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Thermosensitive poly(lactic acid-valine) material and preparation method thereof

A valine and temperature-sensitive technology, which is applied in the field of temperature-sensitive poly(lactic-valine) materials and their preparation, can solve the problem of not being able to have both biocompatibility, biodegradability and temperature-sensitive properties, single, etc. problem, to achieve the effect of excellent biodegradability and excellent biocompatibility

Inactive Publication Date: 2017-09-05
HEBEI UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The present invention provides a temperature-sensitive poly(lactic acid-valine) to solve the technical problem that the polymer materials prepared by modification cannot simultaneously have biocompatibility, biodegradability and temperature-sensitive properties in the prior art. Material and preparation method thereof, the polymer material of the present invention is a single polymer, rather than a mixture, a blend, or a graft of various polymers, and the polymer material has excellent biocompatibility, biodegradability Sexuality and temperature sensitivity

Method used

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  • Thermosensitive poly(lactic acid-valine) material and preparation method thereof
  • Thermosensitive poly(lactic acid-valine) material and preparation method thereof
  • Thermosensitive poly(lactic acid-valine) material and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] (1) Dehydration stage

[0042] In a microwave reactor (such as CEM microwave synthesizer, DISCOVER SP), put 5.0 g of lactic acid in a 100 mL long-necked flask, and put a magnetic stirring bar. React at a vacuum of 0.06 MPa and a temperature of 120° C. for 30 minutes to remove free water in the reaction solution. Then, add 0.6% SnCl in the reaction flask 2 and p-toluenesulfonic acid as a reaction catalyst, reacted for 45 minutes at a vacuum of 0.08MPa and a temperature of 160°C, SnCl 2 And the addition of p-toluenesulfonic acid is 0.6%, calculated with the mass of lactic acid.

[0043] (2) Polymerization stage

[0044] 6.0 g of valine was added, and the reaction was continued at a vacuum of 0.08 MPa and a temperature of 170° C. for 30 minutes.

[0045] (3) Insulation stage

[0046] The reaction was maintained for 60 minutes at a vacuum of 0.08 MPa and a temperature of 160°C. After the reaction temperature dropped to 50°C, fully dissolve it with 6mL of anhydrous met...

Embodiment 2

[0053] (1) Dehydration stage

[0054] In a microwave reactor (such as CEM microwave synthesizer, DISCOVER SP), put 5.0 g of lactic acid in a 100 mL long-necked flask, and put a magnetic stirring bar. React at a vacuum of 0.04 MPa and a temperature of 110° C. for 35 minutes to remove free water in the reaction solution. Then, add 0.6% SnCl in the reaction flask 2 With p-toluenesulfonic acid as a reaction catalyst, the vacuum was 0.06MPa, and the temperature was 158°C for 50 minutes.

[0055] (2) Polymerization stage

[0056] 6.0 g of valine was added, and the reaction was continued at a vacuum of 0.06 MPa and a temperature of 165° C. for 40 minutes.

[0057] (3) Insulation stage

[0058] The reaction was maintained for 70 minutes at a vacuum of 0.06 MPa and a temperature of 158°C. After the reaction temperature drops to 40°C, fully dissolve it with 6mL of anhydrous methanol, and then add it dropwise into 160mL of diethyl ether under stirring, a yellowish precipitate precip...

Embodiment 3

[0063] (1) Dehydration stage

[0064] In a microwave reactor (such as CEM microwave synthesizer, DISCOVER SP), put 5.0 g of lactic acid in a 100 mL long-necked flask, and put a magnetic stirring bar. React for 40 minutes at a vacuum of 0.05 MPa and a temperature of 130° C. to remove free water in the reaction solution. Then, add 0.6% SnCl in the reaction flask 2 and p-toluenesulfonic acid as a reaction catalyst, and reacted for 58 minutes at a vacuum of 0.07 MPa and a temperature of 168°C.

[0065] (2) Polymerization stage

[0066] 6.0 g of valine was added, and the reaction was continued at a vacuum of 0.07 MPa and a temperature of 172° C. for 50 minutes.

[0067] (3) Insulation stage

[0068] The reaction was maintained for 65 minutes at a vacuum of 0.07 MPa and a temperature of 164°C. After the reaction temperature drops to 45°C, fully dissolve it with 6mL of anhydrous methanol, and then add it dropwise into 160mL of diethyl ether under stirring, and a yellowish precip...

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Abstract

The invention discloses a thermosensitive poly (lactic acid-valine) material, and belongs to the field of thermosensitive polymers in smart materials. Poly (lactic acid-valine) is formed by a structural unit which is as shown in a formula (I); the poly (lactic acid-valine) is a random copolymer; the molecular weight of the poly (lactic acid-valine) is 6,000 to 15,000; in the formula (I), x:y=1:(0.3 to 0.8). The invention also discloses a preparation method of the thermosensitive poly (lactic acid-valine) material. The thermosensitive poly (lactic acid-valine) material prepared by the invention not only has a thermosensitive characteristic, but also integrates excellent biocompatibility and excellent biodegradability.

Description

technical field [0001] The invention belongs to the field of temperature-sensitive polymers in intelligent materials, and relates to a molecular structure design and a preparation method of a polymer material with good biocompatibility and temperature-sensitive properties, in particular to a temperature-sensitive poly(lactic acid) - valine) material and preparation method thereof, the polymer material itself is a single polymer, rather than a mixture, graft, or blend of two or more polymers in the modification method. Background technique [0002] As one of the most important smart materials, temperature-sensitive polymers refer to materials with reversible response characteristics to the external environment temperature. The temperature-sensitive properties of polymer materials are actually a relative balance between the hydrophilicity and hydrophobicity of the macromolecular chain. In other words, there are hydrophilic groups and hydrophobic groups on the main chain of the...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G63/685C08G63/78
CPCC08G63/6852C08G63/78
Inventor 邓奎林徐俊连杨震赵漫宋计花郑畅范智慧
Owner HEBEI UNIVERSITY
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