Method for preparing polymer porous nanofiber through mixed phase separation

A nanofiber, polymer technology, applied in the direction of single-component synthetic polymer rayon, chemical post-treatment of synthetic polymer rayon, rayon made of cellulose derivatives, etc. High requirements, limited range of polymer selection, etc., to achieve the effect of wide application range and simple preparation method

Inactive Publication Date: 2012-06-27
ZHEJIANG UNIV
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  • Abstract
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  • Claims
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Problems solved by technology

However, this method is based on the volatilization refrigeration effect of the high-volatility solvent chloroform, which has high requirements for solvent selection, and usually can only form holes on the surface of the fiber. For polymers that can only be dissolved in low-volatility solvents, this method is not applicable. Limits the choice of polymers
[0005] Chinese invention patent (CN

Method used

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

Examples

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Example Embodiment

[0023] Example 1

[0024] Select ethylene glycol as the additive, N,N-dimethylacetamide as the solvent, the mass ratio of additive to solvent is 1:4, and the mass ratio of polyvinylidene fluoride to solvent is 1:5, and mix in a round bottom flask. Evenly, heat to 90°C, fully stir until the mixed system becomes a homogeneous solution, and then stand to defoam. Then the solution was electrospinned under the conditions of spinning voltage of 20kV, micro-syringe pump flow rate of 0.5mL / h, and spinning distance of 11cm, and the obtained fibers were received in an ice water bath. The obtained nanofibers were soaked in ethanol at 0°C for 60 minutes, ethylene glycol and N,N-dimethylacetamide were extracted, and then soaked in n-hexane for 30 minutes to replace the ethanol, and then the nanofibers were vacuum dried at 30°C. 6 After hours, porous polyvinylidene fluoride nanofibers are obtained. The average diameter of the fiber is about 450 nm, and the pore diameter ranges from 30 to 70 ...

Example Embodiment

[0029] Example 2

[0030] Choose dimethyl sulfoxide as the additive, N,N-dimethylformamide as the solvent, the mass ratio of additive to solvent is 1:1, and the mass ratio of polyacrylonitrile to solvent is 1:3, in a round bottom flask Mix uniformly, heat to 90°C, stir well until the mixed system becomes a homogeneous solution, and then stand to defoam. Then the solution was electrospinned under the conditions of a spinning voltage of 16kV, a flow rate of a micro-syringe pump of 0.7mL / h, and a spinning distance of 5cm, and the resulting fibers were received in an ice water bath. The obtained fiber was immersed in ethanol at 0°C for 30 minutes, dimethyl sulfoxide and N,N-dimethylformamide were extracted, and then soaked in n-hexane for 20 minutes to replace the ethanol, and then the nanofibers were vacuumed at 40°C Drying for 8 hours to remove n-hexane to obtain polyacrylonitrile porous nanofibers. The average diameter of nanofibers is about 450nm, and the pore size ranges from ...

Example Embodiment

[0032] Example 3

[0033] Choose dimethyl sulfone as the additive, N,N-dimethylformamide as the solvent, the mass ratio of additive to solvent is 1:1, and the mass ratio of polyacrylonitrile to solvent is 1:4, and mix in a round bottom flask Evenly, heat to 90°C, fully stir until the mixed system becomes a homogeneous solution, and then stand to defoam. Then the solution was electrospinned under the conditions of a spinning voltage of 10kV, a microsyringe pump flow rate of 0.5mL / h, and a spinning distance of 7cm, and the resulting fibers were received in a water bath at 10°C. The obtained fiber was soaked in ethanol at 10°C for 30 minutes, dimethyl sulfone and N,N-dimethylformamide were extracted, and then soaked in n-hexane for 15 minutes to replace the ethanol, and then the nanofibers were vacuum dried at 30°C The n-hexane was removed for 8 hours to obtain polyacrylonitrile porous nanofibers. The average diameter of nanofibers is about 700 nm, and the pore diameter ranges fro...

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Abstract

The invention discloses a method for preparing polymer porous nanofiber through mixed phase separation. The diameter of the prepared polymer porous nanofiber is between 300nm and 900nm, and the aperture is 1 to 120nm. The preparation method for the polymer porous nanofiber comprises the following steps of: mixing a polymer, an additive and a solvent according to certain proportion; heating and stirring the mixture until the mixture is completely dissolved and forms transparent solution; performing electrostatic spinning on the solution; depositing primarily generated fibers in ice-water bath or the water bath with the temperature of 0 to 20 DEG C, wherein thermally induced phase separation and nonsolvent induced phase separation are caused; and extracting residual solvent and additive through post treatment to obtain the polymer porous nanofiber. The preparation method is simple and highly effective and is convenient to perform; and polymer porous nanofibers with different diameters and porosities can be prepared by adjusting the conditions of electrostatic spinning. The method has enormous application prospect in aspects, such as high-tech composite materials, water treatment, catalyst carriers, electrode materials and the like.

Description

technical field [0001] The invention relates to the technical field of functional fiber materials and their preparation, in particular to a porous nanofiber material and a preparation method thereof. Background technique [0002] When the diameter of the polymer fiber is reduced to the submicron level (0.1-10 μm), it will have the characteristics of ultra-high specific surface area, diversified surface functions and excellent mechanical properties, making polymer nanofibers used in high-tech composite materials, water treatment, Many important fields such as catalyst supports and electrode materials have great application prospects. Electrospinning is a simple and effective technology for preparing continuous and uniform nanofibers, which is suitable for most polymers, inorganic materials, and composite materials. The use of this technology to prepare nanofibers has become the main choice at present. The porous polymer fiber can further increase the specific surface area of...

Claims

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Application Information

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IPC IPC(8): D01F6/48D01F6/54D01F6/94D01F6/92D01F6/52D01F2/28D01F1/10D01F11/06D01F11/08D01F11/02D01D5/00D01D1/02
Inventor 徐志康吴青芸欧洋
Owner ZHEJIANG UNIV
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