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Method for synthesizing vinyl solution-polymerization butadiene-isoprene rubber adopting composite regulation system

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, and can solve the problems of no public coupling, inability to separate, and no mention of the synthesis of solution-polymerized butadiene-butadiene rubber.

Active Publication Date: 2007-08-01
CHINA PETROLEUM & CHEM CORP
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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 patent only mentions that it is suitable for vinyl polybutadiene MVPB, high vinyl polybutadiene HVPB, random solution styrene-butadiene rubber S-SBR and polystyrene-polybutadiene-polystyrene The industrial production of thermoplastic elastomer SBS and other products does not mention the synthesis of solution-polymerized butadiene rubber, let alone disclose the coupling situation

Method used

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  • Method for synthesizing vinyl solution-polymerization butadiene-isoprene rubber adopting composite regulation system
  • Method for synthesizing vinyl solution-polymerization butadiene-isoprene rubber adopting composite regulation system
  • Method for synthesizing vinyl solution-polymerization butadiene-isoprene rubber adopting composite regulation system

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] Embodiment 1 adopts 1G / THF as composite structure regulator, and cyclohexane / n-hexane mixed solvent (=88 / 12, weight ratio) system is synthesized star-shaped solution polybutadiene rubber (BD / IP=70 / 30, weight ratio )

[0043] 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 50°C, and the cold oil temperature at 30°C. First, 2600 g of refined cyclohexane / n-hexane, 271.95 g of butadiene, and 116.55 g of isoprene were added in one go. Then add 1G and THF according to the designed amount, heat the reaction material with hot oil, and when the temperature in the reactor rises to 50°C, control the ratio of hot oil and cold oil to keep the temperature of the material stable, and then add miscellaneous killing and initi...

Embodiment 2

[0073] Example 2 Using 1G / THF (1G / THF / Li molar ratio: 0.8 / 30 / 1) as composite structure regulator, cyclohexane / n-hexane mixed solvent (=88 / 12, weight ratio) system to synthesize star-shaped soluble polybutylene Rubber (BD / IP=70 / 30, weight ratio)

[0074] 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 initiation temperature is 70°C. The relationship between the 1,2-structure in the product and the amount of 1G / THF added is shown in Figure 5. The coupling efficiency and physical and mechanical properties of the products are shown in Table 5.

[0075] Table 5 Coupling efficiency and physical and mechanical properties of star-shaped solution polybutylene rubber

Embodiment 3

[0076] Example 3 Using 1G / THF (1G / THF / Li molar ratio: 0.8 / 30 / 1) as composite structure regulator, cyclohexane / n-hexane mixed solvent (=88 / 12, weight ratio) system to synthesize star-shaped soluble polybutylene Rubber (BD / IP=50 / 50, weight ratio)

[0077] 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 amount of raw materials added is 2600 g of cyclohexane / n-hexane, 194.25 g of butadiene, and 194.25 g of isoprene. The coupling efficiency and physical and mechanical properties of the products are shown in Table 6.

[0078] Table 6 Coupling efficiency and physical and mechanical properties of star-shaped solution polybutylene rubber

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PUM

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Abstract

The invention relates to a polymerization process for preparing solution polymerized butadiene-isoprene rubber, comprising carrying out copolymerization with butadiene and isoprene at 0- 130 Deg. C by taking organolithium as initiating agent and with existence of compound structure moderating system, and then carrying out coupling reaction with ploy degree of functionality of coupling agent after polymerization. The invention employs 1G / THF, 1G / Et3N or 2G / TMEDA compound structure moderating agent to get 1, 2- solution polymerized butadiene-isoprene rubber with construction content being 30- 50%. The invention is characterized by quality- stable product, easy- to- controlable process, and especial suitability for industrial production for medium ethenyl solution polymerized butadiene-isoprene rubber.

Description

technical field [0001] The present invention relates to a kind of polymerization method of solution polymerization butadiene rubber (IBR), more specifically, relate to a kind of adopting 1G / THF, 1G / Et 3 The polymerization method of N or 2G / TMEDA composite adjustment system to synthesize solution-polymerized butadiene rubber with medium vinyl content and the resulting solution-polymerized butadiene rubber with medium vinyl 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 63.7%. 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] It is mentioned in US 4,523,618 t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F236/06C08F4/48C08F2/44C08K5/54C08F236/08
Inventor 王雪李伟刘天鹤徐炜梁爱民
Owner CHINA PETROLEUM & CHEM CORP
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