CN103422184A - Preparation method of porous fiber with high specific surface area - Google Patents
Preparation method of porous fiber with high specific surface area Download PDFInfo
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- CN103422184A CN103422184A CN2012101625468A CN201210162546A CN103422184A CN 103422184 A CN103422184 A CN 103422184A CN 2012101625468 A CN2012101625468 A CN 2012101625468A CN 201210162546 A CN201210162546 A CN 201210162546A CN 103422184 A CN103422184 A CN 103422184A
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Abstract
The invention provides a preparation method of porous fiber with high specific surface area. The method includes: preparing raw material for preparing porous fiber precursor into even solution; subjecting the prepared solution to filamentization to obtain fiber 0.01-10 micrometers in diameter, namely the precursor of the porous fiber with high specific surface area; placing the precursor in a high-pressure kettle for supercritical extraction drying or supercritical drying; or subjecting the precursor to gradient drying to obtain the porous fiber with high specific surface area; wherein the raw material comprises one or more of soluble natural polymer, soluble synthetic polymer, and soluble metal salt or metal organic compound capable of hydrolytic polycondensation reaction or soluble silicon compound capable of hydrolytic polycondensation reaction.
Description
Technical field
The present invention relates to field of porous materials, a kind of preparation method of high specific surface area porous fiber is provided.
Background technology
The fields such as that porous material can be used for is heat insulation, sound-absorbing, catalyst and catalyst carrier, porous fibre is a kind of version of porous material.Owing to being fibrous, have good toughness, can weave or make non-woven constructions, porous fibre can be divided into inorganic porous fiber, Porous-Organic fiber and organic/inorganic composite porous fiber according to forming, because various fibers have difference, applicable to different fields.At present, the method for preparing porous fibre adopts spin processes structure filament more, the method of structure loose structure mainly is divided three classes, the first kind is to adopt solvent evaporates or non-solvent contact to cause being separated, produce loose structure, solvent evaporates is multiplex in dry method or semidry method spinning process, and solvent evaporates forms filamentary structure, by controlling its process, can form loose structure simultaneously; Non-solvent method is multiplex in semidry method or wet method.The Equations of The Second Kind method is the multicomponent cospinning, at Cheng Sihou, adopts lixiviation process to remove the component that wherein dissolves in leaching agent, forms loose structure.The 3rd class methods, at multicomponent cospinning Cheng Sihou, are utilized high-temperature process, remove the component that stability is lower, form loose structure.
Although the preparation method of various porous fibres can prepare porous fibre easily, there is the problem that porosity is low, specific area is little in current porous fibre.Main cause is in solvent or leaching agent volatilization process, and pore structure shrinks or part is subsided.The invention provides and a kind ofly by the method for controlling drying and leaching, avoid or reduce drying stress, prepare high specific surface area porous fiber.
Summary of the invention
The purpose of this invention is to provide a kind of preparation method who prepares high specific surface area porous fiber.By the fiber preparation method, prepare multicomponent fibre, wherein at least one component is pore former, remove pore former by last handling process, form loose structure, by controlling drying or controlling the method leached and avoid or reduce interfacial stress, make porous fibre keep higher porosity and specific area.
Implement concrete grammar of the present invention
The porous fibre of indication of the present invention refers to one or more fiber or the non-woven constructions consisted of fiber or the textile structure of gained.Fiber refers to the fiber of diameter 0.01-10 micron, one or more in natural polymer, synthetic polymer, inorganic oxide or charcoal of its active principle.The preparation process of this fiber comprises preparation and the last handling process of precursor fibre.The preparation method of Precursors of Fibers so long as can obtain the method for above-mentioned diameter fibers presoma and get final product, is not particularly limited it, preferably electrospinning process.Below take electrospinning process as example explanation the present invention.
According to the design of final fibre fractionation, become the silk component can comprise solubility natural polymer, solubility synthetic polymer, solubility and the slaine of hydrolysis-condensation reaction can occur or metallo-organic compound or solubility and one or more in the silicon compound of hydrolysis-condensation reaction can occur.By becoming the silk component to be dissolved in suitable solvent, be ejected in electric field, under electric field action, to the electrode direction towing, be accumulated on trap, form fibre bundle, fiber matting or fibrous braid.The fiber now formed can be porous fibre, can be also feltwork; Can be solvent evaporates dry fiber completely, can be also the wet fiber that contains solvent; Trap can be in air, also can be in solvent, and therefore fiber also comprises the fiber be immersed in solvent.The fiber now obtained becomes the presoma of high specific surface area porous fiber.Presoma is placed in to autoclave, add leaching agent or drying medium, autoclave is heated on the critical-temperature of leaching agent or drying medium, autoclave is spontaneous to be depressed on the critical pressure of leaching agent or drying medium, then autoclave constant temperature is decompressed to normal pressure, be cooled to room temperature, open autoclave and obtain high specific surface area porous fiber; For the porous wet fiber formed through spinning process, can adopt the method for gradient drying to obtain the porous fibre of high-specific surface area, method comprises puts into container or the atmosphere drier with gradient humidity by wet fiber, perhaps use the mode drying of gradient increased temperature, obtain high specific surface area porous fiber.
