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Isotactic polylactic acid porous microspheres and preparation method thereof

A technology of porous microspheres and polylactic acid, which is applied in the preparation of microspheres, microcapsule preparations, etc., can solve the problem that polylactic acid microspheres cannot have both stereocrystalline and porous structures, and achieve easy movement and heat resistance Good, high porosity effect

Active Publication Date: 2019-12-31
北京朗净汇明生物科技有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The purpose of the present invention is to solve the problem that polylactic acid microspheres in the prior art cannot have both a full stereotype and a porous structure, and to provide a full stereotactic polylactic acid porous microsphere and a preparation method thereof

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  • Isotactic polylactic acid porous microspheres and preparation method thereof
  • Isotactic polylactic acid porous microspheres and preparation method thereof
  • Isotactic polylactic acid porous microspheres and preparation method thereof

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Embodiment 1

[0030] A full-stereopolylactic acid porous microsphere, the preparation method of which is as follows: firstly, the weight-average molecular weights with a mass ratio of 1:1 are both 0.5*10 4 g / mol of PLLA and PDLA were dissolved in DMF solvent at a temperature of 50°C to obtain a polylactic acid solution, wherein the sum of the weights of PLLA and PDLA per 100 mL of the polylactic acid solution was 1 g, and then the polylactic acid solution was heated at 10°C / min. The rate was reduced to a temperature of 5 °C to obtain all-stereopolylactic acid porous microspheres.

[0031] The finally obtained all-stereopolylactic acid porous microspheres are polylactic acid microspheres with all-stereoscopic crystal morphology and porous structure, which were characterized by SEM, XRD and DSC respectively. The results are as follows: figure 1 , figure 2 and image 3 As shown, the average particle size of all-stereopolylactic acid porous microspheres is 5 μm, the porosity is 10%, the heat...

Embodiment 2

[0039] An all-stereopolylactic acid porous microsphere, the preparation method of which is as follows: firstly, the weight-average molecular weights with a mass ratio of 1:1 are respectively 0.5*10 4 g / mol and 10.8*10 4 g / mol of PLLA and PDLA were dissolved in DMF solvent at a temperature of 65°C to obtain a polylactic acid solution, wherein the sum of the weights of PLLA and PDLA per 100 mL of the polylactic acid solution was 5 g, and then the polylactic acid solution was heated at 8°C / min. The rate of reducing the temperature to 0 °C to obtain all-stereopolylactic acid porous microspheres, followed by post-processing, the post-processing process is: using water to extract the DMF solvent in the all-stereopolylactic acid porous microspheres, washing and drying .

[0040] The finally prepared all-stereopolylactic acid porous microspheres are polylactic acid microspheres with all-stereoscopic crystal morphology and porous structure. The heat distortion temperature was 109 °C ...

Embodiment 3

[0042] A full-stereopolylactic acid porous microsphere, the preparation method of which is as follows: firstly, the weight-average molecular weights with a mass ratio of 1:1 are respectively 6.6*10 4 g / mol and 12.7*10 4 g / mol of PLLA and PDLA were dissolved in DMSO solvent at a temperature of 100 °C to obtain a polylactic acid solution, wherein the sum of the weights of PLLA and PDLA per 100 mL of polylactic acid solution was 12 g, and then the polylactic acid solution was heated to 4.5 °C / The rate of min is lowered to 20 °C to obtain all-stereopolylactic acid porous microspheres, which are then subjected to post-treatment. The post-treatment process is as follows: methanol is used to extract the DMSO solvent in the all-stereopolylactic acid porous microspheres, and washing and dry.

[0043] The finally prepared all-stereopolylactic acid porous microspheres are polylactic acid microspheres with a full-stereoscopic crystal form and a porous structure. The heat distortion tem...

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Abstract

The invention relates to isotactic polylactic acid porous microspheres and a preparation method thereof. The preparation method comprises the following steps: preparing: dissolving PLLA and PDLA in adimethyl series solvent at the temperature of T1 to obtain a polylactic acid solution; cooling the polylactic acid solution to a temperature T2 at a rate of 0.5-10 DEG C / min to obtain the isotactic polylactic acid porous microspheres, wherein T1 is greater than or equal to 50 DEG C, T2 is less than or equal to 25 DEG C, and the dimethyl series solvent is DMF, DMSO or DMAc. The finally prepared isotactic polylactic acid porous microspheres are polylactic acid microspheres of isotactic crystal forms and porous structures. The preparation method of the isotactic polylactic acid porous microspheres is simple and easy to implement and low in cost, and the solvent can be recycled and separated for use; the polylactic acid porous microsphere prepared by the method is wide in application range, and can be used as a drug controlled-release material, a cell carrier, cosmetics, plastics, a coating additive and the like.

Description

technical field [0001] The invention belongs to the technical field of biofunctional polymer materials, and relates to an all-stereopolylactic acid porous microsphere and a preparation method thereof. Background technique [0002] Polylactic acid is a green polymer material polymerized from starch-fermented lactic acid as raw material. It has the advantages of degradability and good biocompatibility. application prospects. However, the poor heat resistance of ordinary polylactic acid materials (the heat distortion temperature is about 60 °C) and the defects of easy hydrolysis hinder its further development and promotion. Stereocomplex polylactic acid is a kind of polylactic acid with high heat resistance and hydrolysis resistance prepared by mixing PLLA and PDLA through a special treatment process, which has attracted widespread attention in recent years. Porous microspheres have attracted more and more attention in the fields of adsorption and separation, heterogeneous ca...

Claims

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Application Information

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IPC IPC(8): B01J13/02B01J13/04
CPCB01J13/02B01J13/04
Inventor 马博谋何勇王学利李乃强俞建勇
Owner 北京朗净汇明生物科技有限公司
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