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Preparation method of lactone and lactide block copolymer

A technology of block copolymer and lactide, which is applied to the preparation field of lactone and lactide block copolymer, can solve the problems such as difference in activity of monomers, difficulty in copolymerization, etc., so as to reduce the difference in activity, simplify the route, and reduce the monomer activity. High conversion rate

Active Publication Date: 2022-03-01
深圳市鑫元素新材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] In view of the above deficiencies in the prior art, the object of the present invention is to provide a method for preparing a lactone and lactide block copolymer, aiming at solving the problem of the existing lactone and lactide due to the difference in monomer activity during ring-opening polymerization. Difficult to reconcile issues

Method used

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  • Preparation method of lactone and lactide block copolymer
  • Preparation method of lactone and lactide block copolymer
  • Preparation method of lactone and lactide block copolymer

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0063]Example 1: In a pre-dried three-necked reaction flask with a stirring bar under the protection of nitrogen, add 400 mL of toluene, 1.08 g (0.01 mol) of benzyl alcohol, 144 g (1.0 mol) of lactide, 2,6- 1.5 g (0.01 mol) of dimethyl-4-dimethylaminopyridine and 2.42 g (0.01 mol) of triphenylborane, the reaction solution was heated to 60° C. and kept for 1 hour to complete the first-stage polymerization. Afterwards, 114 g (1.0 mol) of ε-caprolactone was added to the polymerization system to continue block copolymerization, and the reaction ended after 8 hours. The reaction product was reprecipitated in methanol, then filtered, and dried to obtain a white cyclic diblock copolymer PLA-b-PCL was obtained with a yield of 92%, a number average molecular weight of 36,300 g / mol by gel permeation chromatography (GPC) in tetrahydrofuran solvent, and a molecular weight distribution of 1.42.

Embodiment 2

[0064] Example 2: In the pre-dried three-necked reaction flask with stirring bar under the protection of nitrogen, add 400 mL of xylene, 1.08 g (0.01 mol) of benzyl alcohol, 116 g (1.0 mol) of glycolide, 2,6 - 1.5 g (0.01 mol) of dimethyl-4-dimethylaminopyridine and 2.42 g (0.01 mol) of triphenylborane, the reaction solution was heated to 80° C. and kept for 1 hour to complete the first-stage polymerization. Afterwards, 114 g (1.0 mol) of ε-caprolactone was added to the polymerization system to continue block copolymerization, and the reaction ended after 5 hours. The reaction product was reprecipitated in methanol, then filtered, and dried to obtain a white cyclic diblock copolymer The yield of PGA-b-PCL was 88%, the number average molecular weight of gel permeation chromatography (GPC) in tetrahydrofuran solvent was 33,600 g / mol, and the molecular weight distribution was 1.48.

Embodiment 3

[0065] Example 3: In the pre-dried three-neck reaction flask with stirring bar under the protection of nitrogen, add 400 mL of toluene, 0.74 g (0.01 mol) of butanol, 144 g (1.0 mol) of lactide, 2,6-di Methyl-4-dimethylaminopyridine 1.5g (0.01mol) and tris(pentafluorophenyl)borane 5.48g (0.01mol), the reaction solution was heated to 60°C and maintained for 1 hour to complete the first stage polymerization. Afterwards, 114 g (1.0 mol) of ε-caprolactone was added to the polymerization system to continue block copolymerization, and the reaction ended after 6 hours. The reaction product was reprecipitated in methanol, then filtered, and dried to obtain a white cyclic diblock copolymer The product PLA-b-PCL has a yield of 85%, the number average molecular weight of the gel permeation chromatography (GPC) in tetrahydrofuran solvent is 38,500 g / mol, and the molecular weight distribution is 1.53.

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Abstract

The invention discloses a preparation method of a lactone and lactide block copolymer. The method comprises the following steps: adding a solvent (if necessary), an alcohol initiator, a first monomer and an organic Lewis acid-base pair with steric hindrance into a pre-dried reactor with a stirring function under the protection of an inert atmosphere, and carrying out a polymerization reaction; adding a second monomer into the reaction system, and continuously carrying out polymerization reaction to obtain a block copolymer; the first monomer is lactide, and the second monomer is lactone; or, the first monomer is lactone, and the second monomer is lactide. The lactone and lactide block copolymer is prepared by adopting a steric hindrance organic Lewis acid-base pair one-pot method. The steric hindrance organic Lewis acid-base pair synergistically activates an active center and a monomer in a system, so that the activation energy of a ring-opening reaction is greatly reduced, the difference of monomer activity is reduced, and the problem that lactone and lactide are difficult to copolymerize due to great difference of monomer activity during ring-opening polymerization is solved.

Description

technical field [0001] The invention relates to the technical field of polymer materials, in particular to a preparation method of a lactone and lactide block copolymer. Background technique [0002] Aliphatic polyesters have good biocompatibility and biodegradability, and have been widely and deeply studied in the fields of biomedicine, drug delivery, packaging, agriculture, etc., and are a class of polymer materials with great development prospects. For example, polyglycolide (trade name: Dexon) was first used in the medical field in 1962 as an absorbable suture for surgical implantation and tissue repair (R.K.Kulkarni, K.C.Pani, C.Neuman and F.Leonard, Arch. Surg., 1966, 93, 839–843.). A few years later, people further developed a copolymer composed of glycolide and lactide: poly[(L-lactide (8%)-co-glycolide (92%)], which can be absorbed by the human body The degradable surgical suture material has more superior mechanical properties and biocompatibility, and a more sui...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G63/08C08G63/06C08G63/78C08G63/81C08G63/84C08G63/87
CPCC08G63/08C08G63/06C08G63/81C08G63/78C08G63/823Y02W90/10
Inventor 陈建弛
Owner 深圳市鑫元素新材料科技有限公司