CN105363349A - Preparation method of filter membrane with uniform pore size - Google Patents
Preparation method of filter membrane with uniform pore size Download PDFInfo
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- CN105363349A CN105363349A CN201510919814.XA CN201510919814A CN105363349A CN 105363349 A CN105363349 A CN 105363349A CN 201510919814 A CN201510919814 A CN 201510919814A CN 105363349 A CN105363349 A CN 105363349A
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- filter membrane
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
- B01D69/02—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor characterised by their properties
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2325/00—Details relating to properties of membranes
- B01D2325/02—Details relating to pores or porosity of the membranes
Abstract
The invention discloses a preparation method of a filter membrane with uniform pore size. Hollow or core-shell fiber with uniform size undergoes oriented assembly, cutting and subsequent processing to prepare the filter membrane with uniform pore size at large scale. Thereby, promotion and application of the filter membrane material are enhanced. People pay much attention to the filter membrane with extensive application value in the field of substances separation in production and life. However, it is hard to accurately separate different sizes including biomacromolecules and nano-particles due to nonuniform pore sizes of existing filter membrane materials so as to influence further promotion and application of the filter membrane materials. Then, the easily available hollow or core-shell fiber with uniform size is combined with the processes of oriented assembly, fixing, cutting and subsequent processing so as to prepare the filter membrane material with uniform pore size and make a small contribution to accurate separation of nano-particles and further promotion and application of the filter membrane.
Description
Technical field
The present invention relates to the preparation method of a kind of homogeneous aperture filter membrane, particularly by the hollow of single-size or nucleocapsid structure fiber by orientation assembling, cutting and subsequent treatment batch prepare the filter membrane in homogeneous aperture thus promote the material particularly separation of nano particle and application.
Background technology
Usually need to be separated the microparticle in some solution in the productive life of people, the such as nano particle etc. of cell, bacterium, virus, protein, nucleic acid, artificial preparation, is developed for this reason and comprises filter membrane, electrophoresis, chromatogram, the multiple technologies such as centrifugal.Wherein filter film technology is due to easy to use, quick, cheap and applied widely.But being limited by the heterogeneity in current membrane filtration aperture, the application of filter membrane is very restricted.Such as, although people know that the cell size of one species is similar, then there is size difference in different types of cell, therefore the different types of cell of different pore size filter membrane quick separating can be passed through in principle, but owing to lacking the filter membrane in corresponding homogeneous aperture, people can only be separated by comprising the methods such as centrifugal or electrophoresis, and consequently leads to and comprise the problem such as the raising of cost, the prolongation of time.Similar problem appears at the numerous areas such as Separation of Proteins and the acquisition of dispersed nano particle equally.Therefore in the urgent need to developing the correlation technique of homogeneous aperture filter membrane.
Summary of the invention
Technical problem: the preparation method that the object of this invention is to provide a kind of homogeneous aperture filter membrane, by single-size hollow or nucleocapsid structure fiber by orientation assembling, cutting and subsequent treatment thus batch prepares the filter membrane in homogeneous aperture to promote separation and the application of microparticle.
Technical scheme: the preparation method of a kind of homogeneous aperture of the present invention filter membrane, comprises the steps:
A. first single-size nucleocapsid or doughnut assembled by orientation or weave and become the film with orientation characteristic and solidified by adhesive and obtain the fiber membrane sheet material with orientation characteristic;
B. the fiber membrane sheet material with orientation characteristic is superposed blend compounds mutually along fiber-wall-element model to stick agent and fix the orientation fibers bulk being formed and built by single-size fibrous material;
C. by orientation fibers bulk along fiber axis to vertical direction carry out machine cuts and obtain the array plane thin slice being distributed in adhesive plane by the nucleocapsid of single-size or hollow fiber material, wherein namely nucleocapsid structure fibrous material array plane thin slice obtains homogeneous aperture filter membrane after removal nuclear material, and hollow structure fibrous material array plane thin slice is homogeneous aperture filter membrane;
Described single-size refers to that diameter or aperture deviation average are less than 5% of mean value;
Described removal nuclear material refers to by dissolving or corrode and is removed from Core-shell structure material by nuclear material;
Described subsequent treatment comprises the processing method that cleaning, drying, annealing etc. improve homogeneous aperture film.
