CN106757788A - A kind of filter for infusion filtering nano fibrous membrane and preparation method thereof - Google Patents
A kind of filter for infusion filtering nano fibrous membrane and preparation method thereof Download PDFInfo
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- CN106757788A CN106757788A CN201611213539.0A CN201611213539A CN106757788A CN 106757788 A CN106757788 A CN 106757788A CN 201611213539 A CN201611213539 A CN 201611213539A CN 106757788 A CN106757788 A CN 106757788A
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- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
- D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
- D04H1/70—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres
- D04H1/72—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres the fibres being randomly arranged
- D04H1/728—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres the fibres being randomly arranged by electro-spinning
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
- D01F1/103—Agents inhibiting growth of microorganisms
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/44—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds
- D01F6/52—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds of polymers of unsaturated carboxylic acids or unsaturated esters
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/88—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds
- D01F6/94—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds of other polycondensation products
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- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
- D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
- D04H1/40—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
- D04H1/42—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties characterised by the use of certain kinds of fibres insofar as this use has no preponderant influence on the consolidation of the fleece
- D04H1/4282—Addition polymers
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- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
- D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
- D04H1/40—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
- D04H1/42—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties characterised by the use of certain kinds of fibres insofar as this use has no preponderant influence on the consolidation of the fleece
- D04H1/4326—Condensation or reaction polymers
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- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
- D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
- D04H1/40—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
- D04H1/42—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties characterised by the use of certain kinds of fibres insofar as this use has no preponderant influence on the consolidation of the fleece
- D04H1/4374—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties characterised by the use of certain kinds of fibres insofar as this use has no preponderant influence on the consolidation of the fleece using different kinds of webs, e.g. by layering webs
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- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
- D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
- D04H1/40—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
- D04H1/54—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties by welding together the fibres, e.g. by partially melting or dissolving
- D04H1/559—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties by welding together the fibres, e.g. by partially melting or dissolving the fibres being within layered webs
Abstract
The invention discloses a kind of filter for infusion filtering nano fibrous membrane and preparation method thereof, wherein preparation method includes：(1) polymer and electrolyte are added in solvent, heated at constant temperature is stirred to dissolving, obtains polymer spinning solution；Nano-Ag particles are added in polymer spinning solution, antibacterial spinning solution is obtained；(2) electrostatic spinning after polymer spinning solution deaeration is obtained into separating layer；After antibacterial spinning solution deaeration antibiotic layer will be obtained in separating layer surface electrostatic spinning；(3) drying of the static spinning membrane containing separating layer and antibiotic layer, hot pressing and the sterilizing that will be obtained in step (2), obtain the filter for infusion filtering nano fibrous membrane with antibacterial action.Preparation method is simple of the present invention is easy, can facilitate and be accurately controlled the aperture of film, meets the filtering of transfusion liquid under different situations, while being easily achieved industrialization large-scale production.
Description
Technical field
The present invention relates to bio-medical separation material field, more particularly to a kind of filter for infusion filtering nano fibrous membrane and
Its preparation method.
Background technology
China's infusion preparation sells more than 10,000,000,000 bottles every year, although China halts tertiary hospitals Transfusion For Outpatients in many ground one after another,
But still there is hundreds of thousands of them to be got killed because of transfusion every year.Transfusion injection is numerous the reason for cause death, but impurity in transfusion finished product into
It is a major reason.Impurity in infusion process be mainly make up a prescription during produce 5~10 microns of particle, cutting ampoule to produce
A large amount of 5~20 μm of particles of life, puncture cannula, rubber produces a large amount of 5~20 μm of particles, a large amount of 5~20 μm of particulates of glass, plastic bottle
Come off, in addition with the trace of bacteria that uncontrollable factor is produced.Different bacterium it is not of uniform size, for example bacillus is about 0.5
~10 μm, wide about 0.2~1.0 μm, the diameter of coccus is about 0.3~1.2 μm, and spirillar bacterium is about 3~50 μm.
In order to prevent adverse reaction of the impurity to patient, filter for infusion is provided with transfusion device.Filter for infusion filtering is used
Film is the core material of filter for infusion, current Clinical practice it is main have poly tetrafluoroethylene, polypropylene screen, polyester nucleopore membranes,
Cellulose mixture film and nylon membrane etc..
