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Method of preparing polymer porous beads based on liquid drop settling and freezing technology

A technology of polymer and droplet, applied in the field of preparation of polymer porous beads, can solve the problems of uneven size of microspheres, low size distribution of spheres, etc., and achieve the effect of simple and easy preparation method

Inactive Publication Date: 2015-01-14
EAST CHINA UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there are some shortcomings in the above-mentioned methods. The diameter of the polylactic acid microspheres used in the drug release carrier is limited to about 250 microns, and the size of the microspheres prepared by the solvent evaporation method is not uniform. The main problem of the spray drying method is the formation of balls during the spraying process. low probability and wide size distribution
So far, the preparation of large-diameter and uniform porous beads by droplet sedimentation freezing method has not been reported.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Using 11 grams of dimethyl sulfoxide as a solvent and 0.55 grams of polylactic acid as a solute, a polylactic acid solution was formed by magnetic stirring at a constant temperature of 80 degrees Celsius. Then transfer the polylactic acid solution to the syringe, and under the action of the syringe pump, the solution droplet drops through the syringe into the 0°C condenser tube, and then the droplet is precipitated from top to bottom in the precipitation solution of ethanol and water 1:1 Freeze crystallization to form solid pellets, collect porous polymer beads at the bottom, wash away dimethyl sulfoxide with deionized water, and freeze-dry to obtain porous polymer beads with large diameters.

[0017] The obtained polymer porous beads had a diameter of 1.50 mm and a porosity of 95.43%.

Embodiment 2

[0019] Using 11 grams of dioxane as a solvent and 1.1 grams of polycaprolactone as a solute, a polylactic acid solution was formed by magnetic stirring at a constant temperature of 80 degrees Celsius. Then transfer the polylactic acid solution to the syringe, and under the action of the syringe pump, the solution droplet drops through the syringe into the 0°C condenser tube, and then the droplet is precipitated from top to bottom in the precipitation solution of ethanol and water 1:1 Freeze crystallization to form solid pellets, collect porous polymer beads at the bottom, wash away dimethyl sulfoxide with deionized water, and freeze-dry to obtain porous polymer beads with large diameters.

[0020] The obtained polymer porous beads had a diameter of 2.34 mm and a porosity of 95.64%.

Embodiment 3

[0022] Using 11 grams of dimethyl sulfoxide as a solvent and 1.1 grams of polylactic acid as a solute, a polylactic acid solution was formed by magnetic stirring at a constant temperature of 80 degrees Celsius. Then transfer the polylactic acid solution to the syringe, and under the action of the syringe pump, the solution droplet drops through the syringe into the 0°C condenser tube, and then the droplet is precipitated from top to bottom in the precipitation solution of ethanol and water 1:1 Freeze and crystallize to form solid pellets, collect the polymer porous beads at the bottom, wash away dimethyl sulfoxide with a 1:1 solution of ethanol and water, and freeze-dry to obtain large diameter polymer porous beads.

[0023] The resulting polymer porous beads had a diameter of 1.71 mm and a porosity of 89.38%.

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Abstract

The invention discloses a method of preparing polymer porous beads from polymer organic liquids through liquid drop settling and freezing. The method comprises the following steps: injecting polymer organic liquids with different concentrations into settling and freezing liquid at a certain temperature by virtue of an injecting device, and enabling liquid drops to freeze and crystallize from top to bottom to form polymer porous beads; collecting the polymer porous beads at the bottom, and freeze-drying after eluting the polymer porous beads by virtue of a de-eluting agent, wherein the velocity of the liquid drops of the injected liquid can be regulated by virtue of an injecting pump, and the temperature of the settling and freezing liquid is controlled by virtue of an external low-temperature circulating slot. The method disclosed by the invention is simple and easy to implement, green and environmentally friendly and capable of obtaining the polymer porous beads with diameters of 1.50-2.95 millimeters.

Description

technical field [0001] The invention relates to a preparation method of polymer porous beads, in particular to using polymer as a solute, dimethyl sulfoxide or dioxane as a solvent, forming it through droplet settling and freezing, directional crystallization, washing and drying , A method of preparing a polymeric porous bead material. Background technique [0002] Porous polymer materials have the advantages of high porosity, low density, large specific surface area, and good material transport capacity, and have high application value in adsorption and separation, catalysis, biological tissue engineering, and environmental science. big interest. There have been many reports on the preparation methods of polymer porous materials, such as using supercritical fluid, air blowing, colloidal template assembly, polymer precursor template method and high internal phase emulsion template method. At the same time, granular biomaterials have become a research hotspot in recent year...

Claims

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Application Information

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IPC IPC(8): C08J9/00C08L67/04
Inventor 章圣苗陈建定卢贞肖晨晨张芳宁王彦华朱芸杨华清储叶倩
Owner EAST CHINA UNIV OF SCI & TECH
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