Beneficial effect: often pore size distribution range is wider for current commercial filter membrane, this just makes the accurate microparticle that is separated have difficulties, and the application by homogeneous aperture filter membrane that the nucleocapsid of size uniformity or doughnut are obtained by orientation assembling, cutting, subsequent treatment because aperture is homogeneous therefore, it is possible to the microparticle of effective separation different size, thus to offer help for the further genralrlization application of filter membrane and further developing of microparticle science and technology.
Accompanying drawing explanation
Fig. 1 is for prepare homogeneous aperture filter membrane schematic flow sheet by single-size doughnut.
Fig. 2 is for prepare homogeneous aperture filter membrane schematic flow sheet by single-size nucleocapsid structure fiber.
Detailed description of the invention
Below in conjunction with drawings and Examples, the present invention is further illustrated.
Homogeneous aperture filter membrane schematic flow sheet is prepared by mono-disperse doughnut shown in Fig. 1.Doughnut a is assembled into aligned single-layer along preferential direction, and blend compounds sticks agent c fixing formation thin slice d.Thin slice d is carried out superposition when the different thin slice fiber-wall-element model of guarantee is parallel by adhesive and obtains block e.The thin slice f that block e obtains hollow short pipe array is being cut with the axial vertical direction of orientation fibers.Namely thin slice f is obtained homogeneous aperture filter membrane by last handling processes such as annealing, cleaning, cuttings.
Fig. 2 then gives and prepares homogeneous aperture filter membrane schematic flow sheet by mono-disperse nucleocapsid structure fiber.The nucleocapsid structure fiber a of to be first b shell by core be a is assembled into aligned single-layer along preferential direction, and blend compounds sticks that agent c is fixing forms thin slice d.Thin slice d is carried out superposition when the different thin slice fiber-wall-element model of guarantee is parallel by adhesive and obtains block e.The thin slice f that block e obtains nucleocapsid quarter butt array is being cut with the axial vertical direction of orientation fibers.Namely obtain nuclear material by dissolving or the caustic solution nuclear material removed in nucleocapsid structure and remove the hole array film stayed.Namely homogeneous aperture filter membrane is obtained further by post-processing steps such as annealing, cleaning and cuttings.
Embodiment 1:
First be shitosan and the molecular weight polyethylene glycol oxide that is 900,000 the aqueous solution that is 8wt% with quality 1:1 ratio by the solution concentration containing 50% acetic acid of 10,000 with the molecular weight that de-acetyl rate is 88%.Then when between the collection cylinder that syringe needle and diameter are 8 centimeter length 10 centimetres, apply the voltage of 15KV on syringe needle by orientation electrospinning device with the speed of 0.5 ml/hour when 15 centimetres, interval by high-voltage power cathode, aluminium foil coated on collection cylinder and high voltage source are rotated to collect to Electrode connection and with the speed of 1000 revs/min and are penetrated from syringe needle the nanofiber come.Nano-fiber film was obtained about 10 micron thickness by cutting off nano-fiber film with drum rotating direction vertical direction and taking off from collection cylinder after about 2 hours by electrostatic spinning from collection cylinder, and the internal diameter of polyethylene glycol oxide to be nucleocapsid glycan be shell is about the nano-fiber film that 100 nanometer external diameters are about 130 nanometers.Repeat said process 4000 times, and inspection each obtain the size of nano-fiber film nanofiber, choose nanofiber diameter change in size amplitude and be less than the nano-fiber film of 5% to guarantee that nuclear shell structure nano fibre inner diameter scope is in 95-105 nanometer range.Then get the above-mentioned nuclear shell structure nano fiber membrane chosen of a slice to be bonded at and double faced adhesive tape to be fixed on polyethylene board and epoxy resin coating makes to fill up epoxy resin in the space of nano-fiber film, remove unnecessary epoxy resin by scraper plate, and when 100 degrees Celsius curing nano fiber membrane.Subsequently the oriented nanofibers film of epoxy resin cure taken off from polyethylene board and use water and the ethanol purge repeatedly rear dry oriented nuclei shell structural nano fiber membrane thin slice namely obtaining epoxy resin cure.This thin slice to be fixed on polyethylene board and epoxy resin coating by double faced adhesive tape, then get an other plate sheet nanofiber on two thin slices in oriented nanofibers film to be parallel to each other and to compress two thin slices epoxy resin unnecessary between two thin slices is overflowed, repeat said process and make 3000 plate sheets to be superimposed by epoxy resin along same orientation and under 100 degrees Celsius, to solidify the block namely obtaining and built by oriented nuclei shell structural nano fiber.By this block along the direction vertical with nanofiber orientation by slicer cutting obtain thickness be 20 microns on have the film of nucleocapsid structure quarter butt array arrangement.This film is cleaned in distilled water remove polyethylene glycol oxide and dry i.e. acquisition has aperture to be about the homogeneous aperture film of 100 nanometers.Be 2.54 centimetres of puncher process by this film by internal diameter be 2.54 centimetres to obtain diameter, thickness is 20 microns, and aperture is the homogeneous aperture filter membrane of 100 nanometers.
