CN102407038A - Syringe-driven filter able to filter viruses efficiently and its production method - Google Patents
Syringe-driven filter able to filter viruses efficiently and its production method Download PDFInfo
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- CN102407038A CN102407038A CN2011102694263A CN201110269426A CN102407038A CN 102407038 A CN102407038 A CN 102407038A CN 2011102694263 A CN2011102694263 A CN 2011102694263A CN 201110269426 A CN201110269426 A CN 201110269426A CN 102407038 A CN102407038 A CN 102407038A
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Abstract
The invention relates to a syringe-driven filter able to filter viruses efficiently and its production method. The syringe-driven filter comprises a filtering membrane which is characterized by consisting of a substrate and an electrostatic net spraying membrane. The production method includes: dissolving a polymer and adding it into an inorganic salt so as to obtain a homogeneous spinning solution; subjecting the obtained spinning solution to electrostatic net spraying, and depositing the electrostatic net spraying membrane containing two dimensional reticular fiber and unidimensional electrospun fiber on a receiving device adhered with the substrate, taking the obtained composite material as the filtering membrane and making it into a syringe-driven filter. The filtering membrane of the invention has a larger specific surface area which enhances flow velocity and filtration capacity and makes filtration easier, and also has small pore size, great porosity, thus being able to bear high pressure.
Description
Technical field
But the present invention relates to a kind of needle-based filter and production method thereof of high efficiency filter virus, is biomedical research equipment commonly used.
Background technology
Membrane separation technique is described as " one of new and high technology that mid-term 21st century is the most rising ", and it is the most noticeable that wherein microporous barrier is separated in biology, chemical analysis and pharmaceutical field application.Compare with existing separation process, the film separation process at liquid purifying, concentrate, separation field has its special advantages, the film separation process does not have phase transformation mostly, operation at normal temperatures, equipment and flow process are simple, easy realization of industrial amplification etc.Nearly 10 for many years, and the government of developed countries such as North America, Europe, Japan and large enterprises' associating drop into the huge fund developmental research.
Removing virus filtration is an important use in the membrane separation technique, is applied in widely in the high-technology fields such as bioengineering, pharmaceuticals industry, life science.And in the application study of laboratory correlation technique, the needle-based virus filter is a kind of conventional quick, convenient, reliable virus filtration instrument that uses.In needle-based virus filtration device, most critical be can filter virus membrane material.Present homemade needle-based is filtered filter and is divided into disposable and muptiple-use, organic system or water system, and specification has Φ 13 or Φ 25, is used for liquid phase or gas phase analysis sample filtering.Filtering material has: nylon, Kynoar, polytetrafluoroethylene (PTFE), cellulose mixture, cellulose acetate, glass fibre, polypropylene, polyether sulfone.
With the core filter membrane material that above-mentioned material carries out traditional melting and spraying, technology such as spunbond, coating has just obtained the needle-based filter.Though the filter membrane material by these traditional handicraft preparations has the viral efficient of certain filtration, because the restriction of technology more than the 0.3 μ m of this membrane material average fiber aperture, can't realize the high efficiency filter to virus.Though this type of homemade needle-based filter need not change film and cleaning filter; Saved complicated, time-consuming preparation, but still existed operating pressure low, service life is short; Cost is high; Aperture low inadequately (aperture is more than 300 nm), problem such as flow velocity is low, this has just limited the advance of product technology, the acceptance rate of product quality and the competitiveness of cost of goods manufactured.
Static spray network technology is the association technology in the electrostatic spinning process, just can realize static spray net through the technological parameter in the adjustment electrostatic spinning process.But it is the new method for preparing the compound multi-layer film material of one dimension electrospinning fibre and two-dimension netted tunica fibrosa as a kind of one-step method, has caused the extensive concern of academia and industrial quarters.Common one dimension electrospinning fibre and two-dimension netted film (average fibre diameter is less than 20 nm in the net) mutual superposition in the static spray net composite membrane finally form a kind of porous film material.This film has that fibre diameter is little, specific area is big, the aperture is little and the porosity advantages of higher, can effectively stop the invasion of deleterious particles such as bacterium, virus, has kept higher gas permeability simultaneously.