For example, the Chinese patent literature of Publication No. CN202289067U discloses a kind of transfusion filter device, filter membrane
Using poly tetrafluoroethylene, the film being made of biaxial tension, basic unit is non-woven fabrics, is bonded between two-layer, and basic unit's direction is entered
Liquid mouthful.The polytetrafluoroethyltwo two-way stretch film thickness that patent is used is 1.5 μm~200 μm.This patent uses polytetrafluoroethylene (PTFE)
Biaxially oriented film, by the aperture of different sizes of micropore on polytetrafluoroethyltwo two-way stretch film, is filtered as filter medium
Various impurity.It is micro- that the patent document of Publication No. CN104826197A discloses a kind of efficient low-resistance impurity for venous transfusion
Grain filtration system, the filter medium that the woven filter cloth of use is bonded with dimethyl silicone polymer filter membrane.The hole of compound filter cloth
Footpath is 4 μm, and it also ensure that filter effect while mechanical property is improved.
But, the aperture of common filter membrane is different from 0.2 micron to more than ten micron, simultaneously because the structure of filter membrane
And material is different, the decay of the filtering velocity and filtering velocity of filtering film differs greatly (bibliography：Li Yuanchun, disposable infusion
Device Medieine qilter membrane flux depression experimental study, Beijing biomedical engineering [J], 2000,19,105-107).
The major technique of currently manufactured filter for infusion film includes inversion of phases, stretching, acupuncture, melt-blown etc..But existing system
Membrane technology generally existing filming technology is complicated, pore-size distribution is uneven, pore size control is difficult, film porosity is too small, nonreactive
The defects such as bacterium effect, these defects limit the use scope and extensive special pore size distribution membrane material system of bio-medical seperation film
Make.Nano fibrous membrane is the novel film materials for occurring in recent years, is porosity (bibliography high the characteristics of its is maximum：
V.Thavasi, G.Singh, S.Ramakrishna, Electrospun nanofibers in energy and
Environmental applications [J], Energy Environ.Sci., 2008,1：205-221.), this give and receive
The characteristics of rice tunica fibrosa high flux and low pressure drop.In addition, nano fibrous membrane also have that pore size is adjustable, equipment simple,
The features such as adaptability to raw material is wide, fluid separation field have huge potentiality (Shichao Zhang, Hui Liu, Xia Yin,
Jianyong Yu, Bin Ding, Anti-deformed Polyacrylonitrile/Polysulfone Composite
Membrane with Binary Structures for Effective Air Filtration [J], ACS
Appl.Mater.Interfaces, 2016,8 (12)：8086-8095.).The particle diameter of Nano Silver is right mostly in 25 rans
Various pathogenic microorganisms such as bacillus, coccus, chlamydia trachomatis have strong suppression and killing action.In infusion and transfusion
During, there is no one bottle of transfusion liquid to accomplish integral asepsis, so far also not using the electrostatic with antibacterial action
Spinning nano fibrous membrane is used as research and the report of filter for infusion filtering film.Therefore, convenient, efficient, safety, antibacterial are developed
Filter for infusion filtering with film turn into its current prior development direction.
The content of the invention
The invention provides a kind of filter for infusion filtering nano fibrous membrane and preparation method thereof, filter for infusion filtering is used
Nano fibrous membrane is made up of separating layer and antibiotic layer two-layer, and its preparation method is simple and convenient, the film good anti-bacterial effect, porosity
Greatly, pore size is adjustable, and retention scope is wide, and flux is big, and drag minimization in filter process, good mechanical property meets bio-medical
The antibacterial of transfusion Chinese medicine liquid and filtration.
A kind of preparation method of filter for infusion filtering nano fibrous membrane, including：
(1) polymer and electrolyte are added in solvent, heated at constant temperature is stirred to dissolving, obtain polymer spinning molten
Liquid；Nano-Ag particles are added in polymer spinning solution, antibacterial spinning solution is obtained；
Described polymer is polyether sulfone, polyurethanes, polyacrylate, Polyhedral Oligomeric silsesquioxane, poly-
At least one in urethane, Poly(D,L-lactide-co-glycolide, polyacrylonitrile；In described polymer spinning solution, polymer
Mass percent concentration be 10~35%.
