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Copolymer of fibroin and poly L-lactic acid, solid phase polymerization preparation method and application thereof

A technology of silk protein and solid-state polymerization, which is applied in the field of copolymers of silk protein and poly-L-lactic acid and its preparation, can solve the problems of no research reports, etc., and achieve the effects of simple process, short production cycle and low product cost

Inactive Publication Date: 2009-06-03
NANJING FORESTRY UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, there is no research report on this aspect at home and abroad

Method used

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  • Copolymer of fibroin and poly L-lactic acid, solid phase polymerization preparation method and application thereof
  • Copolymer of fibroin and poly L-lactic acid, solid phase polymerization preparation method and application thereof
  • Copolymer of fibroin and poly L-lactic acid, solid phase polymerization preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0051] Add 90% aqueous solution of L-lactic acid into the reaction kettle, dehydrate at 180°C, first dehydrate under normal pressure for 4 hours, then depressurize to 100 mmHg for 4 hours, and finally dehydrate at 10 mmHg for 6 hours to obtain the molecular weight 2000 L-lactic acid oligomers.

[0052] After dehydration, the SnCl 2 2H 2 O / p-toluenesulfonic acid catalyst system (SnCl 2 2H 2 The molar content of O accounts for 50% of the entire catalyst system) into the prepolymer, SnCl 2 2H 2 The amount of O used is 0.4 wt% of the L-lactic acid oligomer. The pressure of the system was gradually reduced to 0 mmHg (manometer reading), and the reaction temperature was raised to 200° C. to carry out the polymerization reaction. As the reaction progressed, lactide monomers began to appear and reflux, the temperature of the condensing reflux device was controlled at 90°C, and the reactant gradually became viscous. The polymerization reaction was stopped after 4 hours to obtain...

Embodiment 2

[0056] Add 85% aqueous solution of L-lactic acid into the reaction kettle and dehydrate at 140°C. First dehydrate the mixed monomers under normal pressure for 1 hour, then reduce the pressure to 100 mmHg for 4 hours, and finally dehydrate for 1 hour at 50 mmHg to obtain L-lactic acid oligomers with a molecular weight of 500.

[0057] After dehydration, the SnCl 2 / p-toluenesulfonic acid catalyst system (SnCl 2 The molar content accounts for 1% of the entire catalyst system) is added to the prepolymer, SnCl 2The dosage is 0.01wt% of the L-lactic acid oligomer. The pressure of the system was gradually reduced to 1 mm Hg, the reaction temperature was raised to 180° C., and the condensing reflux temperature was 50° C. to carry out the polymerization reaction. As the reaction progressed, the lactide monomer was produced and began to reflux, and the reactant gradually became viscous. The reaction time was 20 hours to obtain poly-L-lactic acid with a molecular weight of 13,000. ...

Embodiment 3

[0061] Add 90% aqueous solution of L-lactic acid into the reaction kettle, and dehydrate at 150°C. First dehydrate the monomer under normal pressure for 2 hours, then reduce the pressure to 150 mmHg for 2 hours, and finally dehydrate for 6 hours at 10 mmHg to obtain L-lactic acid oligomers with a molecular weight of 1500.

[0062] After dehydration, the SnCl 2 2H 2 O / octanoic acid catalyst system (SnCl 2 2H 2 The molar content of O accounts for 60% of the entire catalyst system) into the prepolymer. SnCl 2 2H 2 The amount of O used is 0.80 wt% of the L-lactic acid oligomer. The pressure of the system was gradually reduced to 10 mm Hg, the reaction temperature was 180° C., and the condensation reflux temperature was 20° C. As the reaction progressed, lactide monomers began to appear and reflux, and the reactant gradually became viscous. The reaction was stopped after 25 hours to obtain poly-L-lactic acid with a molecular weight of 18,000.

[0063] Then add silk protein...

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Abstract

The invention discloses a copolymer of fibroin and a poly L-lactic acid. The molecular weight of the copolymer having the structure is 5,000-200,000, and the mass ratio of the fibroin chain segment and the poly L-lactic acid chain segment is 1 / 99-99 / 1. The invention also discloses a solid phase polymerization preparation method thereof and the application thereof in biomedical materials. The invention adopts the method of direct polymerization, the copolymer of fibroin and the poly L-lactic acid is prepared through main body melt / solid phase polymerization, and solvent is not used in the synthesis technique; therefore, the invention has the advantages that the process is simple, the product cost is low, the production cycle is short, and no pollution is generated. Through the invention, copolymer of fibroin and poly L-lactic acid with different number average molecular weight can be prepared, with the molecular weight of 5,000-200,000. Copolymer of fibroin and poly L-lactic acid prepared through the invention can improve the hydrophilicity, the biocompatibility and the cellualar affinity of lactic acid material and control the degradation speed of the material.

Description

Technical field: [0001] The invention belongs to the technical field of polymer materials, and in particular relates to a copolymer of silk protein and poly-L-lactic acid, a preparation method and application thereof. Background technique: [0002] Polylactic acid (PLA) is a biodegradable and absorbable polymer material with good biocompatibility. It has the advantages of good biocompatibility, degradation products can participate in the metabolism of the human body, and low toxicity. It has been widely used in tissue engineering and other biomedical fields. However, polylactic acid also has performance defects, such as greater brittleness, lower mechanical strength, and difficulty in controlling the degradation cycle. In addition, PLA is a hydrophobic polymer with poor adhesion to cells. Pure polylactic acid as a tissue engineering material will cause some mild inflammatory reactions after implantation into the organism, so the polylactic acid material must be modified. ...

Claims

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Application Information

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IPC IPC(8): C08H1/00C08G63/685
Inventor 高勤卫李明子周壮丽吴国成
Owner NANJING FORESTRY UNIV
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