Summary of the invention
The purpose of this invention is to provide a kind of high to virus filtration efficient, can bear pressure high needle-based filter and production method thereof.
In order to achieve the above object, the invention provides a kind of needle-based filter, comprise filter membrane, it is characterized in that, described filter membrane comprises base material and static spray nethike embrane.
Preferably, described static spray nethike embrane contains two-dimension netted fiber and one dimension electrospinning fibre.
Preferably, described needle-based filter also comprises shell, and filter membrane is located in the shell, and the two ends of shell are respectively equipped with inlet union and outlet connection.
More preferably, described inlet union is taper hose connection or luer-lock joint.
More preferably, described outlet connection is taper hose connection or luer-slip joint.
More preferably, the material of described shell is polypropylene, high density polyethylene (HDPE), MBS (methacrylic acid-butadiene-styrene terpolymer), polyvinyl chloride, modacrylic, Merlon or polytetrafluoroethylene (PTFE).
The present invention also provides the production method of above-mentioned needle-based filter, it is characterized in that, comprising: with polymer dissolution, add inorganic salts, obtain the spinning solution of character homogeneous; The spinning solution of gained is carried out static spray net, and the static that will contain two-dimension netted fiber and one dimension electrospinning fibre sprays nethike embrane and is deposited on the receiving system that is attached with base material, and the composite of gained as filter membrane, is processed the needle-based filter.
Preferably; The condition of described static spray net is: temperature is that 20-35 ℃, relative humidity are 20 ~ 60 %; Spinning solution is input on the spinning nozzle of static spray net arrangement with the flow velocity of 0.5 ~ 6 mL/h; Distance between spinning nozzle and the receiving system (being receiving range) is 5 ~ 25 cm, and spinning voltage is 10 ~ 40 kV.
Preferably, described inorganic salts are: a kind of or mixture more than two kinds in sodium chloride, potassium chloride, calcium chloride, magnesium chloride, iron chloride, potassium hydroxide, NaOH, sodium carbonate, sodium acid carbonate, potash, silver nitrate, copper nitrate, sodium nitrate, potassium nitrate, sodium sulphate and the sodium sulfite.
Preferably, the percentage by weight solubility of the inorganic salts in the described spinning solution is 0.05 ~ 5%.
Preferably, described base material is one or more in nonwoven, copper mesh, iron net, aluminium net and the stainless (steel) wire.
Preferably, described polymer is one or more the mixture in nylon 6, nylon 66, nylon 1010, polyether sulfone, cellulose acetate, cellulose mixture, polytetrafluoroethylene (PTFE), Kynoar, improvement polyether sulfone, polyurethane, polyacrylic acid, polyvinyl alcohol, polyacrylonitrile, aramid fiber 1313, polybenzimidazoles, polypyrrole, polystyrene, ethyl cellulose, PEO, polymethyl methacrylate, PTT, polybutylene terephthalate (PBT), polysulfones and the poly butylene succinate.
Preferably, the used solvent of described polymer dissolution is one or more the mixture in formic acid, ethanol, acetate, N-N-dimethyl formamide, carrene, chloroform, N-N-dimethylacetylamide, ethanol, methyl alcohol, hexafluoroisopropanol, trifluoroacetic acid, acetone and the toluene.
Preferably, the weight percent concentration of the polymer in the described spinning solution is 5 ~ 30%.
Compared with prior art, the invention has the advantages that:
1. filter membrane of the present invention has bigger specific area, has increased flow velocity and filtration yield, also makes filtered fluid become and is more prone to, and have less aperture, bigger porosity, and the pressure that can bear is higher.
2. but static spray network technology one-step method provided by the invention obtains one dimension electrospinning fibre and the compound multi-layer film material of two-dimension netted tunica fibrosa, and the preparation process is simple, and cost is low.
3. the efficient anti-virus needle-based filter of the present invention's preparation can efficiently stop particulates such as bacterium, virus to pass through, and has kept gas permeability preferably simultaneously.
Description of drawings
Fig. 1 is the needle-based filter structure schematic representation;
Fig. 2 is needle-based filter profile figure;
Label declaration among the figure: 1-inlet union; The 2-shell; The 3-filter membrane; The 4-outlet connection.