Embodiment 1
The polyvinylpyrrolidone of 2g mean molecule quantity 1300000 (PVP) is dissolved in the 10g absolute ethyl alcohol, add 4g butyl titanate and 2g acetic acid, stir, add in the syringe of 15ml with No. 12 syringe needles (internal diameter 0.8mm), syringe is vertically placed, and under Action of Gravity Field, spinning solution flows out, and applies the voltage of 25KV between syringe needle and sample trap, spacing 20cm between syringe needle and trap obtains the porous fibre presoma on trap.Presoma is placed in to autoclave, adds appropriate absolute ethyl alcohol, autoclave is heated to 250 ℃, pressure rises to 8MPa, and constant temperature is decompressed to normal pressure, passes into nitrogen blowing, is cooled to room temperature, obtains the titanium oxide porous fibre of 3 microns of diameters, pulp freeness 241m
2/ g, pore volume 0.43cm
3/ g, average pore diameter 7.2nm.
Embodiment 2
The polyacrylonitrile (PAN) of the PVP of mean molecule quantity 1300000 and mean molecule quantity 150000 is configured to respectively to the N that mass concentration is 10% and 20%, N dimethyl formamide (DMF) solution, two kinds of solution are become to mixed solution according to PVP with the proportional arrangement of PAN mass ratio 3:1, and electrostatic spinning condition and post-treatment condition are with embodiment 1.Obtain the PAN fiber of 0.5 micron of diameter, pulp freeness 70m
2/ g, pore volume 0.11cm
3/ g, average pore diameter 15.7nm.
Claims (4)
1. the preparation method of a high specific surface area porous fiber, it is comprised of following step:
(1) raw material that will prepare the porous fibre presoma is made into uniform solution, and raw material is from one or more in following: solubility natural polymer, solubility synthetic polymer, solubility and the slaine of hydrolysis-condensation reaction can occur or metallo-organic compound or solubility and the silicon compound of hydrolysis-condensation reaction can occur;
(2) homogeneous solution prepared is made to the fiber of diameter 0.01-10 micron, i.e. high specific surface area porous Precursors of Fibers by shredding process;
(3) high specific surface area porous Precursors of Fibers is placed in to autoclave, carries out overcritical leaching drying or supercritical drying;
(4) or by high specific surface area porous Precursors of Fibers carry out the gradient drying;
Obtain high specific surface area porous fiber.
2. method according to claim 1, wherein: shredding process is restriction not, preferably electrospinning process.
3. method according to claim 1, wherein: in raw material, have a kind ofly during as pore former, overcritical leaching drying, leach the good solvent that dry medium is pore former, and become the non-solvent of silk components for other.
4. method according to claim 1, wherein: when high specific surface area porous Precursors of Fibers is wet porous fibre, adopt supercritical drying, the good solvent of liquid in the hole that drying medium is wet porous fibre, and be the non-solvent of other one-tenth components.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2012101625468A CN103422184A (en) | 2012-05-23 | 2012-05-23 | Preparation method of porous fiber with high specific surface area |
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| CN2012101625468A CN103422184A (en) | 2012-05-23 | 2012-05-23 | Preparation method of porous fiber with high specific surface area |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105862174A (en) * | 2016-04-08 | 2016-08-17 | 合肥工业大学 | Preparation method of novel metal organic complex fibers and derivative porous carbon fibers thereof |
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| CN101244384A (en) * | 2007-11-08 | 2008-08-20 | 武汉科技大学 | Photocatalyst having response to visible light and preparation thereof |
| CN101357996A (en) * | 2008-09-12 | 2009-02-04 | 中国科学院广州化学研究所 | Multi-microporous epoxy thermosetting resin, preparation method and application thereof |
| CN102268784A (en) * | 2011-06-17 | 2011-12-07 | 北京化工大学常州先进材料研究院 | Preparation of porous natural polymer nanofiber non-woven fabric |
| CN102417364A (en) * | 2011-08-02 | 2012-04-18 | 中国科学院化学研究所 | Micro-nano porous material and preparation method thereof |
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2012
- 2012-05-23 CN CN2012101625468A patent/CN103422184A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0760249A1 (en) * | 1995-08-24 | 1997-03-05 | Dainichiseika Color & Chemicals Mfg. Co. Ltd. | Process for the production of connected microgel particles and articles treated with connected microgel particles |
| CN1256381A (en) * | 1998-10-20 | 2000-06-14 | 松下电器产业株式会社 | Organic porous body |
| CN1978037A (en) * | 2005-12-08 | 2007-06-13 | 李鑫 | Method for polyolefin porous film mfg. method |
| CN101244384A (en) * | 2007-11-08 | 2008-08-20 | 武汉科技大学 | Photocatalyst having response to visible light and preparation thereof |
| CN101357996A (en) * | 2008-09-12 | 2009-02-04 | 中国科学院广州化学研究所 | Multi-microporous epoxy thermosetting resin, preparation method and application thereof |
| CN102268784A (en) * | 2011-06-17 | 2011-12-07 | 北京化工大学常州先进材料研究院 | Preparation of porous natural polymer nanofiber non-woven fabric |
| CN102417364A (en) * | 2011-08-02 | 2012-04-18 | 中国科学院化学研究所 | Micro-nano porous material and preparation method thereof |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105862174A (en) * | 2016-04-08 | 2016-08-17 | 合肥工业大学 | Preparation method of novel metal organic complex fibers and derivative porous carbon fibers thereof |
| CN105862174B (en) * | 2016-04-08 | 2018-02-06 | 合肥工业大学 | A kind of preparation method of novel metal organic coordination compound fiber and its derivative porous carbon fiber |
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Application publication date: 20131204 |