With molecular weight be 50,000 shitosan replace molecular weight be 10,000 shitosan repeat said process can obtain the homogeneous aperture filter membrane that aperture is 70 nanometers.
By the particle of two kinds of films for separating of diameter 90 nanometer and 150 nanometers, then can be separated the nano particle of 150 nanometers with the filter membrane of aperture 100 nanometer, and the filter membrane of aperture 70 nanometer is separated the nano particle of 90 nanometers.
Embodiment 2:
First molecular weight is prepared to be 100,000 concentration is the N of the polyacrylonitrile of 20wt%, N '-dimethyl formamide solution. the aperture then polyacrylonitrile solution being imported coaxial syringe needle is the outer syringe needle of 1.6 millimeters, and methyl-silicone oil to be imported aperture be syringe needle in 0.7 millimeter.Syringe needle is connected to the positive pole of high voltage source, it is on aluminium foil coated on 8 centimeter length, 10 centimetres of collection cylinders that negative pole is then connected to 15 centimetres of diameters outward.Opening collection cylinder makes its speed be 1000 revs/min.Then by syringe pump, the flow velocity of interior syringe needle and outer syringe needle is all controlled at 1 ml/hour.It is 15KV that unlatching high voltage source arranges electrostatic spinning voltage.Electrostatic spinning takes off oriented nanofibers film from collection cylinder after 2 hours and processes 2 hours at 900 degrees Celsius under nitrogen protection 250 degrees Celsius of process again after 2 hours; obtain external diameter and be about 500 nanometers, internal diameter is about the hollow carbon oriented nanofibers film of 300 nanometers.This film to be bonded on polyethylene board by double faced adhesive tape and to be coated with between gap that adhesive for polyurethane makes adhesive be distributed in hollow Nano fiber in use and not to infiltrate in doughnut the thin slice then solidifying and namely obtain orientation hollow carbon fiber film and fixed by polyurethane.A large amount of above-mentioned thin slice is carried out superposing obtaining according to the mode that adhesive for polyurethane pastes passed in principle that fiber-wall-element model is parallel the block that the orientation hollow carbon nanofiber of thickness more than 3 centimetres fixed by polyurethane.Laser cutting machine is utilized to carry out cutting along the direction vertical with hollow carbon nanofiber orientation the polyurethane film namely obtaining and have hollow carbon microtubule arrays.By this film 100 degrees Celsius of annealing, and further cut growth and wide be respectively the film of 10 centimetres, then with to be 300 nano thickness be in i.e. acquisition aperture dry after distilled water, the ethanol purge homogeneous aperture filter membrane of 20 microns.
