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A kind of 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 effect of simple operation and simple structure.

Active Publication Date: 2017-11-07
NANJING TECH UNIV
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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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  • A kind of preparation method of polyester-polycarbonate-polyester multi-block copolymer
  • A kind of preparation method of polyester-polycarbonate-polyester multi-block copolymer
  • A kind of preparation method of polyester-polycarbonate-polyester multi-block copolymer

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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 H NMR 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 H NMR 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 first Tri-block polyme...

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 H NMR 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 H NMR 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 first Tri-block polymeriza...

Embodiment 3

[0044] Add β-butyrolactone (144 μL, 1.8 mmol), TfOH (5.14 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 under magnetic stirring for 5 hours, 1 H NMR 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 H NMR 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 first Tri-block poly...

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Abstract

The invention discloses a preparation method of a polyester-polycarbonate-polyester multi-block copolymer, belonging to the technical field of polymer materials. In the present invention, the multi-block polymerization is accomplished by the "one-pot method", that is, the Bronsted acid catalyst sequentially catalyzes the ring-opening polymerization of cyclic lactones and cyclic carbonates, and then puts in a preset relative acid excess tertiary amine (R3N: ), wherein the acid in the system forms the conjugate acid R3N+-Hδ+ of the base itself as a hydrogen bond donor, and the excess base acts as a hydrogen bond acceptor, and the bifunctional catalyzes the ring-opening of the lactide that is finally put into Polymerization to finally synthesize polyester‑polycarbonate‑polyester triblock copolymers. The invention has the following advantages: the structure of the catalyst is simple and easy to obtain, the reaction is mild and efficient, the "one-pot method" is easy to operate, the whole polymerization reaction is active, the molecular weight of the polymer is controllable and the 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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Patent Type & Authority Patents(China)
IPC IPC(8): C08G63/64C08G63/87
Inventor 郭凯王鑫李振江崔赛德王慧颖智绪
Owner NANJING TECH UNIV
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