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Synthetic method of solution polymerized butadiene-isoprene rubber

A technology of solution-polymerized butadiene-butadiene rubber and a polymerization method, which is applied in the field of polymerization of solution-polymerized butadiene-butadiene rubber, can solve the problems such as the inability to remove the structure regulator, the influence of the recovered solvent, and the coupling efficiency close to 0.

Inactive Publication Date: 2012-07-11
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this alcohol ether has two major disadvantages as a regulator: one is that it cannot be directly separated from hexane; the other is that the coupling efficiency is close to zero.
However, the structure regulator cannot be completely removed from the polymerization solvent, and the recovery of the solvent has an impact on the subsequent polymerization reaction

Method used

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  • Synthetic method of solution polymerized butadiene-isoprene rubber
  • Synthetic method of solution polymerized butadiene-isoprene rubber
  • Synthetic method of solution polymerized butadiene-isoprene rubber

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] Example 1 Cyclohexane / n-hexane mixed solvent (=82 / 18, weight ratio) system to synthesize star-shaped solution polybutadiene rubber (BD / IP=75 / 25, weight ratio)

[0039] The polymerization is carried out in a 5-liter stainless steel reactor. After the reactor is soaked with cyclohexane / n-hexane, it is evacuated and filled with nitrogen (high-purity nitrogen) for three times. The reactor is heated by hot oil and cooled by cold oil. The temperature of the hot oil is set to Set at 30°C, the cold oil temperature is set at 10°C. First, 2600 g of refined cyclohexane / n-hexane, 0.003 g of ETE, 291.38 g of butadiene, and 97.13 g of isoprene were added in one go. Then heat the reaction material with hot oil, and when the temperature in the reactor rises to 30°C, control the ratio of hot oil and cold oil to keep the temperature of the material stable, and then add 14ml (0.3M cyclohexane / n-hexane solution) to initiate polymerization. After 40 minutes of polymerization reaction, 0...

Embodiment 2-9

[0040] Example 2-9 Cyclohexane / n-hexane mixed solvent (=82 / 18, weight ratio) system to synthesize star-shaped solution polybutadiene rubber (BD / IP=75 / 25, weight ratio)

[0041] The preparation method of the copolymer and the test of the microstructure in the polymer are the same as in Example 1, except that ETE is added according to the designed amount, and the specific amount is shown in Table 1.

[0042] The 1,2-structure content, molecular weight, molecular weight distribution, and coupling efficiency measurement results of ETE addition, polymerization product are shown in Table 1, as can be seen from Table 1: the star-shaped solution-polymerized butadiene rubber prepared according to the present invention can be successfully carried out Coupling reaction, and the content of 1,2-structure in the copolymer is controllable.

[0043] Table 1 Molecular parameters and microstructure of star-shaped solution polybutylene rubber

[0044] Experiment number

Example 1 ...

Embodiment 10-18

[0059] Examples 10-18 Cyclohexane system synthesis of star-shaped solution polybutadiene rubber (BD / IP=65 / 35, weight ratio)

[0060] The preparation method of the copolymer and the test of the microstructure in the polymer are the same as in Example 1, except that the polymerization solvent system is changed to 2600g of cyclohexane, the initiation temperature is changed to 50°C, and ETE is added according to the designed amount. The 1,2-structure content of the product is shown in Table 3.

[0061] Table 3 Microstructure of star-shaped solution polybutylene rubber

[0062] Experiment number

Example 10

Example 11

Example 12

Example 13

Example 14

ETE(g)

0.003

0.03

0.05

0.15

0.45

1，2-(％)

8.0

13.4

16.6

25.1

49.1

[0063] Table 3 (continued)

[0064] Experiment number

Example 15

Example 16

Example 17

Example 18

ETE(g)

0.9

1....

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Abstract

The invention relates to a polymerization method for producing solution polymerized butadiene-isoprene rubber. The polymerization method comprises the following steps of: copolymerizing butadiene and isoprene in a hydrocarbon solvent at 0-130 DEG C in the presence of organic lithium as an initiator and tetrahydrofurfuryl alcohol as a structure regulator and after polymerization reaction basically completes, adding a coupling agent with functionality of 2-4 into the copolymer to perform the coupling reaction. The tetrahydrofurfuryl alcohol is used as the structure regulator, so as to obtain a 1,2-structure content adjustable random copolymer rubber.

Description

technical field [0001] The present invention relates to a method for the polymerization of solution-polymerized butadiene rubber (IBR), more particularly, to a method for the polymerization of star-shaped solution-polymerized butadiene rubber with different 1,2-structure content. Background technique [0002] It is reported in the literature that ethylene glycol dimethyl ether (1G) can be used as a regulator to adjust the vinyl content in polybutadiene to exceed 60.0%. However, this alcohol ether has two major disadvantages as a regulator: one is that it cannot be directly separated from hexane; the other is that the coupling efficiency is close to zero. Therefore, ethylene glycol diethyl ether and ethylene glycol dibutyl ether in this type of compound cannot meet the test requirements. [0003] JP 82 / 87406 relates to a method for synthesizing butadiene and isoprene copolymers using butyllithium and diglyme (2G), but the conversion rate of the method is not high. [0004] ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F236/06C08F236/08C08F4/48C08F2/38C08F2/06C08F8/42
Inventor 王雪李传清刘慧玲徐林刘天鹤李建成徐炜刘凤香吕万树王世朝王丽丽关逸英
Owner CHINA PETROLEUM & CHEM CORP
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