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Structure modifier for anionic polymerization and anionic polymerization method

A structure regulator, anionic polymerization technology, applied in the field of anionic polymerization, can solve the problems of irritating odor, strong, safety and environmental protection problems, and achieve the effect of excellent low temperature resistance and low glass transition temperature

Active Publication Date: 2015-04-29
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the conditioner can be easily removed from the solvent, the conditioner has a strong pungent odor, which is not enough in terms of safety and environmental protection

Method used

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  • Structure modifier for anionic polymerization and anionic polymerization method
  • Structure modifier for anionic polymerization and anionic polymerization method
  • Structure modifier for anionic polymerization and anionic polymerization method

Examples

Experimental program
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Effect test

Embodiment 1

[0073] In a 5-liter stainless steel stirred reactor, under the protection of high-purity nitrogen, add 2288g of mixed solvent (a mixture of cyclohexane and n-hexane, the mass ratio of cyclohexane / n-hexane is 82 / 18), 186g of isopentyl Diene and 186 g butadiene. Then, add 2,2-(ditetrahydrofuryl)propane and tetrahydrofurfuryl butyl ether, wherein, the amount of 2,2-(ditetrahydrofuryl)propane (DTHFP) is 0.69mmol, tetrahydrofurfuryl butyl ether The dosage of (BET) is 0.173mmol (DTHFP / Li=0.2, BET / Li=0.05). Next, after removing impurities with n-butyl lithium initiator, 3.45 mmol of n-butyl lithium was added to initiate polymerization. The polymerization reaction was carried out at a temperature of 70° C., during the polymerization reaction, the pressure was controlled at 0.1 MPa, and the polymerization reaction time was 40 minutes. After the polymerization was completed, 0.59 mmol of tin tetrachloride was added into the reactor, and after stirring for 70 minutes, 0.69 mmol of isop...

Embodiment 2

[0085] In a 5-liter stainless steel stirred reactor, under the protection of high-purity nitrogen, add 2288g of mixed solvent (a mixture of cyclohexane and raffinate, the mass ratio of cyclohexane / raffinate is 82 / 18), 178g Isoprene and 76 g butadiene. Then, add 2,2-(ditetrahydrofuryl)propane and tetrahydrofurfuryl butyl ether, wherein, the amount of 2,2-(ditetrahydrofuryl)propane (DTHFP) is 0.43mmol, tetrahydrofurfuryl butyl ether The dosage of (BET) is 0.43mmol (DTHFP / Li=0.1, BET / Li=0.1). Next, a n-butyllithium initiator was used to kill impurities, and 4.3 mmol of n-butyllithium was added to initiate polymerization. The polymerization reaction was carried out at a temperature of 40° C., during the polymerization reaction, the pressure was controlled at 0.2 MPa, and the polymerization reaction time was 40 minutes. After the polymerization was completed, 0.73 mmol of tin tetrachloride was added into the reactor, and after stirring for 70 minutes, 0.86 mmol of isopropanol was...

Embodiment 3

[0088] In a 5-liter stainless steel stirred reactor, under the protection of high-purity nitrogen, add 2288g of mixed solvent (a mixture of cyclohexane and n-pentane, the mass ratio of cyclohexane / n-pentane is 82 / 18), 187g Isoprene and 125 g butadiene. Then, add 2,2-(ditetrahydrofuryl)propane and tetrahydrofurfuryl butyl ether, wherein, the amount of 2,2-(ditetrahydrofuryl)propane (DTHFP) is 1.34mmol, tetrahydrofurfuryl butyl ether The dosage of (BET) is 0.19mmol (DTHFP / Li=0.7, BET / Li=0.1). Next, a n-butyllithium initiator was used to kill impurities, and then 1.92 mmol of n-butyllithium was added to initiate polymerization. The polymerization reaction was carried out at a temperature of 50° C., during the polymerization reaction, the pressure was controlled at 0.3 MPa, and the polymerization reaction time was 40 minutes. After the polymerization was completed, 0.326 mmol of tin tetrachloride was added into the reactor, and after stirring for 70 minutes, 0.384 mmol of isopro...

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Abstract

The invention discloses a structure modifier for anionic polymerization. The structure modifier comprises a bistetrahydrofuran compound shown in formula I and alkyl tetrahydrofurfuryl ether shown in formula II. The invention also discloses an anionic polymerization method. The anionic polymerization method comprises the step of under the anionic polymerization condition, in the presence of an organolithium initiator and the structure modifier provided by the invention, enabling at least two conjugated dienes to polymerize in at least one solvent. The structure modifier is used for effectively regulating the microstructure of an obtained copolymer to realize random distribution of various structural units on a macromolecular chain during copolymerization of the conjugated diene solutions, particularly during copolymerization of butadiene and isoprene solutions.

Description

technical field [0001] The invention relates to a structure regulator for anionic polymerization, and also relates to an anion polymerization method using the structure regulator. Background technique [0002] With the continuous development of science and technology, the field of scientific research has also been continuously expanded. The range of activities has extended from the inland to the coast, from the equator to the north and south poles. Changes in climate, temperature and other conditions have made the requirements for various scientific instruments become more demanding. For rubber materials, it must have excellent low temperature resistance to meet the above requirements. Usually people use the glass transition temperature (T g ) to evaluate the low temperature resistance of rubber. but except T g In addition, the crystallization properties of rubber should also be considered. Such as butadiene rubber although T g It is lower than -100°C, but because of i...

Claims

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Application Information

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IPC IPC(8): C08F230/06C08F236/08C08F2/38C08F2/06C08F4/48C08F8/42
Inventor 康新贺徐林李传清于国柱王妮妮刘辉孙文娟
Owner CHINA PETROLEUM & CHEM CORP
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