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Method for controlling phenylethene/butadiene block copolymer PB chain 1,2- structural content for hydrogenation

A technology of block copolymer and styrene, applied in the field of controlling PB chain 1 of styrene/butadiene block copolymer for hydrogenation, can solve the problems of low efficiency of polarity regulator, inability to stably control, large dosage and the like , to achieve the effect of easy control of industrial operation and reduced quality of industrial products

Active Publication Date: 2009-06-10
CHINA PETROCHEMICAL CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] The purpose of the present invention is to aim at the low efficiency of existing polar regulators, large dosage, sensitivity to temperature, passivation of regulating performance at high temperature, etc., which cannot stably control polybutadiene anion polymerization homopolymer and copolymer PB chain 1 , 2-structure (1,2-structure) content defects, develop a new structure-regulating reagent system, to achieve stable control of Bv content in the temperature-variable polymerization process

Method used

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  • Method for controlling phenylethene/butadiene block copolymer PB chain 1,2- structural content for hydrogenation

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] A 250ml three-necked bottle was used as the reaction vessel. Use a pipette to pipette 100ml of cyclohexane, accurately absorb 6g of butadiene, and add PMDETA and THF, the amount of which can be seen in Table 1. Add 0.4ml of monolithium initiator with a concentration of 0.734mol / L, and polymerize for 1.5h. After the polymerization is completed, the reaction is terminated with methanol, and then precipitated with methanol that is more than 5 times the amount of the solution to separate the polymer from the solvent. After drying, the polymer is tested by gel liquid chromatography (GPC), nuclear magnetic (NMR), etc. characterization. The following table is the polymerization temperature, the effect of polar reagents on the microstructure Bv content, where R 1 Represents the molar ratio of PMDETA to organic lithium active species, R 2 Represents the molar ratio of THF to active species.

[0018] Table 1 Changes of Bv content in polybutadiene under different conditions

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Embodiment 2

[0022] 3500ml of solvent was added to the 5L reactor, and 63g of styrene monomer, 54mmol of THF, 0.84mmol of PMEDTA and 4.2mmol of n-BuLi were added, and the polymerization temperature was 50°C to 70°C. After 30 minutes, add 294 grams of butadiene to carry out polymerization. The polymerization temperature is 50°C to 90°C, and the reaction time is 30 minutes to 60 minutes. Finally, an additional 63 grams of styrene was added for polymerization. Take a small amount of polymer, through GPC, H 1 Characterized by -NMR, the measured molecular weight is 100,000, the molecular weight distribution is 1.1, the polybutadiene PB chain 1,2-structure content is 30%, and the styrene content in the polymer is 30%.

[0023] The polymerization solution is fed with hydrogen to terminate, and then an appropriate amount of titanocene catalyst is added to keep the hydrogen pressure at 1 MPa to 2 MPa, and hydrogenation is carried out for 1 hour to 3 hours. The product was desolvated by water vapo...

Embodiment 3

[0025] 3500ml of solvent was added to a 5L reactor, and 58g of styrene monomer, 41mmol of THF, 0.64mmol of PMEDTA and 1.6mmol of n-BuLi were added, and the polymerization temperature was 50°C to 70°C. After 30 minutes, add 234 grams of butadiene to carry out polymerization. The polymerization temperature is 50°C to 90°C, and the reaction time is 30 minutes to 60 minutes. Finally, an additional 57 grams of styrene was added for polymerization. Take a small amount of polymer, through GPC, H 1 Characterized by -NMR, the measured molecular weight is 220,000, the molecular weight distribution is 1.1, the polybutadiene PB chain 1,2-structure content is 30%, and the polystyrene content in the polymer is 33%.

[0026]The polymerization solution is fed with hydrogen to terminate, and then an appropriate amount of titanocene catalyst is added to keep the hydrogen pressure at 1 MPa to 2 MPa, and hydrogenation is carried out for 1 hour to 3 hours. The product was desolvated by water vap...

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Abstract

The invention provides a control method for 1, 2-level structure contents in styrene / butadiene block copolymer PB chain, which are used for hydrogenation. The structure regulator system is composed of two polar modifiers, and used to regulate the microstructure of polybutadiene. The regulation system has high efficiency and low consumption, and is not sensitive to temperature. The stability control of Bv content can be realized in the temperature-changing polymerization process.

Description

technical field [0001] The invention relates to a method for controlling the 1,2-structure content of a styrene / butadiene block copolymer PB chain for hydrogenation. Background technique [0002] Butadiene is anionic polymerized with organic lithium as initiator and hydrocarbon compound as solvent. The microstructure of polybutadiene can be controlled by polar reagent as structure regulator, and various products can be prepared to meet different needs. Such as: the industrialized medium vinyl polybutadiene (MVPB), high vinyl polybutadiene (HVPB), random solution polystyrene butadiene rubber (S-SBR) three kinds of rubber, respectively containing vinyl (relative to Polybutadiene), that is, 1,2-structure (Bv), is 35% to 55%, greater than 70% and 25% to 70%, while S-EB-S thermoplastic elastomers require SBS middle block polybutadiene Diene B must contain vinyl (1,2-structure) between 35% and 55% to ensure elastic properties after hydrogenation. Therefore, in the homopolymer an...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F297/04C08F2/38C08K5/17
Inventor 韩丙勇邬智勇李望明夏金魁周立新梁红文
Owner CHINA PETROCHEMICAL CORP