Method for preparing thiol-functionalized polyester with micro-reaction unit

A micro-reaction device and functionalized technology, which is applied in the field of polymer chemistry, can solve the problems of poor molecular weight distribution control, harsh reaction conditions, and low thiol introduction rate, and achieve high thiol introduction rate, low cost, and strong operability. Effect

Inactive Publication Date: 2016-08-10
NANJING UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The technical problem to be solved in the present invention is to provide, to solve the problems such as low sulfhydryl introduction rate, poor controllability of molecular weight distribution and harsh reaction conditions existing in the prior art

Method used

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  • Method for preparing thiol-functionalized polyester with micro-reaction unit
  • Method for preparing thiol-functionalized polyester with micro-reaction unit
  • Method for preparing thiol-functionalized polyester with micro-reaction unit

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] Before the experiment, argon and freshly steamed toluene were used to remove water and air from the micro-reaction device.

[0039] Two groups of samples were injected, and two 20mL schlenk bottles were taken, corresponding to bottle number A and bottle B. Bake under a high temperature oven, and use a schlenk device to replace the gas three times, so that the inside of the two schlenk bottles is in an argon atmosphere. Liquid A is a mixed organic solvent solution of catalyst and initiator, and solid catalyst Sn(OTf) is added in the glove box 2 (55.2mg, 0.1324mmol, 1eq), then add the initiator 6-mercapto-1-hexanol MH (1777.3mg, 13.24mmol, 100eq) with a micro syringe, and finally add 10mL of newly steamed toluene and tetrahydrofuran mixed solvent (4: 1), A solution is prepared and kept for use. Liquid B is pure δ-valerolactone, add pure δ-VL to bottle B with a syringe for future use.

[0040] To carry out the reaction, pump liquid A and liquid B into two 50mL syringes ...

Embodiment 2

[0042] Before the experiment, argon and freshly steamed toluene were used to remove water and air from the micro-reaction device.

[0043] Two groups of samples were injected, and two 20mL schlenk bottles were taken, corresponding to bottle number A and bottle B. Bake under a high temperature oven, and use a schlenk device to replace the gas three times, so that the inside of the two schlenk bottles is in an argon atmosphere. Liquid A is a mixed organic solvent solution of catalyst and initiator, and solid catalyst Sn(OTf) is added in the glove box 2 (55.2mg, 0.1324mmol, 1eq), then add the initiator 6-mercapto-1-hexanol MH (1777.3mg, 13.24mmol, 100eq) with a micro syringe, and finally add 10mL of newly steamed toluene and tetrahydrofuran mixed solvent (4: 1), A solution is prepared and kept for use. Liquid B is pure δ-valerolactone, add pure δ-VL to bottle B with a syringe for future use.

[0044] To carry out the reaction, pump liquid A and liquid B into two 50mL syringes ...

Embodiment 3

[0046] Before the experiment, argon and freshly steamed toluene were used to remove water and air from the micro-reaction device.

[0047] Two groups of samples were injected, and two 50mL schlenk bottles were taken, corresponding to bottle number A and bottle B. Bake under a high temperature oven, and use a schlenk device to replace the gas three times, so that the inside of the two schlenk bottles is in an argon atmosphere. Liquid A is a mixed organic solvent solution of catalyst and initiator, and solid catalyst Sn(OTf) is added in the glove box 2 (55.2mg, 0.1324mmol, 1eq), then add initiator 6-mercapto-1-hexanol MH (1777.3mg, 13.24mmol, 100eq) with a micro syringe, finally add 34mL of newly steamed toluene and tetrahydrofuran mixed solvent (4: 1), A solution is prepared and kept for use. Liquid B is pure δ-valerolactone, add pure δ-VL to bottle B with a syringe for future use.

[0048] To carry out the reaction, pump liquid A and liquid B into two 50mL syringes respecti...

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Abstract

The invention discloses a method for preparing mercapto-functionalized polyester using a micro-reaction device, which uses δ-valerolactone (VL) or ε-caprolactone (CL) as a reaction monomer, tin trifluoromethanesulfonate ( Sn(OTf) 2 ) is a metal complex catalyst, and the aliphatic alcohol with a mercapto group as a terminal group is a functional initiator, which is prepared in a microreactor. Compared with the prior art, the metal complex catalyst adopted in the present invention is simple and easy to obtain, has high catalytic activity, and the process of the present invention has strong operability and low cost. At the same time, the present invention has short polymerization process time, high reaction conversion rate, high polymer mercapto group introduction rate and high-precision control of polymerization reaction.

Description

technical field [0001] The invention belongs to the field of macromolecular chemistry, and in particular relates to a method for preparing mercapto-functionalized polyester by using a micro-reaction device. Background technique [0002] Mercapto-functionalized polyester has good biocompatibility and biodegradability, and can be bonded to metal surfaces. It plays an important role in the fields of chemistry and biology, mainly in three aspects: 1) modifying noble metal nanoparticles, 2 ) Click chemical reaction with double bonds, triple bonds or isocyanate groups to construct macromolecules with new structures, 3) Prepare biomimetic surfaces. Therefore, it is of great theoretical significance and application value to study the synthesis method of new mercapto-containing polymers. [0003] In recent decades, various methods for the synthesis of thiol-functionalized polyesters have been established. Synthetic steps can be divided into multi-step and one-step methods. The mul...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G63/688C08G63/85
CPCC08G63/6882C08G63/85
Inventor 郭凯冯卫杨朱宁胡欣方正张锴刘一寰黄卫军张子龙
Owner NANJING UNIV OF TECH
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