Polymer solution concentration is higher, and its viscosity is bigger, and surface tension is bigger, and leave after nozzle drop breakup ability with
Surface tension increases and weakens.Generally when other conditions are constant, with the diameter of the increase fiber of polymer solution concentration
Increase.
Preferably, described polymer is polyether sulfone, polyacrylate or polyurethane；Described polymer spinning solution
In, the mass percent concentration of polymer is 15~30%.
Similar to conventional solution-polymerized SBR, the shaping of the property of solvent to electrospun fibers has very big with structure and performance
Influence, the volatility of solvent plays an important role to the form of fiber.Preferably, the solvent is N, N- dimethyl methyls
One kind in acid amides, DMA, 1-METHYLPYRROLIDONE, tetrahydrofuran, acetone, ethanol, dimethyl sulfoxide (DMSO) or
It is several.
Described electrolyte is lithium chloride, sodium chloride or potassium chloride, in described polymer spinning solution, the matter of electrolyte
Amount percent concentration is 0.001~0.01%.
Polymer is dissolved in organic solvent, can form the solution of transparent stable homogeneous, adds the mesh of qs Electrolyte
Be increase solution electric conductivity, make polymer solution in high voltage electric field be easier spray.
The particle diameter of described nano-Ag particles is 20~50nm；In described antibacterial spinning solution, the matter of nano-Ag particles
Measure 0.1~0.5% of the quality for polymer.
It is further preferred that the particle diameter of described nano-Ag particles is 20~30nm；In described antibacterial spinning solution, receive
The quality of rice Argent grain is the 0.1~0.5% of the quality of polymer.The particle diameter of 20~30nm nano-Ag particles doping effect compared with
Good, spinning is easy.If the particle diameter of nano-Ag particles is excessive, nanofiber easily produces defect, if the grain of nano-Ag particles
Footpath is too small, and Nano Silver is easily embedded in fiber, and antibacterial effect is bad.In addition, if can shadow when the concentration of nano-Ag particles is too high
Film forming is rung, antibacterial effect is not obvious when concentration is too low.
The particle diameter of Nano Silver mostly in 25 rans, to various pathogenic microorganisms such as bacillus, coccus, chlamydia trachomatis all
There is strong suppression and killing action.
Preferably, to ultrasonic 2~4 hours after addition nano-Ag particles in polymer spinning solution.Using ultrasonic wave added
During scattered method makes nano-Ag particles dispersed with polymer spinning solution, while may also function as the effect of froth breaking.
(2) electrostatic spinning after polymer spinning solution deaeration is obtained into separating layer；To divide after antibacterial spinning solution deaeration
Absciss layer surface electrostatic spinning obtains antibiotic layer；
Described separating layer is the main body of filter for infusion filtering film, the filtration in filter for infusion, and described is anti-
Bacterium layer is to spin a thin layer on separating layer, and thickness is 10 μm or so, plays antibacterial action.
Preferably, separating layer is identical with the procedure parameter of the electrostatic spinning of antibiotic layer, described procedure parameter：Voltage is
6~50kV, the fltting speed of spinning solution is 0.3~5mL/min, and the relative humidity of spinning process air is 30~60%, ring
Border temperature be 10~35 DEG C, electrostatic spinning syringe needle internal diameter be 0.06~1.55mm, needle point to receive roller distance be 5~
30cm, the rotating speed for receiving roller is 4~60r/min.
As the voltage applied to polymer solution increases, the electrostatic force increase of system, the splitting ability of drop accordingly increases
By force, the diameter of gained fiber tends to reducing；After polymer drop sprays through nozzle, in atmosphere along with solvent volatilization thread
While, polymer concentration is solidified into fiber, is finally received by reception roller.
It is further preferred that described procedure parameter：Voltage is 20~30kV, the fltting speed of spinning solution for 0.8~
1.2mL/min, the relative humidity of spinning process air is 40~50%, and environment temperature is 30~35 DEG C, in electrostatic spinning syringe needle
Footpath is 0.1~0.5mm, and needle point to the distance for receiving roller is 15~20cm, and the rotating speed for receiving roller is 30~60r/min.