The specific embodiment
Below in conjunction with embodiment, further the present invention is set forth in detail.The used all kinds of solvents of the spinning of using in following examples, inorganic salts all can crystalline substance pure reagent Co., Ltd be buied in Shanghai; Organic polymer all can buied on the market; The molecular weight of used nylon 6 is 18000 among the embodiment, and the molecular weight of nylon 66 is 15000, and the molecular weight of nylon 1010 is 14000, and the molecular weight of polyether sulfone is 50000 ~ 100000, and the molecular weight of Kynoar is 97000, the molecular weight 90000 of polyacrylonitrile; High voltage source is the DW-P303-1ACD8 type that east, Tianjin civilian high voltage source factory produces; The spinning solution induction system is the LSP02-113 type that Baoding LanGe constant flow pump Co., Ltd produces; Static spray net arrangement is the contrive equipment of Chinese invention patent CN101565878A.
Embodiment 1: needle-based filter and production method thereof
(1) at ambient temperature; The nylon 6 of 0.5 g is joined in the formic acid solvent of 9.5 g; Add 0.01g sodium chloride again; Rotating speed with 150 rpm on magnetic stirrer stirs 10 h, and until the spinning solution that obtains the character homogeneous, obtaining mass fraction is the nylon that contains sodium chloride 6 spinning solutions of 5 %.
(2) under room temperature, relative humidity are 20% condition; The speed of the nylon that is disposed 6 solution with 0.9 mL/h is transported on the spinning head; Spinning head connects the HV generator of 10 kV, carries out the effect of static spray net, at last with collect the nylon 6 static spray nethike embrane that contains two-dimension netted fiber and one dimension electrospinning fibre with the receiving system of copper mesh; Receiving range is 5cm, obtains nylon 6 static spray nethike embrane/copper mesh composite film material.
(3) gained nylon 6 static are sprayed nethike embrane/copper mesh composite film material as filter membrane; Carry out seamless link with taper flexible pipe inlet union, luer-slip outlet connection, polypropylene material shell through ultrasonic bonding, but finally obtain the needle-based filter of high efficiency filter virus.
(4) as shown in Figure 1, be the needle-based filter structure schematic representation, Fig. 2 is its profile, and described needle-based filter comprises filter membrane 3, and filter membrane 3 is located in the shell 2, and the two ends of shell 2 are respectively equipped with inlet union 1 and outlet connection 4.Described filter membrane 3 comprises base material and static spray nethike embrane.Described static spray nethike embrane contains two-dimension netted fiber and one dimension electrospinning fibre.Described needle-based filter carries out filter test with YY0286.1-2007 industry standard method to 25 ~ 120 nm viruses, and its filter efficiency is 99%, finds that with the GB/T7689.5-2001 standard testing the highest operating pressure that can bear is 8.5 bar.
Embodiment 2: needle-based filter and production method thereof
(1) at ambient temperature; The nylon 66 of 2 g is joined in the formic acid solvent of 7.85 g; Add 0.15 g potassium chloride; Rotating speed with 180 rpm on magnetic stirrer stirs 12 h, and until the spinning solution that obtains the character homogeneous, obtaining mass fraction is the nylon that contains potassium chloride 66 solution of 20 %.
(2) in room temperature; Relative humidity is under 25% the condition, the speed of the nylon that is disposed 66 solution with 1 mL/h to be transported on the spinning head, and spinning head connects the HV generator of 30 kV; Carry out the effect of static spray net; With collect the nylon 66 static spray nethike embrane that contains two-dimension netted fiber and one dimension electrospinning fibre with the receiving system of copper mesh, receiving range is 15 cm, obtains nylon 66 static spray nethike embrane/copper mesh composite film material at last.
(3) gained nylon 66 static are sprayed nethike embrane/copper mesh composite film material as filter membrane; Carry out seamless link with taper flexible pipe inlet union, taper flexible pipe outlet connection, polytetrafluoroethylene (PTFE) material shell through ultrasonic bonding, but finally obtain the needle-based filter of high efficiency filter virus.
