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A kind of high vinyl polybutadiene rubber with adjustable microstructure and preparation method thereof

A technology of polybutadiene and butadiene, which is applied in the field of high vinyl polybutadiene rubber and its preparation, can solve the problems of unadjustable microstructure, reduce the molecular weight of polymerization products, reduce the viscosity of polymerization reaction glue, etc., and achieve broad The effect of market and development prospects, low cost, and good safety

Active Publication Date: 2021-11-16
QINGDAO UNIV OF SCI & TECH
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  • Description
  • Claims
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AI Technical Summary

Problems solved by technology

[0008] In the technology disclosed in China about Mo-catalyzed preparation of high vinyl polybutadiene rubber, the co-catalyst m-cresol is used to replace triisobutyl aluminum, which can effectively reduce the molecular weight of the polymerization product, broaden the molecular weight distribution, and reduce the viscosity of the glue in the polymerization reaction. Viscosity, but the 1,2-structure content of the product is more than 80%, and the microstructure cannot be adjusted

Method used

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  • A kind of high vinyl polybutadiene rubber with adjustable microstructure and preparation method thereof
  • A kind of high vinyl polybutadiene rubber with adjustable microstructure and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Under the protection of nitrogen, add MoCl to the dry catalyst reaction bottle in sequence 5 , octanol and hydrogenated gasoline, of which octanol / MoCl 5 2 / 1, react at 20°C for 48h to obtain the main catalyst MoCl for butadiene polymerization 3 (OC 8 h 17 ) 2 . In a plurality of airtight containers vacuumized and filled with nitrogen, the quantitative MoCl 3 (OC 8 h 17 ) 2 with variable AlEt 3 well mixed.

[0034] Under nitrogen protection, 30 ml of a hydrogenated gasoline solution of butadiene monomer was added to a dry and sealed 50 ml reaction flask, wherein the concentration of butadiene was 1.4 g / 10 ml. Add MoCl 3 (OC 8 h 17 ) 2 with AlEt 3 The reaction liquid, wherein the molar ratio of Mo / Bd is 2×10 -3, the polymerization was carried out at 30 °C. After 6 hours, the polymerization reaction was terminated with an ethanol solution containing 0.02 g / ml anti-aging agent 264, and the ethanol was condensed to obtain polybutadiene. The polybutadiene pr...

Embodiment 2

[0039] Prepare MoCl according to Example 1 3 (OC 8 h 17 ) 2 Catalyst, in a plurality of airtight containers that are evacuated and filled with nitrogen, variable MoCl 3 (OC 8 h 17 ) 2 with quantitative AlEt 3 Mix well, wherein the Al / Mo molar ratio is 3. Polymerization was carried out according to the polymerization method of Example 1 and the polybutadiene obtained in this example was characterized. Polymerization conditions and polymer test results are shown in Table 2.

[0040] Table 2 MoCl 3 (OC 8 h 17 ) 2 Effect of / Bd on polymer structure

[0041]

[0042] It can be seen from Table 2 that when Mo / Bd>0.8×10 -3 Finally, the conversion rate is in the range of 60% to 70%. Mo / Bd has little effect on the 1,2-structure content. With the increase of Mo / Bd, the number of active centers increases, and the molecular weight and molecular weight distribution gradually decrease.

Embodiment 3

[0044] Prepare MoCl according to Example 1 3 (OC 8 h 17 ) 2 Catalyst, in a vacuum-filled airtight container filled with nitrogen, a certain amount of MoCl 3 (OC 8 h 17 ) 2 with quantitative AlEt 3 Mix well, wherein the Al / Mo molar ratio is 3. During polymerization, the Mo / Bd molar ratio was 1.2×10 -3 . Polymerization was carried out according to the polymerization method of Example 1. The difference is that the polymerization is carried out at different temperatures, and the reaction time is 120h. According to the method of Example 1, the polybutadiene obtained in this example was characterized. The polymerization conditions and polymer test results are shown in Table 3.

[0045] Table 3 Temperature vs. AlEt 3 / MoCl 3 (OC 8 h 17 ) 2 Effect of Catalytic System on Obtained Polymer Structure

[0046] temperature Conversion rates% 1,2％ Mn*10 4

[0047] The data in Table 3 shows that as long as sufficient time is given to the polymerization, low-te...

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Abstract

The invention relates to a high-vinyl polybutadiene rubber with adjustable microstructure and a preparation method thereof, which uses alkyl alcohol to replace MOCl 5 The catalytic system is the main catalyst and the alkyl aluminum is the co-catalyst. By adjusting the polymerization conditions such as the ratio of the catalyst and the polymerization temperature, the polymerization behavior and the microstructure of the product can be adjusted to obtain polybutadiene with the expected 1,2-structure content. rubber. The present invention is a new synthetic method for preparing polybutadiene whose vinyl content is adjustable in a wide range of 60-90%. New material with excellent performance.

Description

technical field [0001] The invention relates to the field of synthetic rubber, in particular to a catalytic system and a high-vinyl polybutadiene rubber with adjustable structure prepared by using the catalytic system and a preparation method. Background technique [0002] The European Commission introduced tire labeling laws in 2012, marking three key performance levels of tires: fuel efficiency, wet road grip and rolling noise. The aim is to increase energy efficiency, which in turn contributes to sustainable development and increased competitiveness. [0003] The promulgation of the tire labeling law requires the tread of automobile tires to have good wet skid resistance and low rolling resistance, but none of the existing rubber varieties can meet these two performance requirements at the same time. [0004] The microstructure of the polymer determines its physical properties. Due to the presence of a large number of vinyl side groups on the main chain of the polymer, r...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F136/06C08F4/69
Inventor 耿洁婷华静
Owner QINGDAO UNIV OF SCI & TECH
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