Electrostatic spinning is carried out under the procedure parameter, the fibre diameter of the nano fibrous membrane for obtaining, aperture, porosity meet
The demand of biological medicine filter for infusion.
Preferably, the electrostatic spinning time of separating layer is 4~8 hours, the electrostatic spinning time of antibiotic layer is 0.2~1
Hour.
The electrostatic spinning time is more long, and the thickness of the film of gained is bigger, the nanofiber obtained under the electrostatic spinning time
The thickness of film, its separating layer and antibiotic layer causes that it has stronger mechanical strength and good antibacterial effect.
(3) static spinning membrane containing separating layer and antibiotic layer that will be obtained in step (2) is dried, hot pressing and sterilization disappear
Poison, obtains the filter for infusion filtering nano fibrous membrane with antibacterial action.
Preferably, hot pressing time is 1~4h, hot pressing temperature is 60~250 DEG C, and hot pressing pressure is 0.1~5Mpa.
The method of described sterilizing can be gone out using hot-air sterilization, moist hear heat test, radiation sterilization, ultraviolet
Bacterium method, ethylene oxide sterilizing method, ozone sterilization method etc..
Hot pressing is in order to the nanofiber of the free state for allowing electrostatic spinning to be formed is combined into a film, the choosing of hot pressing temperature
Selecting will select according to the property of polymer, the fusing point of general slightly below polymer.
Present invention also offers a kind of filter for infusion filtering nano fibrous membrane prepared using above-mentioned preparation method.
Preferably, a diameter of 0.1~5 μm of fiber in described filter for infusion filtering nano fibrous membrane, average hole
Footpath is 0.1~5 μm, and porosity is 70~90%, and thickness is 70~200 μm, and water contact angle is 10 °~70 °.
The nanofiber membrane porosity is big, and retention scope is wide, and flux is big, drag minimization in filter process, good mechanical property,
Meet antibacterial and the filtration of bio-medical transfusion Chinese medicine liquid.
Preferably, a kind of preparation method of filter for infusion filtering nano fibrous membrane, including：
(1) polyether sulfone and electrolyte are added to the mixed solvent of 1-METHYLPYRROLIDONE and DMF
In, the mass ratio of 1-METHYLPYRROLIDONE and DMF is 1: 5~6.5, and heated at constant temperature is stirred to dissolving, is obtained
The mass percent concentration of polyether sulfone is 15~30% polymer spinning solution；
Nano-Ag particles are added in polymer spinning solution, antibacterial spinning solution, the quality of nano-Ag particles is obtained
It is the 0.1~0.5% of the quality of polyether sulfone；
(2) electrostatic spinning after polymer spinning solution deaeration is obtained into separating layer；To divide after antibacterial spinning solution deaeration
Absciss layer surface electrostatic spinning obtains antibiotic layer；
Separating layer is identical with the procedure parameter of the electrostatic spinning of antibiotic layer, described procedure parameter：Voltage is 20~30kV,
The fltting speed of spinning solution is 0.8~1.2mL/min, and the relative humidity of spinning process air is 40~50%, environment temperature
It it is 30~35 DEG C, electrostatic spinning syringe needle internal diameter is 0.1~0.5mm, needle point to the distance for receiving roller is 15~20cm, receives rolling
The rotating speed of cylinder is 30~60r/min；
The electrostatic spinning time of separating layer is 4~8 hours, and the electrostatic spinning time of antibiotic layer is 0.2~1 hour；
(3) static spinning membrane containing separating layer and antibiotic layer that will be obtained in step (2) is dried, hot pressing and sterilization disappear
Poison, obtains the filter for infusion filtering nano fibrous membrane with antibacterial action；
Hot pressing time is 1~2h, and hot pressing temperature is 200~250 DEG C, and hot pressing pressure is 4~5Mpa.
Use the preparation method can the separating layer thickness of obtained filter for infusion filtering nano fibrous membrane be 90~100 μ
M, antibiotic layer thickness is 8~10 μm, and average pore size is 5 μm, and pore-size distribution is 4.6~5.2 μm, and porosity is 85~90%.Can
For the filtering of transfusion liquid of being grown up.
