Method for preparing branched high vinyl polybutadiene rubber using molybdenum series catalysis

A technology for branching high-vinyl polybutadiene and high-vinyl polybutadiene, which is applied in the field of molybdenum-based catalyzed preparation of branched high-vinyl polybutadiene rubber, which can solve branching tunability and physical and mechanical problems. Unsatisfactory performance, etc.

Inactive Publication Date: 2006-12-27
QINGDAO UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This reflects that the branching modification of rubber is a hot spot in the development of new rubber varieties, but its branching adjustability and physical and mechanical properties are still unsatisfactory.

Method used

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  • Method for preparing branched high vinyl polybutadiene rubber using molybdenum series catalysis
  • Method for preparing branched high vinyl polybutadiene rubber using molybdenum series catalysis

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] Add the hydrogenated gasoline solution of butadiene into the stirred reactor that has been evacuated and filled with nitrogen, and then add stoichiometric benzyl chloride and PPh sequentially with a syringe. 3 Toluene solution, MoCl 3 (OC 8 h 17 ) 2 , m-cresol substituted triisobutylaluminum Al(OPhCH 3 )(i-Bu) 2 . Heating with an oil bath, the constant temperature is T=90°C, the reaction time is 8h, the reaction is terminated with ethanol, the polymer is precipitated, washed and dried. Among them, Al / Mo=30, Mo / Bd=2×10 -4 , benzyl chloride / PPh 3 / Bd=1 / 3 / 2000 (molar ratio).

[0045] aggregation method

C％

M n ×10 4

M w ×10 4

DPI

Gel(%)

P

P+A

100

83.4

19.6

9.3

37.1

24.1

1.9

2.6

0

1.36

[0046] P: coordination polymerization; A: ATRP; P+A: coordination polymerization and ATRP in situ polymerization.

[0047] Coordination polymerization conditions: Al / Mo=60, Mo / ...

Embodiment 2

[0050] Add the hydrogenated gasoline solution of butadiene into the stirred reactor that has been evacuated and filled with nitrogen, and then add the stoichiometric amount of benzyl chloride as the initiator, octanol disubstituted MoCl 5 As a catalyst, triphenylphosphine was used as a ligand to initiate butadiene, reacted at 110 ° C for 40 h, and then sequentially added stoichiometric hydrogenated gasoline solution with additional monomer butadiene and Al(OPhCH 3 )(i-Bu) 2 、MoCl 3 (OC 8 h 17 ) 2 The GPC molecular weight distribution curve of the product obtained by the coordination polymerization of butadiene and the PB obtained by the direct coordination polymerization of butadiene under the same conditions is compared and analyzed as attached figure 2 .

Embodiment 3

[0052] In toluene solution at 110°C, using benzyl chloride as the initiator, octanol disubstituted MoCl 5 As a catalyst, triphenylphosphine was used as a ligand to initiate the ATRP reaction of butadiene for 20 hours, and the conversion rate was 20%, Mn=1.19×10 4 , Mw / Mn=1.73 macromolecule glue polybutadiene macromonomer. Add the hydrogenated gasoline solution of butadiene in the stirred 3-liter polymerizer that has been evacuated and filled with nitrogen, and then add the stoichiometric medium with a syringe. Use this macromolecular glue as a macromolecular monomer, Al(OPhCH 3 )(i-Bu) 2 、MoCl 3 (OC 8 h 17 ) 2 Initiate the coordination polymerization of butadiene. The effects of different amounts of macromolecular glue on monomer conversion rate, polymer viscosity-average molecular weight, molecular weight distribution, 1,2 structure content, gel content and physical and mechanical properties of vulcanized rubber are listed in Table 1.

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PUM

PropertyMeasurementUnit
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Abstract

The invention relates to a method for preparing branched high ethenyl butadiene rubber with molybdenum catalyst, recombining macromolecular monomer prepared through polymerization of molybdenum catalyst butadiene atom free radical or butadiene anion initiated by organic lithium, naphthalene sodium, with coordinate polymerization of butadiene or original position polymerization, to prepare said product with controllable construction. The method is characterized by simple process, special construction of polymer, proper molecular weight and molecular distribution, more than 80% of ethenyl content, controllable property, length, distribution and degree of branching of branch chain in a certain range, good processing behavior and physical mechanics property and low production cost.

Description

technical field [0001] The invention relates to the field of synthetic rubber, in particular to a method for preparing branched high-vinyl polybutadiene rubber by molybdenum-based catalysis. Background technique [0002] With the development of the automobile industry, the requirements for various performances of tires are developing towards high performance and serialization, especially for passenger tire treads, which require both low rolling resistance (combustion consumption) and good moisture resistance Slippery performance (driving safety). High vinyl polybutadiene (polybutadiene with a vinyl content above 65% is called high 1,2 polybutadiene) rubber (HVPBR) has the advantages of excellent wet skid resistance, low heat generation, and aging resistance. , and the blended rubber with natural rubber has both the advantages of natural rubber and styrene-butadiene rubber, showing good comprehensive performance, which can partially replace SBR and improve the defects of BR ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F279/02C08F36/06C08F4/602
Inventor 华静徐玲杨海强李欣仲崇祺
Owner QINGDAO UNIV OF SCI & TECH
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