Embodiment 3:
The stainless steel metal wire that cut-off footpath is 1 micron is at the epoxy resin of its surface coating about 10 microns, then be that the surface of aluminum plate orientations of teflon becomes individual layer and infusion epoxy resin again on top layer by stainless steel metal wire coated for epoxy resin, thickness is that the aluminium sheet of teflon and above-mentioned row have aluminium sheet wiry to be harmonious to pressurize and control at 10 microns by other one piece of top layer, obtains the orientation stainless steel metal wire array sheet that epoxy resin is fixing.10000 layers of above-mentioned thin slice are carried out superposition and infusion epoxy resin again by the differently-oriented directivity of stainless steel metal wire, and the epoxy resin obtaining orientation stainless steel metal wire array fixes block.Along and the vertical direction of stainless steel metal wire differently-oriented directivity carry out cutting that to obtain two sides be the epoxy sheet that stainless steel lattice array thickness is about 100 microns.This thin slice is removed stainless steel material by corrosive liquid obtain by the microporous sheet of 1 micron of hole matrix-like one-tenth.This thin slice is cut into the film that diameter is 2.54 centimetres, and then namely to obtain aperture be 1 micron thickness is the homogeneous aperture filter membrane of 100 microns with dry after distilled water, ethanol purge.
Embodiment 4:
The stainless steel metal wire that cut-off footpath is 5 microns is at the polyimide insulative paint of its surface coating about 25 microns, then the stainless steel metal wire covered by polyimide insulative enamel-cover is that the surface of aluminum plate orientations of teflon becomes individual layer and infusion epoxy resin again on top layer, thickness is that the aluminium sheet of teflon and above-mentioned row have aluminium sheet wiry to be harmonious to pressurize and control at 30 microns by other one piece of top layer, obtains the orientation stainless steel metal wire array sheet that epoxy resin is fixing.10000 layers of above-mentioned thin slice are carried out superposition by the differently-oriented directivity of stainless steel metal wire and again pours into polyimide insulative paint, block fixed by the polyimides obtaining orientation stainless steel metal wire array.Along and the vertical direction of stainless steel metal wire differently-oriented directivity carry out cutting that to obtain two sides be the polyimide that stainless steel lattice array thickness is about 100 microns.This thin slice is removed stainless steel material by corrosive liquid obtain by the microporous sheet of 5 microns of hole matrix-like one-tenth.This thin slice is cut into the film that diameter is 8 centimetres, and then namely to obtain aperture be 5 micron thickness is the homogeneous aperture filter membrane of 100 microns with dry after distilled water, ethanol purge.
Embodiment 5:
The stainless steel metal wire that cut-off footpath is 1 micron is coated with the SU-8 photoresist of 1 micron thickness on surface and has the surface of aluminum plate orientations of sticking double faced adhesive tape become individual layer and pour into SU-8 photoresist on top layer after solidification, thickness controls at 5 microns by even glue, and exposure curing obtains the fixing orientation stainless steel metal wire array sheet of SU-8 photoresist subsequently.100000 layers of above-mentioned thin slice are carried out superposition by the differently-oriented directivity of stainless steel metal wire and again pours into SU-8 photoresist and exposure curing, block fixed by the SU-8 photoresist obtaining orientation stainless steel metal wire array.Along and the vertical direction of stainless steel metal wire differently-oriented directivity carry out cutting that to obtain two sides be the SU-8 photoresist compound foil that stainless steel lattice array thickness is about 100 microns.This thin slice is removed stainless steel material by corrosive liquid obtain by the microporous sheet of 1 micron of hole matrix-like one-tenth.This thin slice is cut into the film that diameter is 6 centimetres, and then namely to obtain aperture be 1 micron thickness is the homogeneous aperture filter membrane of 100 microns with dry after distilled water, ethanol purge.
Embodiment 6:
The copper core enamel-covered wire getting wall thickness 0.002 mm dia 0.025 millimeter has the surface of aluminum plate orientations of sticking double faced adhesive tape to become individual layer and infusion epoxy resin on top layer, thickness is that the aluminium sheet of teflon and above-mentioned row have aluminium sheet wiry to be harmonious to pressurize and control at 30 microns by other one piece of top layer, obtains the orientation enamel-covered wire array sheet that epoxy resin is fixing.10000 layers of above-mentioned thin slice are carried out superposition and infusion epoxy resin again by the differently-oriented directivity of enamel-covered wire, and the epoxy resin obtaining orientation enamel-covered wire array fixes block.Along and the vertical direction of enamel-covered wire differently-oriented directivity carry out cutting that to obtain two sides be the epoxy sheet that enamel-covered wire lattice array thickness is about 100 microns.This thin slice is obtained the microporous sheet become by 21 microns of hole matrix-like by the copper corrosion liquid copper removed in enamel-covered wire.This thin slice is cut into the film that diameter is 5 centimetres, and then namely to obtain aperture be 11 micron thickness is the homogeneous aperture filter membrane of 100 microns with dry after distilled water, ethanol purge.
