Method for preparing polymer porous microspheres through mixed phase separation

A technology of porous microspheres and polymers, applied in the direction of microsphere preparation, microcapsule preparation, etc., can solve the problems of reducing the porosity and strength of microspheres, and achieve the effects of wide size control range, simple preparation method, and wide application range

Inactive Publication Date: 2012-06-20
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This method utilizes non-solvent-induced phase separation to induce the formation of a porous structure. Therefore, a dense skin layer and a f

Method used

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  • Method for preparing polymer porous microspheres through mixed phase separation
  • Method for preparing polymer porous microspheres through mixed phase separation

Examples

Experimental program
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Embodiment 1

[0021] Select ethylene glycol as the additive, N, N-dimethylacetamide as the solvent, the mass ratio of the additive to the solvent is 1:4, and the mass ratio of polyvinylidene fluoride to the solvent is 3:14, and mix them evenly in a three-necked flask , heated to 90°C, fully stirred to prepare a homogeneous solution, and allowed to stand for defoaming. The spinning solution was injected into ice water at 0°C with an injection needle to make spherical particles. The obtained spherical particles were soaked in ethanol at 0°C for 60 minutes to extract ethylene glycol and N,N-dimethylacetamide, then soaked in n-hexane for 30 minutes to replace the ethanol, and then vacuum-dried the porous microspheres at 30°C for 6 hours , to obtain polyvinylidene fluoride porous microspheres with an average diameter of 1.8mm and a porosity of 78.8%.

Embodiment 2

[0023] Select dimethyl sulfoxide as the additive, N,N-dimethylformamide as the solvent, the mass ratio of the additive to the solvent is 1:1, the mass ratio of polyacrylonitrile to the solvent is 6:17, mix in a three-necked flask Evenly, heat to 90°C, stir well to prepare a homogeneous solution, and let it stand for defoaming. The spinning solution was injected into ice water at 0°C with an injection needle to make spherical particles. The obtained spherical particles were soaked in ethanol at 0°C for 30 minutes to extract dimethyl sulfoxide and N,N-dimethylformamide, then soaked in n-hexane for 20 minutes to replace the ethanol, and then the porous microspheres were vacuumed at 40°C After drying for 8 hours, polyacrylonitrile porous microspheres with an average diameter of 1.9 mm and a porosity of 83.0% were obtained.

Embodiment 3

[0025] Choose dimethyl sulfone as the additive, N, N-dimethylformamide as the solvent, the mass ratio of the additive to the solvent is 10:1, the mass ratio of polyacrylonitrile to the solvent is 11:9, mix well in a three-necked flask , heated to 130°C, fully stirred to prepare a homogeneous solution, and allowed to stand for defoaming. The spinning solution was injected into water at 10°C with an injection needle to make spherical particles. The obtained spherical particles were soaked in ethanol at 10°C for 30 minutes to extract dimethyl sulfone and N,N-dimethylformamide, then soaked in n-hexane for 20 minutes to replace the ethanol, and then vacuum-dried the porous microspheres at 30°C After 8 hours, polyacrylonitrile porous microspheres with an average diameter of 2.1 mm and a porosity of 88.6% were obtained.

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Abstract

The invention discloses a method for preparing polymer porous microspheres through mixed phase separation. The method comprises the following steps: 1), dissolving a polymer and an additive into a solvent, and heating and stirring until the polymer and the additive are completely dissolved to form a transparent solution; 2), injecting a high-temperature polymer solution into a low-temperature non-solvent such as ice water or water and the like by using a syringe needle and inducing thermally induced phase separation and non-solvent induced separation to form pores; and 3), washing, drying and the like to obtain the polymer porous microspheres. The characteristics that the thermally induced phase separation is easy to control, pore-forming rate is high and the non-solvent induced separation has high applicability are exerted; the preparation method is simple, high in efficiency and low in cost; and the invention provides the method for preparing the polymer porous microspheres with various pore structures and high porosity. The preparation method has a huge application prospect in the aspects of gas separation, water treatment, biological active substances, catalyst carriers and the like.

Description

technical field [0001] The invention relates to the technical field of porous materials and their preparation, in particular to a porous microsphere material and a preparation method thereof. Background technique [0002] In recent years, the preparation technology of microspheres has become increasingly mature. At the same time, due to its characteristics of easy large-scale production, high repeatability, and stable physical and chemical properties, it has played an important role in many fields such as biotechnology, electronic technology, and medical engineering. Since the 1980s, polystyrene microspheres, dextran series microspheres, agar series microspheres, polyacrylamide microspheres and new polyacrylic acid series microspheres have been used as separation and purification media successively, making chromatography technology a bioactive The most commonly used method for the separation and purification of substances. In the medical field, antibodies are physically ads...

Claims

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Application Information

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IPC IPC(8): B01J13/06
Inventor 徐志康吴青芸万灵书
Owner ZHEJIANG UNIV
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