Preferably, a kind of preparation method of filter for infusion filtering nano fibrous membrane, including：
(1) polymethylacrylic acid 2- hydroxyl ethyl esters and electrolyte are added in ethanol, or polyurethane and electrolyte is added
It is added in DMF and tetrahydrofuran, the mass ratio of DMF and tetrahydrofuran is 1: 1~2,
Heated at constant temperature is stirred to dissolving, obtain the mass percent concentration of polymethylacrylic acid 2- hydroxyl ethyl esters or polyurethane for 15~
25% polymer spinning solution；
Nano-Ag particles are added in polymer spinning solution, antibacterial spinning solution, the quality of nano-Ag particles is obtained
It is the 0.1~0.5% of the quality of polyether sulfone；
(2) electrostatic spinning after polymer spinning solution deaeration is obtained into separating layer；To divide after antibacterial spinning solution deaeration
Absciss layer surface electrostatic spinning obtains antibiotic layer；
Separating layer is identical with the procedure parameter of the electrostatic spinning of antibiotic layer, described procedure parameter：Voltage is 20~30kV,
The fltting speed of spinning solution is 0.8~1.2mL/min, and the relative humidity of spinning process air is 40~50%, environment temperature
It it is 30~35 DEG C, electrostatic spinning syringe needle internal diameter is 0.1~0.5mm, needle point to the distance for receiving roller is 15~20cm, receives rolling
The rotating speed of cylinder is 30~60r/min；
The electrostatic spinning time of separating layer is 4~8 hours, and the electrostatic spinning time of antibiotic layer is 0.2~1 hour；
(3) static spinning membrane containing separating layer and antibiotic layer that will be obtained in step (2) is dried, hot pressing and sterilization disappear
Poison, obtains the filter for infusion filtering nano fibrous membrane with antibacterial action；
Hot pressing time is 1~2h, and hot pressing temperature is 80~120 DEG C, and hot pressing pressure is 3~5Mpa.
Use the preparation method can the separating layer thickness of obtained filter for infusion filtering nano fibrous membrane be 100~110 μ
M, antibiotic layer thickness is 8~10 μm, and average pore size is 1.2 μm, and pore-size distribution is 1.0~1.4 μm, and porosity is 80~85%.
Can be used for the filtering of child infusion liquid.
Compared with prior art, beneficial effects of the present invention are：
(1) preparation method is simple of the present invention is easy, can facilitate and be accurately controlled the aperture of film, meets different situations
The filtering of lower transfusion liquid, while being easily achieved industrialization large-scale production；
(2) present invention prepare nano fibrous membrane surface cover one layer of antibacterial film, can effectively kill transfusion liquid in
The different size of bacterium of remaining；
(3) nano fibrous membrane prepared by the present invention can significantly improve that traditional infusion filter membrane flux is small and resistance is big lacks
Fall into, filter for infusion filtering film is used in the case where extras are not increased.
Brief description of the drawings
Fig. 1 is the scanning electron microscope (SEM) photograph of separating layer in nano fibrous membrane prepared by embodiment 1；
Fig. 2 is the scanning electron microscope (SEM) photograph of antibiotic layer in nano fibrous membrane prepared by embodiment 1.
