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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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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 101455975A) adopts electrospinning process, constant tension thermal drawing, pre-oxidation and high-temperature chemical activation to prepare porous polyacrylonitrile-based nano-carbon fibers, but this method requires thermal drawing at 120-150°C It is not suitable for the preparation of polymer porous nanofibers with poor thermal stability, which also limits the range of polymer choices

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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Effect test

Embodiment 1

[0024] Select ethylene glycol as the additive, N,N-dimethylacetamide as the solvent, the mass ratio of the additive to the solvent is 1:4, the mass ratio of polyvinylidene fluoride to the solvent is 1:5, mix in a round bottom flask Evenly, heat to 90°C, stir well until the mixed system becomes a homogeneous solution, then let it stand for defoaming. Then the solution was electrospun under the condition of spinning voltage of 20kV, micro injection pump flow rate of 0.5mL / h, and spinning distance of 11cm, and the obtained fibers were received in an ice-water bath. Soak the obtained nanofibers in ethanol at 0°C for 60 minutes, extract ethylene glycol and N,N-dimethylacetamide, then soak them in n-hexane for 30 minutes, replace the ethanol, and then vacuum-dry the nanofibers at 30°C for 6 Hours, polyvinylidene fluoride porous nanofibers were obtained. The average diameter of the fiber is about 450nm, and the pore size ranges from 30 to 70nm.

[0025] The above PVDF porous nanofi...

Embodiment 2

[0030] Select dimethyl sulfoxide as additive, N,N-dimethylformamide as solvent, the mass ratio of additive to solvent is 1:1, the mass ratio of polyacrylonitrile to solvent is 1:3, in a round bottom flask Mix evenly, heat to 90°C, stir well until the mixed system becomes a homogeneous solution, then let it stand for defoaming. Then the solution was electrospun 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 obtained fibers were received in an ice-water bath. Soak the obtained fibers in ethanol at 0°C for 30 minutes, extract dimethyl sulfoxide and N,N-dimethylformamide, soak them in n-hexane for 20 minutes, replace the ethanol, and then vacuumize the nanofibers at 40°C Dry for 8 hours to remove n-hexane to obtain polyacrylonitrile porous nanofibers. The average diameter of the nanofiber is about 450nm, and the pore diameter ranges from 20 to 120nm.

[0031] The above polyacrylonitrile ...

Embodiment 3

[0033] Select dimethyl sulfone as additive, N,N-dimethylformamide as solvent, the mass ratio of additive to solvent is 1:1, the mass ratio of polyacrylonitrile to solvent is 1:4, mix in a round bottom flask Evenly, heat to 90°C, stir well until the mixed system becomes a homogeneous solution, then let it stand for defoaming. Then the solution was electrospun under the conditions of a spinning voltage of 10 kV, a flow rate of a micro-syringe pump of 0.5 mL / h, and a spinning distance of 7 cm, and the obtained fibers were received in a water bath at 10° C. Soak the obtained fibers in ethanol at 10°C for 30min, extract dimethyl sulfone and N,N-dimethylformamide, then soak in n-hexane for 15min, replace the ethanol, and then vacuum-dry the nanofibers at 30°C The n-hexane was removed for 8 hours to obtain polyacrylonitrile porous nanofibers. The average diameter of the nanofiber is about 700nm, and the pore diameter ranges from 1 to 120nm.

[0034] The above-mentioned PAN porous n...

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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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