Butadiene styrene rubber and preparation method thereof

A technology of styrene-butadiene rubber and styrene, which is applied in the field of synthetic rubber, can solve the problems that the polymer microstructure cannot be adjusted, the polymer is not easy to couple, and no specific instructions are made, so as to achieve effective control, low production cost, The effect of fast polymerization rate

Active Publication Date: 2018-07-03
PETROCHINA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the solubility of alkyl sulfonate compounds in aliphatic hydrocarbon solvents is poor. At the same time, alkyl sulfonate compounds will generate a lot of foam when they meet water during the coagulation process, which will affect the coagulation effect.
[0008] Patent CN1089272A discloses a method for controlling vinyl content in butadiene homopolymers and copolymers, using two or more Lewis bases of different polarities as structural regulators to synthesize random solution-polymerized styrene-butadiene rubber, but the The focus of the patent is on the control of vinyl content, and no specific instructions are given on the control of styrene content and randomness of styrene-butadiene rubber, and in this method, the monomer must be reacted in cyclohexane solvent or benzene solvent
[0009] In addition, there are also literatures that describe the use of cyclic ether structure regulators, the most common being tetrahydrofuran and its derivatives, such as THF-ONa, 2,5-substituted tetrahydrofuran, etc., but when its addition reaches a certain value, it cannot Then adjust the microstructure of the polymer; or use linear long-chain symmetrical ether compounds (R-O-CH 2 -CH 2 -O-R, R-O-CH 2 -CH 2 -O-CH 2 -CH 2 -O-R) as a structural regulator, but the addition of this regulator will make the polymer difficult to couple, indicating that the addition of this kind of regulator may kill the active species in the system

Method used

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  • Butadiene styrene rubber and preparation method thereof
  • Butadiene styrene rubber and preparation method thereof
  • Butadiene styrene rubber and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] Under the protection of high-purity nitrogen, add 2000g of cyclopentane, 190g of styrene, and 300g of butadiene into a 5L polymerization kettle, then add 0.54mol of ethyl tetrahydrofurfuryl ether and 27.8mol of tetrahydrofuran, and stir for 10min. The temperature was raised to 40° C., and then 0.48 mol of n-butyllithium was added. See Table 1 for the specific raw material ratio.

[0043] About 0.5 hours after the start of the reaction, the temperature of the polymerization tank rose to the highest point of about 68°C. The reaction was continued at this temperature for about 2.5 hours, and then terminated with ethanol.

[0044] The styrene-butadiene rubber that present embodiment makes 1 H-NMR spectrum as figure 1 As shown, the infrared spectrum is shown in figure 2 As shown, after calculation, the styrene content is 37.8%, the vinyl content is 36.3%, and the degree of randomness is 100%. The specific results are shown in Table 2, which illustrates that the method pro...

Embodiment 2

[0046] Under the protection of high-purity nitrogen, add 2000g cyclopentane, 190g styrene, and 300g butadiene to the reactor, then add 0.54mol of ethyl tetrahydrofurfuryl ether and 27.8mol of tetrahydrofuran, and stir for 10min. Warm up to 40°C, and then add 0.40mol of n-butyllithium. See Table 1 for the specific raw material ratio.

[0047] About 0.5 hours after the start of the reaction, the temperature of the reactor rose to the highest point of about 65°C, and the temperature was maintained to continue the reaction for about 3.5 hours, and then terminated with ethanol.

[0048] The styrene-butadiene rubber is tested and characterized, and the styrene-butadiene rubber obtained in the present embodiment has 1 H-NMR spectrum and figure 1 Approximately, the infrared spectrogram and figure 2 Approximately, after calculation, the styrene content is 37.5%, the vinyl content is 40.6%, and the degree of randomness is 100%. The results are shown in Table 2, illustrating that the ...

Embodiment 3

[0050] Under the protection of high-purity nitrogen, 2000g of cyclopentane, 170g of styrene, and 300g of butadiene were sequentially added to the reaction kettle, and then 0.54mol of ethyl tetrahydrofurfuryl ether and 23.7mol of tetrahydrofuran were added, and after stirring for 10min, the reaction kettle The temperature was raised to 40° C., and then 0.40 mol of n-butyllithium was added. See Table 1 for the specific raw material ratio.

[0051] About 0.5 hours after the start of the reaction, the temperature of the reactor rose to the highest point of about 71°C. The reaction was maintained at this temperature for about 1.5 hours, and then terminated with ethanol.

[0052] The styrene-butadiene rubber is tested and characterized, and the styrene-butadiene rubber obtained in the present embodiment has 1 H-NMR spectrum and figure 1 Approximately, the infrared spectrogram and figure 2 Approximately, after calculation, the styrene content is 36.1%, the vinyl content is 42.5%, ...

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Abstract

The invention provides a preparation method of butadiene styrene rubber. The preparation method comprises the following step: carrying out a copolymerization reaction on styrene and butadiene in a hydrocarbon solvent to obtain solution polymerized styrene-butadiene rubber by taking organic lithium as an initiator and tetrahydrofurfuryl alcohol alkyl ether and tetrahydrofuran as a structural regulator, wherein the molar ratio of tetrahydrofurfuryl alcohol alkyl ether and organic lithium is (1-4): 1 and the molar ratio of tetrahydrofuran and organic lithium is greater than 40: 1. Vinyl-based solution polymerized styrene-butadiene rubber in random high styrene is prepared by means of the preparation method, so that the service performance of butadiene styrene rubber is improved. By adopting the preparation method, the raw materials are easily available, and the tetrahydrofuran regulator in industrial production can be recycled with the hydrocarbon solvent, so that the production cost is lowered greatly.

Description

technical field [0001] The invention relates to a styrene-butadiene rubber and a preparation method thereof, in particular to a preparation method of vinyl solution-polymerized styrene-butadiene rubber in random high styrene, belonging to the technical field of synthetic rubber. Background technique [0002] Polymerized Styrene Butadiene Rubber (SBR) is the largest general-purpose synthetic rubber variety and one of the earliest synthetic rubber varieties to achieve industrial production. Styrene butadiene rubber is divided into emulsion polystyrene butadiene rubber and solution polystyrene butadiene rubber according to its preparation method, wherein solution polystyrene butadiene rubber is made of butadiene (CH 2 =CH-CH=CH 2 ) and styrene (C 6 h 5 -CH=CH 2 ) as the main monomer, in a hydrocarbon solvent, using organolithium as an initiator, after sufficient polymerization, adding antioxidants and other auxiliary agents, it is obtained through coagulation, drying and ot...

Claims

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Application Information

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IPC IPC(8): C08F236/10C08F212/08C08F4/48C08F2/06
CPCC08F2/06C08F4/482C08F236/10C08F212/08
Inventor 韩艳费宇晶杨广明韩明哲周豪宋玉萍赵宇徐燕吴利平仝璐孙福权李洪波王喆张伟
Owner PETROCHINA CO LTD
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