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Preparation method of polyester-polycarbonate-polyester multi-block copolymer

A multi-block copolymer and polycarbonate technology, applied in the field of polymer materials, can solve problems such as narrow dispersion, and achieve the effects of narrow molecular weight distribution, easy operation and simple structure

Active Publication Date: 2015-12-16
NANJING UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Nowadays, a large number of organic acids and bases have been developed to catalyze ring-opening polymerization, but there is often no organic catalyst that can catalyze all cyclic lactones and cyclic carbonates well and is suitable for ring-opening polymerization. The reaction process is well controlled
Therefore, it is a real challenge and difficulty to adopt the "one-pot method" to precisely prepare polyester-polycarbonate multi-block copolymers with narrow dispersion

Method used

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  • Preparation method of polyester-polycarbonate-polyester multi-block copolymer
  • Preparation method of polyester-polycarbonate-polyester multi-block copolymer
  • Preparation method of polyester-polycarbonate-polyester multi-block copolymer

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] Add δ-valerolactone (162 μL, 1.8 mmol), DPP (15.0 mg, 60 μmol) into a solution with 2 mL of CH 2 Cl 2 in the polymerization tube. The initiator benzyl alcohol (6.24 μL, 60 μmol) was added into the reaction system to start the polymerization reaction, and the polymerization reaction was carried out at room temperature, and the whole system was under the protection of argon. After the first polymerization reaction was carried out in magnetic stirring for 45 minutes, 1 HNMR detected that δ-valerolactone was substantially consumed, and trimethylene carbonate (183.6 mg, 1.8 mmol) was added to the reaction mixture to start the second block polymerization. When the second block polymerization was carried out for 15 hours, 1 HNMR detection of the second monomer trimethylene carbonate is also basically consumed, then add DBU (17.8 μ L, 120 μ mol) to the mixture, after magnetic stirring for about 10 minutes, add lactide (260 mg, 1.8 mmol) to start the third block polymerizati...

Embodiment 2

[0042] Add ε-caprolactone (191 μL, 1.8 mmol), MSA (4.0 μL, 60 μmol) into a solution with 2 mL of CH 2 Cl 2 in the polymerization tube. The initiator benzyl alcohol (6.24 μL, 60 μmol) was added into the reaction system to start the polymerization reaction, and the polymerization reaction was carried out at room temperature, and the whole system was under the protection of argon. After the first polymerization reaction was carried out in magnetic stirring for 1.5 hours, 1 HNMR detected that δ-valerolactone was substantially consumed, and trimethylene carbonate (183.6 mg, 1.8 mmol) was added to the reaction mixture to start the second block polymerization. When the second block polymerization was carried out for 3 hours, 1 HNMR detection of the second monomer trimethylene carbonate is also basically consumed, then add DBU (17.8 μ L, 120 μ mol) to the mixture, after magnetic stirring for about 10 minutes, add lactide (260 mg, 1.8 mmol) to start the third block polymerization. ...

Embodiment 3

[0044] Add β-butyrolactone (144 μL, 1.8 mmol), TfOH (5.14 μL, 60 μmol) 2 Cl 2 in the polymerization tube. The initiator benzyl alcohol (6.24 μL, 60 μmol) was added into the reaction system to start the polymerization reaction, and the polymerization reaction was carried out at room temperature, and the whole system was under the protection of argon. After the first polymerization reaction was carried out under magnetic stirring for 5 hours, 1 HNMR detected that δ-valerolactone was substantially consumed, and trimethylene carbonate (183.6 mg, 1.8 mmol) was added to the reaction mixture to start the second block polymerization. When the second block polymerization was carried out for 0.5 hours, 1 HNMR detection of the second monomer trimethylene carbonate is also basically consumed, then add DBU (17.8 μ L, 120 μ mol) to the mixture, after magnetic stirring for about 10 minutes, add lactide (260 mg, 1.8 mmol) to start the third block polymerization. But after 3 hours of reac...

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Abstract

The invention discloses a preparation method of polyester-polycarbonate-polyester multi-block copolymer and belongs to the technical field of high molecular materials. The preparation method comprises the steps that a multi-block polymerization is completed through a 'one-pot method', in another word, a Bronsted acid catalyst sequentially catalyzes cyclic lactone and cyclic carbonate for achieving ring opening polymerization, then a preset amount of tertiary amine R<3>N which is excessive relative to acid is input, wherein conjugate acid R<3>N<+>-H<delta+> formed by alkali which is equal to acid in a system in proton number serves as a hydrogen bond donor, spare alkali serves as a hydrogen bond receptor, ring opening polymerization of lactide which is finally input is catalyzed in a bifunctional mode, and the polyester-polycarbonate-polyester triple-block copolymer is finally synthesized. The preparation method has the advantages that the catalyst is simple in structure and easy to obtain, the reaction is mild and high in efficiency, the 'one-pot method' is easy and convenient to operate, the whole polymerization reaction exhibits active characteristics, the polymer molecular weight is controllable, and molecular weight distribution is narrow.

Description

technical field [0001] The invention belongs to the technical field of polymer materials, and in particular relates to a catalytic method for precisely preparing a polyester-polycarbonate-polyester multi-block copolymer with a narrow polydispersity. Background technique [0002] Polyester and polycarbonate materials have far-reaching research significance and broad industrial application prospects because of their biodegradability and environmental friendliness. At the same time, they have good biocompatibility, have no obvious toxicity and rejection to organisms, and can be well applied in the field of biomedicine. [0003] Ring-opening polymerization is a method of preparing polyester and polycarbonate polymers. In the early ring-opening polymerization reaction, metal catalysts such as organotin salts, organozinc salts and organoaluminum salts are generally used as catalysts, such as JP0124651, CN1544504 ​​and CN1814644. It has been extensively studied in ring-opening po...

Claims

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Application Information

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IPC IPC(8): C08G63/64C08G63/87
Inventor 郭凯王鑫李振江崔赛德王慧颖智绪
Owner NANJING UNIV OF TECH
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