(4) as shown in Figure 1, be the needle-based filter structure schematic representation, Fig. 2 is its profile, and described needle-based filter comprises filter membrane 3, and filter membrane 3 is located in the shell 2, and the two ends of shell 2 are respectively equipped with inlet union 1 and outlet connection 4.Described filter membrane 3 comprises base material and static spray nethike embrane.Described static spray nethike embrane contains two-dimension netted fiber and one dimension electrospinning fibre.Described needle-based filter carries out filter test with YY0286.1-2007 industry standard method to 25 ~ 120 nm viruses, and its filter efficiency is 99.5%, finds that with the GB/T7689.5-2001 standard testing the highest operating pressure that can bear is 8.3 bar.
Embodiment 3: needle-based filter and production method thereof
(1) at ambient temperature; The polyether sulfone of 0.7 g is joined in the N-N-solvent dimethylformamide of 9.25 g; Add 0.05 g sodium chloride again; Rotating speed with 220 rpm on magnetic stirrer stirs 15 h, and until the spinning solution that obtains the character homogeneous, obtaining mass fraction is the polyether sulfone solution that contains sodium chloride of 7 %.
(2) in room temperature; Relative humidity is under 25% the condition, the speed of the polyether sulfone solution that is disposed with 5 mL/h to be transported on the spinning head, and spinning head connects the HV generator of 40 kV; Carry out the effect of static spray net; With collect the polyether sulfone static spray nethike embrane that contains two-dimension netted fiber and one dimension electrospinning fibre with the receiving system of aluminium net, receiving range is 20 cm, obtains polyether sulfone static spray nethike embrane/aluminium net composite film material at last.
(3) gained polyether sulfone static is sprayed nethike embrane/aluminium net composite film material as filter membrane; Carry out seamless link with luer-lock inlet union, luer-slip outlet connection, high density polyethylene (HDPE) material shell through ultrasonic bonding, but finally obtain the needle-based filter of high efficiency filter virus.
(4) as shown in Figure 1, be the needle-based filter structure schematic representation, Fig. 2 is its profile, and described needle-based filter comprises filter membrane 3, and filter membrane 3 is located in the shell 2, and the two ends of shell 2 are respectively equipped with inlet union 1 and outlet connection 4.Described filter membrane 3 comprises base material and static spray nethike embrane.Described static spray nethike embrane contains two-dimension netted fiber and one dimension electrospinning fibre.Described needle-based filter carries out filter test with YY0286.1-2007 industry standard method to 25 ~ 120 nm viruses, and its filter efficiency is 98.9%, is standard law with GB/T7689.5-2001, and test finds that the highest operating pressure that can bear is 9.2 bar.
Embodiment 4: needle-based filter and production method thereof
(1) at ambient temperature; The Kynoar of 1 g is joined in the 8.9 gN-N-solvent dimethylformamides; Add 0.1 g silver nitrate again; Rotating speed with 150 rpm on magnetic stirrer stirs 16 h, and until the spinning solution that obtains the character homogeneous, obtaining mass fraction is the Kynoar solution that contains silver nitrate of 10 %.
(2) in room temperature; Relative humidity is under 30% the condition, the speed of the Kynoar solution that is disposed with 3 mL/h to be transported on the spinning head, and spinning head connects the HV generator of 30 kV; Carry out the effect of static spray net; With collect the Kynoar static spray nethike embrane that contains two-dimension netted fiber and one dimension electrospinning fibre with the receiving system of aluminium net, receiving range is 18 cm, obtains Kynoar static spray nethike embrane/aluminium net composite film material at last.
(3) gained Kynoar static is sprayed nethike embrane/aluminium net composite film material as filter membrane; Carry out seamless link with luer-lock inlet union, taper flexible pipe outlet connection, high density polyethylene (HDPE) material shell through ultrasonic bonding, but finally obtain the needle-based filter of high efficiency filter virus.
(4) as shown in Figure 1, be the needle-based filter structure schematic representation, Fig. 2 is its profile, and described needle-based filter comprises filter membrane 3, and filter membrane 3 is located in the shell 2, and the two ends of shell 2 are respectively equipped with inlet union 1 and outlet connection 4.Described filter membrane 3 comprises base material and static spray nethike embrane.Described static spray nethike embrane contains two-dimension netted fiber and one dimension electrospinning fibre.Described needle-based filter carries out filter test with YY0286.1-2007 industry standard method to 25 ~ 120 nm viruses, and its filter efficiency is 99.9%, is standard law with GB/T7689.5-2001, and test finds that the highest operating pressure that can bear is 9.6 bar.