Specific embodiment
Embodiment 1
The present embodiment is prepared for the filter for infusion filtering nano fibrous membrane with antibacterial action that a kind of aperture is 5 μm,
Can be used for the filtering of adult's transfusion liquid, specific preparation method is comprised the following steps：
(1) 0.004 part of 30 parts of polyether sulfone and sodium chloride are dissolved in 10 parts of 1-METHYLPYRROLIDONEs and 60 parts of N, N- dimethyl
In the mixed solvent of formamide, constant temperature is stirred 2 hours under 50 DEG C of water-baths, obtains the polymer spinning solution of stable homogeneous, will
The solution left standstill is overnight removing bubble；
To the nano-Ag particles added in polymer spinning solution equivalent to the 0.3% of polyether sulfone quality, nano-Ag particles
A diameter of 30nm, by mixed liquor in ultrasonic pond ultrasound 2 hours, nano-Ag particles therein is completely dispersed in the solution
Obtain antibacterial spinning solution；
(2) polymer spinning solution is carried out into the electrostatic spinning time 4.5 hours, nanofiber separating layer is obtained, by antibacterial
Spinning solution carries out 0.5 hour electrostatic spinning time prepared nanofiber antibiotic layer；Wherein syringe needle is flat mouth syringe needle, pin
Head connects high-voltage power cathode, and electrostatic spinning liquid is extruded by medical injection pump.The procedure parameter of electrostatic spinning is：Syringe needle internal diameter
0.41mm, high-voltage power voltage 30kV, electrostatic spinning extruded velocity 0.8mL/h, needle point to the distance for receiving roller is 15cm, is connect
Receive drum rotation speed 10r/min, diameter of cylinder 10cm, 30 DEG C of environment temperature, envionmental humidity 40~50%, obtained in this process
The thickness of the polyether sulfone nano fibrous membrane containing antibiotic layer is total up to 100 μm, and the wherein thickness of separating layer is 90 μm, antibiotic layer
Thickness is 10 μm, and mean flow pore footpath size is 5 μm, and pore size distribution range is 4.6~5.2 μm, and porosity is 90%；
(3) polyether sulfone nano fibrous membrane obtained in step (2) is dried 12 hours at 80 DEG C, makes solvent therein complete
After evaporating, polyether sulfone nano fibrous membrane is placed in the middle of two smooth stainless steel plates, is forced into 5Mpa, the hot pressing 2 at 220 DEG C
Hour takes out, and through sterilizing, obtains final product filter for infusion filtering nano fibrous membrane.
The filter for infusion A of the filter for infusion filtering nano fibrous membrane that will be prepared added with embodiment 1 be not added with filter for infusion
The filter for infusion B of filtering nano fibrous membrane does transfusion contrast test, defeated compared with filter for infusion B under identical transfusion height
The flow-reduction rate of liquid filter A is less than 10%, and the impurity rejection to being wherein more than 5 μm is 100%；
Tolerance test is done to filter for infusion filtering nano fibrous membrane prepared by embodiment 1, after continuously filtering 10 times, its
Flux and cutoff performance decline degree and are respectively less than 1%；
Antibiotic property test is done to filter for infusion filtering nano fibrous membrane prepared by embodiment 1, is found under ESEM
Filter for infusion filtering is little with the bacterial number on nano fibrous membrane surface, and the ne ar and normal bacteria form phase for occurring
Than there occurs change, represent that bacterium has been killed.
In nano fibrous membrane manufactured in the present embodiment, the scanning electron microscope (SEM) photograph of separating layer is as shown in figure 1, the scanning electricity of antibiotic layer
Mirror figure is as shown in Figure 2.
Embodiment 2
The present embodiment is prepared for the filter for infusion filtering nanofiber with antibacterial action that a kind of aperture is 1.2 μm
Film, can be used for the filtering of child infusion liquid, and specific preparation method is comprised the following steps：
(1) 0.002 part of 25 parts of polymethylacrylic acid 2- hydroxyl ethyl esters and lithium chloride are dissolved in 75 parts of ethanol, in 40 DEG C of water-baths
Lower constant temperature is stirred 4 hours, obtains the polymer spinning solution of stable homogeneous, by the solution left standstill overnight removing bubble；
To the Nano Silver added in polymer spinning solution equivalent to the 0.5% of polymethylacrylic acid 2- hydroxyl ethyl ester quality
Grain, a diameter of 30nm of nano-Ag particles is ultrasonic 2 hours in ultrasonic pond by mixed liquor, makes nano-Ag particles therein complete
Full dispersion obtains antibacterial spinning solution in the solution；
(2) polymer spinning solution is carried out into 5 hours electrostatic spinning time prepared nanofiber separating layer, by antibacterial spinning
Solution carries out 0.5 hour electrostatic spinning time prepared nanofiber antibiotic layer；Wherein syringe needle is flat mouth syringe needle, and syringe needle connects
High-voltage power cathode, electrostatic spinning liquid is extruded by medical injection pump.The procedure parameter of electrostatic spinning is：Syringe needle internal diameter
0.41mm, high-voltage power voltage 20kV, electrostatic spinning extruded velocity 0.8mL/h, needle point to the distance for receiving roller is 15cm, is connect
Receive drum rotation speed 30r/min, diameter of cylinder 20cm, 30 DEG C of environment temperature, envionmental humidity 40~50%, obtained in this process
The thickness of the polymethylacrylic acid 2- hydroxyl ethyl ester nano fibrous membranes containing antibiotic layer is total up to 110 μm, the wherein thickness of separating layer
It is 100 μm, the thickness of antibiotic layer is 10 μm, and mean flow pore footpath size is 1.2 μm, and pore size distribution range is 1.0~1.4 μm,
Porosity is 80%；
(3) polymethylacrylic acid 2- hydroxyl ethyl esters nano fibrous membrane obtained in step (2) is dried 12 hours at 80 DEG C, is made
After solvent therein is evaporated completely, polymethylacrylic acid 2- hydroxyl ethyl ester nano fibrous membranes are placed in two smooth stainless steel plates
Between, 3Mpa is forced into, hot pressing is taken out for 2 hours at 120 DEG C, through sterilizing, obtains final product filter for infusion filtering nano fibrous membrane.
