Starlike isoprene-styrene block copolymer and preparation method thereof

A styrene block and polystyrene block technology, which is applied in the field of polymer material synthesis and preparation, can solve the problems of wide and complex polymer molecular weight, and achieve the effects of strong thickening ability, convenient operation and simple production process.

Active Publication Date: 2014-06-04
PETROCHINA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, many kinds of star-shaped butadiene-isoprene-styrene copolymers have been reported in the literature. For example, a Chinese patent (CN1350012A) has invented a star-shaped block copolymer and its preparation method. The copolymer has the following structure : C-(SBR-IBR)n, where SBR is butadiene, styrene random copolymer block, IBR is butadiene, isoprene random copolymer block, n is the initiator functionality, n is greater than or equal to 3, this synthesis method belongs to the first nuclear rear arm method, that is, first synthesize a multifunctional initiator, and then add the required monomers to synthesize a star-shaped butadiene-isoprene-styrene copolymer, This method is relatively complex due to the strong association of multifunctional initiators resulting in a wide range of polymer molecular weights.
Another synthesis method is the arm-first-nucleus method, such as the US patent (US6034042), which first synthesizes the polymer arm, and then performs a coupling reaction by adding a coupling agent to obtain a star-shaped butadiene-isoprene-styrene Copolymer, the difficulty of this method is the control of coupling efficiency

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  • Starlike isoprene-styrene block copolymer and preparation method thereof
  • Starlike isoprene-styrene block copolymer and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0021] In a 500mL glass reaction bottle with magnetic stirring, add 90g cyclohexane and 7.5g isoprene, raise the temperature to 50°C, add 1.0mmol n-butyllithium initiator, when the polymerization reaction reaches 60 minutes, the isoprene The pentadiene polymerization reaction is completely completed, that is, the isoprene is completely consumed, and the polyisoprene block PI is obtained. Add 2.5 g of styrene and continue the reaction for 90 minutes until all styrene monomers are consumed to obtain polystyrene block S. The reaction temperature is lowered from 50°C to 20°C, adding tetrahydrofuran polar additives and divinylbenzene coupling agent for coupling reaction, wherein the molar ratio of tetrahydrofuran to n-butyllithium is 3:1, divinylbenzene to n-butyl The molar ratio of the base lithium is 3:1, and the divinylbenzene coupling agent is added dropwise, with an interval of 20 minutes each time. After all the divinylbenzene coupling agents are added, the reaction is contin...

Embodiment 2

[0025]In a 500mL glass reaction bottle with magnetic stirring, add 90g cyclohexane and 9.5g isoprene, heat up to 90°C, add 0.1mmol n-butyllithium Li initiator, when the polymerization reaction reaches 30 minutes The pentadiene polymerization reaction is completely completed, that is, the isoprene is completely consumed, and the polyisoprene block PI is obtained. Then add 0.5 g of styrene and continue the reaction for 60 minutes until all the styrene monomers are consumed to obtain polystyrene blocks. Cool down to 50°C, add tetrahydrofuran (THF) and divinylbenzene (DVB) for coupling reaction, where THF: Li (molar ratio) = 1:1, DVB: Li (molar ratio) = 3:1, DVB is added The method is to add dropwise, with an interval of 15 minutes each time. After all the DVB is added, the reaction is continued for 120 minutes, and a terminator containing 2,6,4-anti-aging agent is added to terminate the reaction; then the glue is settled by the traditional method, Drying in a vacuum oven at 50°C...

Embodiment 3

[0027] In a 500mL glass reaction bottle with magnetic stirring, add 90g cyclohexane and 5g isoprene, the temperature of the water bath is 20°C, add n-butyllithium Li initiator, when the polymerization reaction reaches 120 minutes, the isoprene The olefin polymerization reaction is all completed, that is, the isoprene is completely consumed, and the polyisoprene block PI is obtained; 5 g of styrene is added, and the reaction is continued for 150 minutes until the styrene monomer is completely consumed, and the polystyrene block PI is obtained. Section; add tetrahydrofuran (THF) and divinylbenzene (DVB) for coupling reaction, where THF: Li (molar ratio) = 5: 1, DVB: Li (molar ratio) = 1: 1, DVB is added in a split Dropping each time with an interval of 15 minutes. After all the DVB is added, continue the reaction for 180 minutes, and add a terminator containing 2,6,4-anti-aging agent to terminate the reaction. Subsequently, the glue solution was settled by traditional methods, a...

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Abstract

The invention relates to a starlike isoprene-styrene block copolymer and a preparation method thereof. The starlike isoprene-styrene segmented copolymer has a structure of (PI-S)n-C in which PI is a polyisoprene block, S is a polystyrene block, C is a residue of a starlike coupling reagent with the coupling efficiency being greater than 80%, and n is the average arm number and is greater than or equal to 3. The number-average molecular weight of the starlike copolymer (PI-S)n-C is 5*10<4>-5*10<5>, the number-average molecular weight of the polymer arm PI-S is 1*10<3>-1*10<5>, the content of S in the copolymer is 5-80wt% and the content of PI is 20-95wt%. The preparation method of the copolymer is realized by dropwise adding the coupling reagent step by step. The copolymer hydrogenated is a viscosity index improver with excellent performance, strong thickening ability and excellent low-temperature performance, and can satisfy the demand on the polymer performance on different occasions. The block copolymer is simple in preparation method, convenient to operate and high in yield and the structure and the molecular weight of the polymer are easily controlled.

Description

technical field [0001] The invention relates to a synthesis and preparation method of a polymer material, in particular to a star-shaped isoprene-styrene block copolymer with high coupling efficiency and a preparation method thereof. Background technique [0002] The study found that the star polymer as a viscosity index improver has both good shear resistance and thickening ability, and the performance of the polymer mainly depends on the structure of the polymer. U.S. patent (US4116917) adopts the arm-first-nucleus method and uses polydivinylbenzene as the core to synthesize a series of star-shaped hydrogenated diene polymers with different polymer arms. The number of arms in the star-shaped polymer is 7-15 , When the above polymer is used in multi-grade lubricating oil, its shear resistance performance is greatly improved, especially for high molecular weight polymers, and some polymers show good thickening ability. US patent (US4877836) invented a hydrogenated asymmetri...

Claims

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Application Information

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IPC IPC(8): C08F297/04
Inventor 张雪涛张东恒魏观为
Owner PETROCHINA CO LTD
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