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Preparation method of butadiene/1,3-pentadiene random copolymer

A random copolymer, pentadiene technology, applied in the field of preparation of butadiene/1,3-pentadiene random copolymer, can solve the problem of wide molecular weight distribution, butadiene and isoprene copolymer high molecular weight issues

Inactive Publication Date: 2017-03-08
CHINA PETROLEUM & CHEM CORP +1
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Problems solved by technology

The Chinese patent application with the publication number CN1599762A reports a method for preparing butadiene and isoprene, which uses conjugated diene monomers, organophosphates of rare earth metals, alkylating agents, and Butadiene and isoprene are reacted under the action of the catalytic system using aluminum-based halogen donor as a catalyst system, but the molecular weight of the prepared butadiene and isoprene copolymer is relatively high and the molecular weight distribution is wide

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  • Preparation method of butadiene/1,3-pentadiene random copolymer

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[0018] A preparation method of butadiene / 1,3-pentadiene copolymer, comprising:

[0019] In an anhydrous and oxygen-free atmosphere, add a quantitative amount of butadiene and 1,3-pentadiene cyclohexane solution (concentration is 10-15g monomer / 100ml cyclohexane ), add a measured random additive, shake well, then add a measured organic alkali metal initiator, and react at 30°C to 90°C. After the polymerization is completed, use 2,6-di-tert-butyl p- The methanol solution of cresol terminated the reaction, and after the solvent was removed, it was dried in a vacuum oven at 50°C.

[0020] In the present invention, the microstructure of the synthesized polymer adopts the nuclear magnetic instrument of the model INOVA-400 produced by U.S. Varian Company to measure, and the frequency is 400MHz, with tetramethylsilane (TMS) as the internal standard, and the solvent is CDCl 3 . Infrared analysis was carried out using an infrared instrument of the type IRAffinity-1 produced by Shimadz...

Embodiment 1

[0034] Add the mixed monomer of butadiene and 1,3-pentadiene with a mass ratio of 1:9 to the absorption bottle of cyclohexane (the monomer concentration is 10g / 100ml cyclohexane), and measure 5g of the mixed monomer , and then add a specific amount of randomizing additive a to satisfy n SDS =0.012mmol, finally add 0.12mmol of n-butyllithium (n-BuLi) (the molar ratio of SDS to n-BuLi is 0.1), put the solution into the schlenk reactor and rapidly raise the temperature to 50°C, and polymerize at 50°C for 3-5 Hour. After cooling, stop the reaction with a methanol solution containing 1 wt% 2,6-di-tert-butyl-p-cresol, then precipitate the polymer with excess methanol, wash it repeatedly for 4-5 times, and finally dry it in vacuum at 40°C for 24 hours.

[0035] The calculated polymer yield by weighing is 98%, and the number-average molecular weight of the polymer measured by GPC is 39,000g / mol; the molecular weight distribution is 1.2; 1 H-NMR and IR determined that the 1,4-PB% in ...

Embodiment 2

[0038] Butadiene and 1,3-pentadiene mixed monomers with a mass ratio of 2:8 are added to the absorption bottle of n-hexane (the monomer concentration is 10g / 100ml n-hexane), and the mixed monomers of 5g are measured, and then Add a specific amount of randomizing additive b to satisfy n SDS =0.024mmol, finally add 0.12mmol lithium diisopropylamide (N-Li) (the molar ratio of SDS to N-Li is 0.2), put the solution into the schlenk reactor and rapidly raise the temperature to 60°C, and polymerize at 40°C for 2 ~4 hours. After cooling, stop the reaction with a methanol solution containing 1 wt% 2,6-di-tert-butyl-p-cresol, then precipitate the polymer with excess methanol, wash it repeatedly for 4-5 times, and finally dry it in vacuum at 40°C for 24 hours.

[0039] The calculated polymer yield by weighing is 99%, and the number-average molecular weight of the polymer measured by GPC is 41,000g / mol; the molecular weight distribution is 1.3; 1 H-NMR and IR determined that the 1,4-PB%...

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Abstract

The invention belongs to the technical field of polymer synthesis, and specifically discloses a preparation method of a butadiene / 1,3-pentadiene random copolymer. According to the preparation method, in the absence of water and oxygen, an organic alkali metal initiator is adopted, a randomization additive is added, butadiene and 1,3-pentadiene carry out copolymerization reactions to obtain the butadiene / 1,3-pentadiene random copolymer, the mass ratio of butadiene to 1,3-pentadiene is 1:9-6:4, the reaction temperature is 0 to 100 DEG C, and the reaction time is 1 to 24 hours. The results show that the prepared butadiene / 1,3-pentadiene random copolymer has the advantages of controllable molecular weight, adjustable molecular weight distribution, high randomization degree, controllable microscopic polymer structure, low glass-transition temperature (Tg=-70 to -40 DEG C), quick reaction rate, and high monomer conversion rate (100%).

Description

technical field [0001] The invention belongs to the technical field of polymer synthesis, and in particular relates to a preparation method of a butadiene / 1,3-pentadiene random copolymer. Background technique [0002] With the development of science and technology, people's requirements for the performance of rubber materials are constantly improving. Since butadiene-isoprene copolymer rubber has excellent low temperature resistance, wear resistance and low rolling resistance at low temperature, the research on the copolymerization of these two types of monomers is very extensive. 1,3-Pentadiene as Petroleum C 5 One of the main components in the distillate, the content is second only to isoprene and cyclopentadiene 1,3-pentadiene (also known as piperylene), but for butadiene-1,3-pentadiene However, studies on the copolymerization of alkenes are relatively rare. 1,3-Pentadiene has a terminal methyl group. After polymerization, there are 11 kinds of geometric isomers contai...

Claims

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Application Information

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IPC IPC(8): C08F236/06C08F236/08C08F4/48
Inventor 傅建松刘坤徐伟箭姚亚娟秦技强任磊何卿吴忠平奚军
Owner CHINA PETROLEUM & CHEM CORP
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