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Method for preparing terminal carboxyl group polymer through active anionic polymer termination

A technology of active anions and active polymers, applied in the field of anionic polymerization, can solve the problems of less side reactions and harsh reaction conditions of side reactions, and achieve the effects of mild synthesis conditions, fast reaction speed and high functionalization efficiency

Inactive Publication Date: 2014-01-01
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] Aiming at the problems of many side reactions and harsh reaction conditions in the existing method for preparing carboxyl-terminated polymers by anionic polymerization, the present invention proposes a new carboxyl-terminated functionalization method, which can obtain terminal structures under mild conditions. Controlled carboxyl-terminated functionalized polymer, less side reactions, easy operation

Method used

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  • Method for preparing terminal carboxyl group polymer through active anionic polymer termination
  • Method for preparing terminal carboxyl group polymer through active anionic polymer termination
  • Method for preparing terminal carboxyl group polymer through active anionic polymer termination

Examples

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Effect test

Embodiment 1

[0029] Prepare 8g of polystyrene active anionic polymer, design molecular weight 2000, polymer concentration is 10g per 100ml cyclohexane, pass through 0.4ml of ethylene oxide to react for 30min, add the tetrahydrofuran solution of maleic anhydride (containing maleic anhydride 0.771g ), reacted at 40°C for 30min, and the resulting product was precipitated with HCl ethanol solution, dried in a vacuum oven at 50°C, and then characterized. It is measured that Mn=2100, MWD=1.12, and the capping rate is 80%.

Embodiment 2

[0031] Prepare 8g of polystyrene active anionic polymer, design molecular weight 2000, polymer concentration is 10g per 100ml cyclohexane, pass through 0.3ml of ethylene oxide to react for 30min, add the tetrahydrofuran solution of maleic anhydride (containing maleic anhydride 0.771g ), reacted at 20°C for 30min, and the resulting product was precipitated with HCl ethanol solution, dried in a vacuum oven at 50°C, and then characterized. It is measured that Mn=2200, MWD=1.15, and the capping rate is 77%.

Embodiment 3

[0033] Prepare 8g of polystyrene active anionic polymer, design molecular weight 2000, polymer concentration is 10g per 100ml cyclohexane, pass through 0.4ml of ethylene oxide to react for 30min, add the tetrahydrofuran solution of maleic anhydride (containing maleic anhydride 0.771g ), reacted at 60°C for 30min, and the resulting product was precipitated with HCl ethanol solution, and then placed in a vacuum oven at 50°C for characterization. It is measured that Mn=2300, MWD=1.17, and the end-capping rate is 88%.

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Abstract

The invention discloses a method for preparing terminal carboxyl group polymer through active anionic polymer termination, and belongs to the field of anionic polymerization. The method comprises steps as follows: step (1), an active anionic polymer solution is prepared and has the concentration of 5-20g / 100 ml, active anionic polymer comprises homopolymer or copolymer of styrene, butadiene and isoprene; step (2), oxa-cycloalkane is added into the active anionic polymer solution, the mixture reacts for 10-50 minutes at the temperatures ranging from 20 DEG C to 60 DEG C, and a solution of active polymer with an oxygen anion terminal is prepared; and step (3), the solution of active polymer with the oxygen anion terminal is mixed with acid anhydride, the mixture reacts for 20-120 minutes at the temperatures ranging from 20 DEG C to 100 DEG C, and a product is terminated by a methanol solution of HCl or an ethanol solution of HCl. The method is a new terminal carboxyl group functionalization method and is provided for solving problems of excessive side reactions, rigorous reaction conditions and the like of a conventional method for preparing terminal carboxyl group polymer through anionic polymerization; and by means of the method, terminal carboxyl group functionalized polymer with a controllable terminal structure can be obtained under the mild condition, the side reaction is few, and the operation is simple.

Description

technical field [0001] The invention relates to a method for terminal carboxylation of styrene, butadiene, isoprene homopolymers and copolymers thereof, belonging to the field of anionic polymerization. Background technique [0002] Functionalized polymers have important applications in many aspects such as stabilizing colloids, increasing filler dispersion and synthesizing new block copolymers, so the research on functionalized polymers is of great significance. Anionic polymerization has the characteristics of controllable molecular weight and narrow molecular weight distribution because there is no chain transfer and chain termination reaction. Polymerization is an efficient method to prepare structurally controllable chain-end functionalized polymers. [0003] There are two main methods for the preparation of end-functionalized polymers by anionic method, one is to directly initiate polymerization to obtain end-functionalized polymers through functionalized initiators, ...

Claims

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Application Information

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IPC IPC(8): C08F112/08C08F136/06C08F136/08C08F236/10C08F297/00C08F8/00
Inventor 鲁建民张志菲韩丙勇
Owner BEIJING UNIV OF CHEM TECH
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