The filter for infusion A of the filter for infusion filtering nano fibrous membrane that will be prepared added with embodiment 2 be not added with filter for infusion
The filter for infusion B of filtering nano fibrous membrane does transfusion contrast test, defeated compared with filter for infusion B under identical transfusion height
The flow-reduction rate of liquid filter A is less than 10%, and the impurity rejection to being wherein more than 1.2 μm is 100%；
Tolerance test is done to filter for infusion filtering nano fibrous membrane prepared by embodiment 2, after continuously filtering 10 times, its
Flux and cutoff performance decline degree and are respectively less than 1%；
Antibiotic property test is done to filter for infusion filtering nano fibrous membrane prepared by embodiment 2, is found under ESEM
Filter for infusion filtering is little with the bacterial number on nano fibrous membrane surface, and the ne ar and normal bacteria form phase for occurring
Than there occurs change, represent that bacterium has been killed.
Embodiment 3
The present embodiment is prepared for the filter for infusion filtering nanofiber with antibacterial action that a kind of aperture is 1.2 μm
Film, can be used for the filtering of child infusion liquid, and specific preparation method is comprised the following steps：
(1) 0.004 part of 19 parts of polyurethane and lithium chloride are dissolved in 27 parts of DMFs and 54 parts of tetrahydrochysene furans
In muttering, constant temperature is stirred 4 hours under 45 DEG C of water-baths, obtains the polymer spinning solution of stable homogeneous, by the solution left standstill overnight
To remove bubble；
To the nano-Ag particles added in polymer spinning solution equivalent to the 0.4% of polyurethane quality, Nano Silver
A diameter of 25nm of grain, mixed liquor is ultrasonic 2 hours in ultrasonic pond, nano-Ag particles therein is thoroughly dispersed in solution
In obtain antibacterial spinning solution；
(2) polymer spinning solution is carried out into 5 hours electrostatic spinning time prepared nanofiber separating layer, by antibacterial spinning
Solution carries out 0.5 hour electrostatic spinning time prepared nanofiber antibiotic layer；Wherein syringe needle is flat mouth syringe needle, and syringe needle connects
High-voltage power cathode, electrostatic spinning liquid is extruded by medical injection pump.The procedure parameter of electrostatic spinning is：Syringe needle internal diameter
0.41mm, high-voltage power voltage 20kV, electrostatic spinning extruded velocity 1.2mL/h, needle point to the distance for receiving roller is 20cm, is connect
Receive drum rotation speed 60r/min, diameter of cylinder 10cm, 30 DEG C of environment temperature, envionmental humidity 40~50%, obtained in this process
The thickness of the polyurethane nano fibrous membrane containing antibiotic layer is total up to 110 μm, and the wherein thickness of separating layer is 100 μm, antibacterial
The thickness of layer is 10 μm, and mean flow pore footpath size is 1.2 μm, and pore size distribution range is 1.0~1.3 μm, and porosity is 85%；
(3) polyurethane nano fibrous membrane obtained in step (2) is dried 12 hours at 60 DEG C, makes solvent therein complete
After evaporating entirely, polymethylacrylic acid 2- hydroxyl ethyl ester nano fibrous membranes are placed in the middle of two smooth stainless steel plates, be forced into
5Mpa, hot pressing is taken out for 2 hours at 80 DEG C, through sterilizing, obtains final product filter for infusion filtering nano fibrous membrane.