Claims (4)
1. a preparation method for homogeneous aperture filter membrane, is characterized in that, comprise the steps:
The first step, is assembled into the single thin film with orientation characteristic by the differently-oriented directivity that single-size nucleocapsid or doughnut edge are selected and is solidified by adhesive and obtain the fiber membrane sheet material with orientation characteristic;
Second step, is parallel to each other the fiber membrane sheet material with orientation characteristic according to the fiber in adjacent sheet and carries out superposing blend compounds and stick agent and fix the orientation fibers bulk being formed and built by single-size fibrous material;
3rd step, by orientation fibers bulk along fiber axis to vertical direction carry out cutting obtain by the nucleocapsid of single-size or the array plane thin slice of hollow structure fibrous material, wherein namely the array plane thin slice of nucleocapsid structure fibrous material obtains homogeneous aperture filter membrane through post processing after removal nuclear material, and the direct post processing of hollow structure fibrous material array plane thin slice is homogeneous aperture filter membrane.
2. the preparation method of a kind of homogeneous aperture according to claim 1 filter membrane, it is characterized in that, the aperture deviation average of described filter membrane is less than 5% of mean value.
3. the preparation method of a kind of homogeneous aperture according to claim 1 filter membrane, it is characterized in that, described removal nuclear material refers to by dissolving or corrode and is removed from Core-shell structure material by nuclear material.
4. the preparation method of a kind of homogeneous aperture according to claim 1 filter membrane, is characterized in that, described post processing comprises cleaning, drying, annealing.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201510919814.XA CN105363349A (en) | 2015-12-11 | 2015-12-11 | Preparation method of filter membrane with uniform pore size |
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| CN201510919814.XA CN105363349A (en) | 2015-12-11 | 2015-12-11 | Preparation method of filter membrane with uniform pore size |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109437092A (en) * | 2018-10-23 | 2019-03-08 | 中国工程物理研究院激光聚变研究中心 | A kind of encoding array structural composite material and preparation method thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6097832A (en) * | 1983-11-01 | 1985-05-31 | Jun Taga | Manufacture of porous film |
| EP0195860A1 (en) * | 1983-11-01 | 1986-10-01 | Jun Taga | Porous membranes and processes for producing the porous membranes |
| EP1616985A1 (en) * | 2004-07-09 | 2006-01-18 | Deutsche Rockwool Mineralwoll GmbH & Co. OHG | Manufacture of a mineral fibre web with substantially upright fibres |
| US20080023125A1 (en) * | 2006-07-28 | 2008-01-31 | E. I. Dupont De Nemours And Company | Processes for making fiber-on-end materials |
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2015
- 2015-12-11 CN CN201510919814.XA patent/CN105363349A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6097832A (en) * | 1983-11-01 | 1985-05-31 | Jun Taga | Manufacture of porous film |
| EP0195860A1 (en) * | 1983-11-01 | 1986-10-01 | Jun Taga | Porous membranes and processes for producing the porous membranes |
| EP1616985A1 (en) * | 2004-07-09 | 2006-01-18 | Deutsche Rockwool Mineralwoll GmbH & Co. OHG | Manufacture of a mineral fibre web with substantially upright fibres |
| US20080023125A1 (en) * | 2006-07-28 | 2008-01-31 | E. I. Dupont De Nemours And Company | Processes for making fiber-on-end materials |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109437092A (en) * | 2018-10-23 | 2019-03-08 | 中国工程物理研究院激光聚变研究中心 | A kind of encoding array structural composite material and preparation method thereof |
| CN109437092B (en) * | 2018-10-23 | 2020-10-23 | 中国工程物理研究院激光聚变研究中心 | Composite material with coding array structure and preparation method thereof |
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Application publication date: 20160302 |