Embodiment 5: needle-based filter and production method thereof
(1) at ambient temperature; The nylon 1010 of 1.5 g is joined in the formic acid solvent of 8.35 g; Add 0.15 g barium chloride again; Rotating speed with 100 rpm on magnetic stirrer stirs 10 h, and until the spinning solution that obtains the character homogeneous, obtaining mass fraction is the nylon 1010 solution that contains barium chloride of 15 %.
(2) in room temperature; Relative humidity is under 27% the condition, the speed of the nylon 1010 solution that is disposed with 0.9 mL/h to be transported on the spinning head, and spinning head connects the HV generator of 35 kV; Carry out the effect of static spray net; With collect the nylon 1010 static spray nethike embrane that contains two-dimension netted fiber and one dimension electrospinning fibre with the receiving system of copper mesh, receiving range is 15 cm, obtains nylon 1010 static spray nethike embrane/copper mesh composite film material at last.
(3) gained nylon 1010 static is sprayed nethike embrane/copper mesh composite film material as filter membrane; Carry out seamless link with luer-lock inlet union, luer-slip outlet connection, polytetrafluoroethylene (PTFE) material shell through ultrasonic bonding, but finally obtain the needle-based filter of high efficiency filter virus.
(4) as shown in Figure 1, be the needle-based filter structure schematic representation, Fig. 2 is its profile, and described needle-based filter comprises filter membrane 3, and filter membrane 3 is located in the shell 2, and the two ends of shell 2 are respectively equipped with inlet union 1 and outlet connection 4.Described filter membrane 3 comprises base material and static spray nethike embrane.Described static spray nethike embrane contains two-dimension netted fiber and one dimension electrospinning fibre.Described needle-based filter carries out filter test with YY0286.1-2007 industry standard method to 25 ~ 120 nm viruses, and its filter efficiency is 99.99%, is standard law with GB/T7689.5-2001, and test finds that the highest operating pressure that can bear is 8.9 bar.
Embodiment 6: needle-based filter and production method thereof
(1) at ambient temperature; The polyacrylonitrile of 1 g is joined in the N-N-dimethylacetamide solvent of 8.85 g; Add 0.15 g calcium chloride again; Rotating speed with 150 rpm on magnetic stirrer stirs 17 h, and until the spinning solution that obtains the character homogeneous, obtaining mass fraction is the polyacrylonitrile solution that contains calcium chloride of 10 %.
(2) in room temperature; Relative humidity is under 25% the condition, the speed of the polyacrylonitrile solution that is disposed with 2 mL/h to be transported on the spinning head, and spinning head connects the HV generator of 30 kV; Carry out the effect of static spray net; With collect the polyacrylonitrile static spray nethike embrane that contains two-dimension netted fiber and one dimension electrospinning fibre with the receiving system of iron net, receiving range is 15 cm, obtains polyacrylonitrile static spray nethike embrane/iron net composite film material at last.
(3) gained polyacrylonitrile static is sprayed nethike embrane/iron net composite film material as filter membrane; Carry out seamless link with taper flexible pipe inlet union, luer-slip outlet connection, polypropylene material shell through ultrasonic bonding, but finally obtain the needle-based filter of high efficiency filter virus.
(4) as shown in Figure 1, be the needle-based filter structure schematic representation, Fig. 2 is its profile, and described needle-based filter comprises filter membrane 3, and filter membrane 3 is located in the shell 2, and the two ends of shell 2 are respectively equipped with inlet union 1 and outlet connection 4.Described filter membrane 3 comprises base material and static spray nethike embrane.Described static spray nethike embrane contains two-dimension netted fiber and one dimension electrospinning fibre.Described needle-based filter carries out filter test with YY0286.1-2007 industry standard method to 25 ~ 120 nm viruses, and its filter efficiency is 99.5%, is standard law with GB/T7689.5-2001, and test finds that the highest operating pressure that can bear is 8.5 bar.