The filter for infusion A of the filter for infusion filtering nano fibrous membrane that will be prepared added with embodiment 3 be not added with filter for infusion
The filter for infusion B of filtering nano fibrous membrane does transfusion contrast test, defeated compared with filter for infusion B under identical transfusion height
The flow-reduction rate of liquid filter A is less than 10%, and the impurity rejection to being wherein more than 1.2 μm is 100%；
Tolerance test is done to filter for infusion filtering nano fibrous membrane prepared by embodiment 3, after continuously filtering 10 times, its
Flux and cutoff performance decline degree and are respectively less than 1%；
Antibiotic property test is done to filter for infusion filtering nano fibrous membrane prepared by embodiment 3, is found under ESEM
Filter for infusion filtering is little with the bacterial number on nano fibrous membrane surface, and the ne ar and normal bacteria form phase for occurring
Than there occurs change, represent that bacterium has been killed.
Claims (8)
1. a kind of preparation method of filter for infusion filtering nano fibrous membrane, it is characterised in that including：
(1) polymer and electrolyte are added in solvent, heated at constant temperature is stirred to dissolving, obtains polymer spinning solution；Will
Nano-Ag particles are added in polymer spinning solution, obtain antibacterial spinning solution；
(2) electrostatic spinning after polymer spinning solution deaeration is obtained into separating layer；By after antibacterial spinning solution deaeration in separating layer
Surface electrostatic spinning obtains antibiotic layer；
(3) drying of the static spinning membrane containing separating layer and antibiotic layer, hot pressing and the sterilizing that will be obtained in step (2), obtain
To the filter for infusion filtering nano fibrous membrane with antibacterial action.
2. the preparation method of filter for infusion filtering nano fibrous membrane according to claim 1, it is characterised in that described
Polymer is polyether sulfone, polyurethanes, polyacrylate, Polyhedral Oligomeric silsesquioxane, polyurethane, polylactic acid-glycolic
At least one in acetic acid copolymer, polyacrylonitrile；In described polymer spinning solution, the mass percent of polymer is dense
Spend is 10~35%.
3. the preparation method of filter for infusion filtering nano fibrous membrane according to claim 1, it is characterised in that described
The particle diameter of nano-Ag particles is 20~50nm；In described antibacterial spinning solution, the quality of nano-Ag particles is the matter of polymer
The 0.1~0.5% of amount.
4. the preparation method of filter for infusion filtering nano fibrous membrane according to claim 1, it is characterised in that step
(2) in, separating layer is identical with the procedure parameter of the electrostatic spinning of antibiotic layer, described procedure parameter：Voltage is 6~50kV, is spun
The fltting speed of silk solution is 0.3~5mL/min, and the relative humidity of spinning process air is 30~60%, and environment temperature is 10
~35 DEG C, electrostatic spinning syringe needle internal diameter is 0.06~1.55mm, and needle point to the distance for receiving roller is 5~30cm, receives roller
Rotating speed be 4~60r/min.
5. the preparation method of filter for infusion filtering nano fibrous membrane according to claim 4, it is characterised in that separating layer
The electrostatic spinning time be 4~8 hours, electrostatic spinning time of antibiotic layer is 0.2~1 hour.
6. the preparation method of filter for infusion filtering nano fibrous membrane according to claim 5, it is characterised in that step
(3) in, hot pressing time is 1~4h, and hot pressing temperature is 60~250 DEG C, and hot pressing pressure is 0.1~5Mpa.
7. a kind of filter for infusion filtering nano fibrous membrane, it is characterised in that defeated according to any one of claim 1~6
It is prepared by the preparation method of liquid filter filtering nano fibrous membrane.
8. filter for infusion filtering nano fibrous membrane according to claim 7, it is characterised in that described filter for infusion mistake
A diameter of 0.1~5 μm of fiber in filter nano fibrous membrane, average pore size is 0.1~5 μm, and porosity is 70~90%, thickness
It it is 70~200 μm, water contact angle is 10 °~70 °.
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| CN113279139A (en) * | 2021-04-26 | 2021-08-20 | 杭州诗蓝过滤科技有限公司 | Preparation method of high-strength fluffy melt-blown fabric |
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