greatly increasing the service life of the rubber by generating a branched structure of the polymer, so as to realize the industrial preparation method of the structure-modified 1,2-polybutadiene rubber product by molybdenum catalytic synthesis.

Description

technical field [0001] The invention relates to a method for preparing structurally modified 1,2-polybutadiene rubber, which belongs to polymer compounds obtained by reacting only carbon-carbon unsaturated bonds, and relates to a method for preparing butadiene homopolymer. Background technique [0002] Polybutadiene rubber is the second largest variety after styrene-butadiene rubber in the world's synthetic rubber. There are vinyl side groups on the main chain of 1,2-polybutadiene molecule, which has good wet skid resistance and aging resistance. , low heat generation and other advantages, can be used to make aircraft and car tires. In addition, with the difference in microstructure and relative molecular weight, 1,2-polybutadiene is widely used in many fields such as plastics, coatings, adhesives, functional polymers, etc., and can be used to prepare films, fibers, rubber products and Modifier for rubber products, etc. [0003] Molybdenum catalyst is one of the main coord...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F293/00C08F136/06C08F4/69C08L53/00C08K13/02C08K3/22C08K5/09C08K3/04C08K3/06
Inventor 华静李迎张洪林王晓敏艾学勤徐玲丛悦鑫李正勇耿洁婷仲崇祺邓志峰
Owner CHINA PETROLEUM & CHEM CORP
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