Claims (10)
1. a needle-based filter comprises filter membrane (3), it is characterized in that, described filter membrane (3) comprises base material and static spray nethike embrane.
2. needle-based filter as claimed in claim 1 is characterized in that, described static spray nethike embrane contains two-dimension netted fiber and one dimension electrospinning fibre.
3. needle-based filter as claimed in claim 1 is characterized in that, described filter membrane (3) is located in the shell (2), and the two ends of shell (1) are respectively equipped with inlet union (1) and outlet connection (4).
4. needle-based filter as claimed in claim 3 is characterized in that, described inlet union (1) is taper hose connection or luer-lock joint, and described outlet connection (4) is taper hose connection or luer-slip joint.
5. needle-based filter as claimed in claim 3 is characterized in that, the material of described shell (2) is polypropylene, high density polyethylene (HDPE), MBS, polyvinyl chloride, modacrylic, Merlon or polytetrafluoroethylene (PTFE).
6. the production method of the described needle-based filter of claim 1 is characterized in that, comprising: with polymer dissolution, add inorganic salts, obtain the spinning solution of character homogeneous; The spinning solution of gained is carried out static spray net, and the static that will contain two-dimension netted fiber and one dimension electrospinning fibre sprays nethike embrane and is deposited on the receiving system that is attached with base material, and the composite of gained as filter membrane (3), is processed the needle-based filter.
7. the production method of needle-based filter as claimed in claim 7; It is characterized in that; The condition of described static spray net is: temperature is that 20-35 ℃, relative humidity are 20 ~ 60%; Spinning solution is input on the spinning nozzle of static spray net arrangement with the flow velocity of 0.5 ~ 6 mL/h, and the distance between spinning nozzle and the receiving system is 5 ~ 25 cm, and spinning voltage is 10 ~ 40 kV.
8. the production method of needle-based filter as claimed in claim 7; It is characterized in that described inorganic salts are: a kind of or mixture more than two kinds in sodium chloride, potassium chloride, calcium chloride, magnesium chloride, iron chloride, potassium hydroxide, NaOH, sodium carbonate, sodium acid carbonate, potash, silver nitrate, copper nitrate, sodium nitrate, potassium nitrate, sodium sulphate and the sodium sulfite.
9. the production method of needle-based filter as claimed in claim 7 is characterized in that, the percentage by weight solubility of the inorganic salts in the described spinning solution is 0.05 ~ 5%.
10. the production method of needle-based filter as claimed in claim 7 is characterized in that, described base material is one or more in nonwoven, copper mesh, iron net, aluminium net and the stainless (steel) wire.
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| CN2011102694263A CN102407038A (en) | 2011-09-13 | 2011-09-13 | Syringe-driven filter able to filter viruses efficiently and its production method |
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| Application Number | Priority Date | Filing Date | Title |
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| CN2011102694263A CN102407038A (en) | 2011-09-13 | 2011-09-13 | Syringe-driven filter able to filter viruses efficiently and its production method |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20020175449A1 (en) * | 2001-05-16 | 2002-11-28 | Benjamin Chu | Apparatus and methods for electrospinning polymeric fibers and membranes |
| CN101538567A (en) * | 2008-03-20 | 2009-09-23 | 杭州优思达生物技术有限公司 | Method for quickly processing filter-type micro nucleic acid clinical samples |
| CN101565878A (en) * | 2009-05-27 | 2009-10-28 | 东华大学 | Ultrathin nanometer cobweb/nanometer fiber composite protective material manufacturing device |
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2011
- 2011-09-13 CN CN2011102694263A patent/CN102407038A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20020175449A1 (en) * | 2001-05-16 | 2002-11-28 | Benjamin Chu | Apparatus and methods for electrospinning polymeric fibers and membranes |
| CN101538567A (en) * | 2008-03-20 | 2009-09-23 | 杭州优思达生物技术有限公司 | Method for quickly processing filter-type micro nucleic acid clinical samples |
| CN101565878A (en) * | 2009-05-27 | 2009-10-28 | 东华大学 | Ultrathin nanometer cobweb/nanometer fiber composite protective material manufacturing device |
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Application publication date: 20120411 |