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Polylactic acid composition as well as self-assembling body and preparation method thereof

A technology of self-assembly and composition, applied in the field of polylactic acid composition, can solve the problems of incapable of stable form, small size of self-assembly, unstable structure, etc., and achieve the effects of large size, wide application and stable structure

Inactive Publication Date: 2019-06-14
EAST CHINA UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] The technical problem to be solved by the present invention is to overcome the use of stereocomplex crystallization of polylactic acid in the prior art to obtain a stable shape or the size of the self-assembled body obtained by homogeneous crystallization of polylactic acid is small, the structure is unstable and the The defects of poor performance limit the application in biology and materials, and provide a polylactic acid composition, its self-assembly body and its preparation method

Method used

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  • Polylactic acid composition as well as self-assembling body and preparation method thereof
  • Polylactic acid composition as well as self-assembling body and preparation method thereof
  • Polylactic acid composition as well as self-assembling body and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0072] 1. Synthesis of triblock copolymer PLLA-b-PDMS-b-PLLA

[0073] Purification of L-lactide: Purify the raw material L-lactide 3 times with ethyl acetate, mix 60g of L-lactide with ethyl acetate with a mass ratio of 75%, and make L-lactide in a water bath at 75°C -Lactide is completely dissolved within 5 minutes, cooled from room temperature to normal temperature and placed in the refrigerator for more than 2 hours, then the ethyl acetate in which impurities have been dissolved is filtered off, and purified three times according to the above method, and finally the purified L-lactide Put it in a cold trap device to vacuum for 48 hours, remove all solvents, and store it in a glove box refrigerator.

[0074] Weighing was carried out under the protection of nitrogen in the glove box, and 5 g of L-lactide and 1000 μl of PDMS (M w =600~850), 500μl stannous octoate, 16ml solvent toluene, put on a rubber stopper, take it out from the glove box, place it in an oil bath at 130°C a...

Embodiment 2

[0086] Synthesis of three-block copolymer PLLA-b-PDMS-b-PLLA and PDLA polymer and the number average molecular weight of the polymer obtained are the same as in Example 1

[0087] 1. Preparation of assembly solution of triblock copolymer and homopolymer PDLA

[0088] Weigh 15mg triblock copolymer and 10mg PDLA polymer powder and mix and place in a 20ml screw bottle, then measure tetrahydrofuran (THF) and n-Hexane with a volume ratio of 8:2 (THF / n-Hexane, v / v) The n-Hexane solvent was placed in a beaker and mixed evenly, and then the mixed solution was transferred to the above-mentioned neck flask to prepare a mixed solution with a concentration of 2 mg / ml.

[0089] 2. Synergistic crystallization of stereocomplexation induced self-assembly of triblock polylactic acid copolymer

[0090] The mixed solution with the above solvent ratio was ultrasonically mixed for 30 min, annealed at 65 °C for 40 min, then slowly cooled at 25 °C for 2 h, and finally placed in a 30 °C incubator fo...

Embodiment 3

[0093] The preparation method of the triblock copolymer PLLA-b-PDMS-b-PLLA is the same as that of Example 1 with the obtained number average molecular weight.

[0094] 1. Synthesis of PDLA polymer

[0095] The purification of D-lactide was the same as in Example 1.

[0096] Weigh the material under the protection of nitrogen in the glove box, add 2.88g of purified D-lactide, 400μl methyl lactate, 288μl stannous octoate, and 12ml solvent toluene into the three-necked flask, plug it with a rubber stopper, take it out of the glove box and place it The reaction was stirred at 400 rpm in an oil bath at 130° C. for 3.5 h. Use 150ml of anhydrous methanol stored in the refrigerator for precipitation, suction filtration to obtain a white solid, and finally place it in a cold trap device for 48 hours to vacuumize, remove all solvents, and obtain a PDLA polymer with a molecular weight of 11043 and a molecular weight dispersion width of 1.24 things.

[0097] 2. Preparation of assembly ...

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Abstract

The invention discloses a polylactic acid composition as well as a self-assembling body and a preparation method thereof. The polylactic acid composition is prepared from the following components: A triblock copolymer poly(L-lactide)-b-polydimethyl siloxane-b-poly(L-lactide) and poly(D-lactide); the two components are mixed according to the mass ratio ranging from (1 to 1.8) to (1.8 to 1), whereinthe number average molecular weight of the triblock copolymer is 10000 to 20000 and the number average molecular weight of the poly(D-lactide) is 10000 to 50000. The composition is commonly dissolvedinto an organic solvent to prepare a mixed solution and then is annealed, subjected to cooling crystallization, and then is subjected to constant-temperature self-assembling to form a two-dimensionalsheet-shaped rhombus edge frame structure; the self-assembling body is obtained through a stereoscopic compound crystallization manner, has the advantages of uniform distribution, larger size and more stable structure, has more excellent performance and can be widely applied to the fields of biology and materials.

Description

technical field [0001] The invention relates to a polylactic acid composition, its self-assembly body and a preparation method. Background technique [0002] As a bio-based, biodegradable polymer material, polylactic acid (PLA) has good biodegradability and biocompatibility, and is widely used in the fields of biomedicine and materials. The lactide molecule contains a chiral carbon, which exists in the form of D-lactide, L-lactide and meso, and various polylactic acids can be prepared: DL-lactide, levo-lactide Lactic acid PLLA, dextro-racemic polylactic acid PDLA, the blend system of PLLA and PDLA can obtain stereocomplex crystals, which have high melting point, high strength and hydrolysis resistance compared with homogeneous crystalline PLA materials, and are widely used in biomedical fields The application is extremely wide. [0003] 2D sheet-like structures have attracted much attention due to their ultrathin and flat morphology structures, for example, graphene, boron...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08L67/04C08L83/10C08G63/695C08J3/00
Inventor 沈学宁张文凭唐颂超姚远华启侠庞懿窈吴单
Owner EAST CHINA UNIV OF SCI & TECH
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