Preparation of functionalized polyesters and polycarbonates by copolymerization of polysubstituted six-membered ring lactones and methods for their post-modification

A polycarbonate and copolymerization technology, which is used in the preparation of functionalized polyesters and polycarbonates and their post-modification through the copolymerization of multi-substituted six-membered ring lactones, and can solve the modification of polyester or polycarbonate. Limited, low content of functional groups, complex process and other problems, to achieve the effect of abundant sites, changing physical and chemical properties, and easy availability of raw materials

Active Publication Date: 2022-03-18
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] 3. Copolymerization of olefinic monomers: Copolymerization of olefinic monomers with lactone or lactide monomers is rarely reported. The main reason is that the polymerization mechanisms of the two are completely different. The former is an addition reaction and the latter is a ring-opening reaction. , so it is more difficult to copolymerize these two monomers
[0007] The functional treatment of polyester or polycarbonate can expand the scope of use of polyester or polycarbonate, but the current post-modification method is complicated and requires the preparation of monomers with functional groups, while the content of functional groups is low , polyester or polycarbonate with limited modifiable sites

Method used

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  • Preparation of functionalized polyesters and polycarbonates by copolymerization of polysubstituted six-membered ring lactones and methods for their post-modification
  • Preparation of functionalized polyesters and polycarbonates by copolymerization of polysubstituted six-membered ring lactones and methods for their post-modification
  • Preparation of functionalized polyesters and polycarbonates by copolymerization of polysubstituted six-membered ring lactones and methods for their post-modification

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0059] The polymerization reaction adopts Schlenk technique. The glass instruments used were pumped and baked in an argon atmosphere for 3 times to achieve the purpose of removing water and oxygen. Draw 0.2mL tetrahydrofuran solution of sodium 2,6-di-tert-butyl-4-methylphenolate into the polymerization bottle after pumping and roasting, remove the THF solvent under reduced pressure, fill with argon, weigh the bottle, and obtain the polymerization The quality of sodium 2,6-di-tert-butyl-4-methylphenate (catalyst) in the bottle is 0.053 g. Add 0.323g EVL, 0.276gε-CL and 2.2mL of anhydrous toluene to another polymerization bottle that has been pumped and baked, stir and mix evenly, then add the uniformly mixed monomer solution into the polymerization bottle containing the catalyst, set React in an oil bath at 25°C for 5 hours. The resulting polymer was first diluted with THF and then precipitated once with ether. The precipitate was dissolved in THF and precipitated in n-hexan...

Embodiment 2

[0062] Other polymerization conditions were the same as in Example 1, and the polymerization reaction time was extended to 12 hours to obtain a crosslinked network of copolyester. The cross-linked network swells in THF solution and increases in volume. It shows that the cross-linked network of the polymer can be obtained by the in-situ one-step method of the copolymer.

Embodiment 3

[0064] Other polymerization conditions are the same as in Example 1, except that δ-VL is used as the polyester monomer. The yield of the obtained copolymer was 66%, the number average molecular weight of the copolymer measured by GPC was 12.1 kDa, and the molecular weight distribution was 2.99. It shows that different lactone monomers can also obtain polyesters with modifiable sites.

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Abstract

The invention discloses a method for preparing functionalized polyester and polycarbonate through multi-substituted six-membered ring lactone copolymerization and post-modification. The multi-substituted six-membered ring lactone 3-ethylene-6-vinyltetrahydro-2H-pyran-2-one, cyclic lactone, cyclocarbonate monomer and its derivatives are synthesized by organometallic salt Catalyst copolymerization is realized, reacting in an organic solvent at a certain temperature to prepare high molecular weight polyester or polycarbonate containing unsaturated side groups and six-membered lactone ring side groups, and through thioene click, alcoholysis, amine The unsaturated bond of its side chain or the side group of six-membered ring lactone can be post-modified by reactions such as hydrolysis. The invention is cheap and the preparation method is simple and easy to realize. The polyester or polycarbonate in the production area is used as the precursor of various functional polymer materials. Various properties of the polyester or polycarbonate can be further changed through modification, and the application is wide .

Description

technical field [0001] The present invention relates to a variety of organometallic salt catalysts: catalysts such as sodium phenate, potassium alkoxide, sodium alkoxide, aluminum alkyl, sodium borohydride, aryloxy rare earth, and a multi-substituted δ-valerolactone cyclic monomer: 3 -Ethylene-6-vinyltetrahydro-2H-pyran-2-one (EVL), and two highly active ring-opening comonomers: cyclic lactone monomer and cyclic carbonate monomer and their derivatives , and the synthesis and modification method of polyester or polycarbonate. Background technique [0002] Polyester has gradually become a research hotspot in recent years because of its excellent physical and mechanical properties, good biocompatibility and degradability. Among them, aliphatic polyester and polycarbonate are typical synthetic degradable materials. Aliphatic polyesters mainly include polylactone (polycaprolactone), polycarbonate and polyanhydride. Although polyester has good biocompatibility and degradability...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G63/08C08G63/84C08G63/83C08G64/02C08G64/30
CPCC08G63/08C08G63/823C08G64/30C08G64/0291
Inventor 倪旭峰朱志琦凌君
Owner ZHEJIANG UNIV
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