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Regulator and method for controlling microstructure of butadiene homopolymer and copolymer

A technology of microstructure and regulator, which is applied in the field of butadiene anionic polymerization, can solve problems such as the inability to stably control the vinyl content of polybutadiene, and the temperature sensitivity of polarity regulator polymerization.

Inactive Publication Date: 2006-10-11
PETROCHINA CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The purpose of the present invention is to solve the sensitivity of the polarity regulator to the polymerization temperature for the defect that the prior art cannot stably control the polybutadiene vinyl content in the butadiene homopolymer and the copolymer

Method used

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  • Regulator and method for controlling microstructure of butadiene homopolymer and copolymer
  • Regulator and method for controlling microstructure of butadiene homopolymer and copolymer

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Take three 250ml polymerization bottles with double-branched tubes, first bake at high temperature, and replace nitrogen more than three times. Then pipette 100ml of butadiene-cyclohexane solution (concentration: 10g butadiene / 100ml cyclohexane solution) respectively, and add to each polymerization bottle. Use the binary composite regulator system of tetrahydrofuran (hereinafter referred to as THF) / sodium dodecylbenzenesulfonate (hereinafter referred to as SDBS), [THF] / [PBLi]=2.0, [SDBS] / [PBLi]=0.3, with n-Butyllithium n-BuLi was used as the initiator (0.85M concentration). First use n-butyllithium initiator to remove impurities, then add 0.24ml of n-butyllithium (design molecular weight is 50000), and carry out polymerization in water baths with constant temperature of 50°C, 60°C, and 70°C respectively, and the polymerization time is 2 hours . After the polymerization, the reaction was terminated with ethanol, and then the polymer was precipitated with ethanol, and d...

Embodiment 2

[0025] Substitute THF in embodiment 1 with pentamethyldivinyltriamine (hereinafter referred to as PMDETA), form the binary composite regulator system of SDBS / PMDETA, all the other polymerization conditions are similar to embodiment 1, according to change PMDETA and SDBS in the system The dosage is different from the active center concentration [PBLi] molar ratio, and can be correspondingly obtained figure 2 . Depend on figure 2 It can be seen that when PMDETA and SDBS are fixed, the 1,2-structure content of the sample decreases slowly with the increase of temperature, and the temperature rises by 20°C, and the 1,2-structure content only decreases by about 6%. Out of very good temperature insensitivity. The measured Mn is about 55000, and the MWD is between 1.2 and 1.3.

Embodiment 3

[0027] Take a 250ml polymerization bottle with a double-branched tube, first bake it at high temperature, and replace the nitrogen more than 3 times. Then use a pipette to pipette 100 ml of butadiene in hexane (concentration: 15 g of butadiene / 100 ml of hexane solution), and add it to the polymerization bottle. Use the binary compound regulator system of PMDETA / SDBS, [SDBS] / [PBLi]=0.3, [PMDETA] / [PBLi]=0.5, take n-butyllithium n-BuLi as initiator, (concentration is 0.85M) . First use n-butyllithium initiator to remove impurities, then add 0.22ml of n-butyllithium (design molecular weight is 80000), and carry out polymerization in a water bath with a constant temperature of 50°C, and the polymerization time is 2 hours. After the polymerization, the reaction was terminated with ethanol, and the polymer was precipitated with ethanol, and dried in a vacuum oven at 50°C. The 1,2-structure content of the sample was analyzed by nuclear magnetic resonance NMR to obtain the content of...

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Abstract

This invention belongs to butadiene anionic polymerization. In industrial production, the content of 1, 2-structure in butadiene rubber changes with the polymerization temperature. The temperature has an impact on product quality as well. The regulator is a binary compound system, consisting of two kinds of separate regulators, A and B. A's structure is as the picture below. R is alkyl more than 6 carbons. M is alkali metal, sodium or kalium. B is Lewis base. The proportion of A and B is 1-15. The controlling method is as followings: prepare polymerized solution of butadiene and butadiene-styrene monomer in the hydrocarbon solvent. Initiate the polymerization reaction by adding regulator mentioned above and organolithium. React at 40deg C-100 deg C for 1-4 hours. Initiating agent is 0.2-2mmol per 100g monomer. The mole ratio of A regulator and initiating agent is 0.1-1.0. While the mole ration of B regulation and initiating agent is 1.0-15. Vacuum dry the product to get the homopolymer or multipolymer of butadiene rubber. This invention is advantageous in the reduced usage amount of regulator and temperature insensitive.

Description

technical field [0001] The invention relates to a method for controlling the microstructure of butadiene homopolymer and copolymer, belonging to the field of butadiene anion polymerization. Background technique [0002] Polarity regulators are often added in anionic polymerization to adjust the polymer microstructure, molecular weight and its distribution, and the speed of the reaction, especially the adjustment of the polymer microstructure (such as the adjustment of the vinyl content of polydiene), so that the polarity Regulators play a pivotal role in anionic polymerization. In polydiene, its microstructure mainly refers to the cis, trans-1,4-structure, 1,2-structure or 3,4-structure of the polymer, as well as the isotactic, syndiotactic and arrhythmia of some polymers. The regular structure also includes the sequence distribution of the copolymer, that is, block and random distribution. There are many factors that affect the microstructure of polymers, such as the type...

Claims

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Application Information

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IPC IPC(8): C08F2/38C08F36/06C08F4/48
Inventor 韩丙勇赵方园胡才仲陈建刚康安福董静陶惠平胡海华杨绮波
Owner PETROCHINA CO LTD
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