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Preparation method of star-shaped solution polymerized butadiene styrene rubber with wide molecular weight distribution

A technology of solution-polymerized styrene-butadiene rubber and wide molecular weight distribution is applied in the field of preparation of star-shaped solution-polymerized styrene-butadiene rubber with wide molecular weight distribution. The effect of reducing shrinkage and rolling resistance

Active Publication Date: 2012-02-08
PETROCHINA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

For the synthesis of solution-polymerized styrene-butadiene with a wide molecular weight distribution, functionalized organolithium or organolithium combined with other reagents are often used as the initiation system, and the technology of adding the initiator at one time is adopted. Slippery can't have both

Method used

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  • Preparation method of star-shaped solution polymerized butadiene styrene rubber with wide molecular weight distribution
  • Preparation method of star-shaped solution polymerized butadiene styrene rubber with wide molecular weight distribution
  • Preparation method of star-shaped solution polymerized butadiene styrene rubber with wide molecular weight distribution

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Bu 3 Synthesis of SiLi:

[0032] In a 5L glass reactor with a silicone oil temperature control device, the system was replaced three times with argon gas. Add 3150ml of hexane and 2.11g of THF to the polymerization kettle, turn on the stirring, add 56g of metal lithium, and use a silicone oil bath to raise the temperature. When the temperature rises to 35°C, add chloroform at a flow rate of 5-10ml / min by dropwise 320ml of n-butane, while adding SiCl at a flow rate of 3-5ml / min in a dropwise way 4 110ml, the temperature of the whole reaction process was controlled at 50°C, after 70 minutes of reaction, it was naturally cooled at room temperature, settled for 4 hours, and suction filtered to obtain Bu 3 SiLi products are stored in vacuum airtight storage at -10°C.

Embodiment 2

[0034] In a jacketed 15L stainless steel reactor, the system was replaced three times with argon gas. In the polymerization kettle, add cyclohexane 7950g, styrene 300g (accounting for 25% of the total amount of monomers), butadiene 900g (accounting for 75% of the total amount of monomers), THF4.32g, once adding 12.1mmol Bu 3 SiLi is used as an initiator, the temperature is raised to 50°C, and the polymerization is carried out for 75 minutes. After the monomer is completely converted, the temperature is raised to 70°C, and 3.3 mmol of SnCl is added at a time. 4 The coupling agent is used for coupling reaction, and the reaction time is 60 minutes. After the coupling reaction was completed, the coupled reaction mixture was treated with water, 100 g of water and 12 g of antioxidant 1010 [tetrakis-(4-hydroxy-3,5-tert-butylphenylpropionic acid) pentaerythritol ester] were added and stirred. The glue is coagulated and dried by wet method.

Embodiment 3

[0038] In a jacketed 15L stainless steel reactor, the system was replaced three times with argon gas. In the polymerization kettle, add cyclohexane 7962g, styrene 330g (27.5% of the total monomers), butadiene 870g (62.5% of the total monomers), THF8.64g, add 12.1mmol of n-butyl Lithium and Bu 3 The initiator composed of SiLi (n-butyllithium and Bu 3 The mass ratio of SiLi is 30:70), the initiator is added in two times, the adding time interval is 3min, 6.1mol is added for the first time, 6.0mol is added for the second time, the temperature is raised to 60°C, and the polymerization is 50min, after the monomer is completely converted Raise the temperature to 80°C, add 6.6mmol SnCl twice 4 (Adding SnCl for the first time 4 80% of the total amount, after 15 minutes of reaction, add the remaining 20%) coupling agent to carry out the coupling reaction, and the reaction time is 80 minutes. After the coupling reaction was completed, the coupled reaction mixture was treated with wa...

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Abstract

The invention provides a preparation method of star-shaped solution polymerized butadiene styrene rubber (SSBR) with wide molecular weight distribution. The star-shaped SSBR is prepared through adopting a combined initiator system comprising an organic monolithium compound and a silicon lithium initiator, adding the initiator system in a multi-time dropwise mode, and carrying out a coupling reaction by adding a coupling agent in a multi-time adding mode after finishing polymerization. The star-shaped SSBR with wide molecular weight distribution, which can be processed under common conditions without adding low molecular weight polymers to improve the processing performance of the star-shaped SSBR and has the advantages of good tensile strength, balanced comprehensive mechanical property, good dynamic mechanical property, and combination of two properties of wet skid resistance and rolling resistance, is special rubber for tyres which has excellent properties. The star-shaped SSBR can be filled with carbon black, liquid rubber and the like, so the cost can be further saved, properties of rigidity, hardness and wear resistance of rubber products are improved, and the shrinkage of the rubber products is reduced, thereby the star-shaped SSBR can be widely applied to the shoemaking industry, the tyre industry and other industries.

Description

technical field [0001] The invention relates to a method for preparing solution-polymerized styrene-butadiene rubber by using combined initiators, in particular to a method for preparing solution-polymerized styrene-butadiene rubber with star structure and molecular weight distribution ≥ 2.5. Background technique [0002] Solution-polymerized styrene-butadiene (SSBR) has the characteristics of low rolling resistance, good wet skid resistance and abrasion resistance, and has become one of the recognized green and energy-saving rubbers. In recent years, people's requirements for rubber have been continuously improved, mainly to reduce rolling resistance as much as possible under the premise of ensuring wet skid resistance to meet energy-saving requirements. Since one end of the star-shaped solution-polymerized styrene-butadiene molecular chain has been linked together by a chemical bond, the number of free-moving molecular chain ends in the macromolecular network after vulcani...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F236/10C08F4/58C08F4/48
Inventor 崔英龚光碧胡才仲陶惠平梁滔张华强董静宋同江李锦山史工昌怀惠珍汤海鲲周漫
Owner PETROCHINA CO LTD
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