CN106757788B - 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
- Publication number
- CN106757788B CN106757788B CN201611213539.0A CN201611213539A CN106757788B CN 106757788 B CN106757788 B CN 106757788B CN 201611213539 A CN201611213539 A CN 201611213539A CN 106757788 B CN106757788 B CN 106757788B
- Authority
- CN
- China
- Prior art keywords
- filter
- infusion
- spinning
- polymer
- spinning solution
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Classifications
-
- 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
-
- 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
-
- 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
-
- 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
-
- 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 membranes and preparation method thereof, and wherein preparation method includes: that polymer and electrolyte are added in solvent by (1), and heated at constant temperature is stirred to dissolution, 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；Antibiotic layer will be obtained in separating layer surface electrostatic spinning after antibacterial spinning solution deaeration；(3) containing the drying of the static spinning membrane of separating layer and antibiotic layer, hot pressing and sterilizing, the filter for infusion filtering nano fibrous membrane with antibacterial action will be obtained obtained in step (2).Preparation method of the present invention is simple and easy to do, can facilitate and be accurately controlled the aperture of film, meets the filtering for medical fluid of being infused under different situations, while being easily industrialized large-scale production.
Description
Technical field
The present invention relates to bio-medical separation material fields more particularly to a kind of filtering of filter for infusion with nano fibrous membrane and
Preparation method.
Background technique
China's infusion preparation sells 10,000,000,000 bottles or more every year, although tertiary hospitals Transfusion For Outpatients are halted one after another in the more ground in China,
But still there is hundreds of thousands of them to get killed because of infusion every year.The impurity that infusion injection causes dead reason numerous, but is infused in finished product at
For a major reason.Impurity in infusion process is mainly the particle that 5~10 microns are generated during making up a prescription, and cutting ampoule produces
Raw a large amount of 5~20 μm of particles, puncture cannula, rubber generate a large amount of 5~20 μm of particles, a large amount of 5~20 μm of particles of glass, plastic bottle
It falls off, in addition there are the trace of bacteria that uncontrollable factor generates.Different bacterium it is not of uniform size, such as bacillus is about 0.5
~10 μm, about 0.2~1.0 μm wide, the diameter of coccus is about 0.3~1.2 μm, and spirillar bacterium is about 3~50 μm.
Adverse reaction of the impurity to patient in order to prevent, is provided with filter for infusion on infusion apparatus.Filter for infusion filtering is used
Film is the core material of filter for infusion, at present clinical use mainly have polytetrafluoroethylene film, 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 polytetrafluoroethylene film, using film made of biaxial tension, base is non-woven fabrics, is bonded between two layers, base towards into
Liquid mouth.The polytetrafluoroethyltwo two-way stretch film thickness that patent uses is 1.5 μm~200 μm.This patent uses polytetrafluoroethylene (PTFE)
Biaxially oriented film passes through the different aperture of micropore size on polytetrafluoroethyltwo two-way stretch film, filtering 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 and dimethyl silicone polymer filter membrane of use are bonded.The hole of compound filter cloth
Diameter is 4 μm, also ensures filter effect while improving mechanical property.
But the aperture of common filter membrane is micron different from 0.2 micron to more than ten, simultaneously because the structure of filter membrane
And material is different, the decaying 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, needle thorn, melt-blown etc..But existing system
The generally existing filming technology of membrane technology is complicated, pore-size distribution is uneven, pore size control is difficult, the porosity of film is too small, nonreactive
The defects of bacterium effect, these defects limit the use scope and extensive special pore size distribution membrane material system of bio-medical seperation film
It makes.Nano fibrous membrane is the novel film materials occurred in recent years, maximum feature be porosity it is high (bibliography:
V.Thavasi, G.Singh, S.Ramakrishna, Electrospun nanofibers in energy and
Environmental applications [J], Energy Environ.Sci., 2008,1:205-221.), this give receive
The characteristics of rice tunica fibrosa high throughput and low pressure drop.In addition to this, nano fibrous membrane also have pore size is adjustable, equipment is 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 partial size of nano silver is right mostly in 25 rans
A variety of pathogenic microorganisms such as bacillus, coccus, chlamydia trachomatis have strong inhibition and killing effect.In infusion and infusion
In the process, it can accomplish integral asepsis without one bottle of infusion medical fluid, there are no using the electrostatic with antibacterial action so far
Research and report of the spinning nano fibrous membrane as filter for infusion filtering film.Therefore, convenient, efficient, safety, antibacterial are developed
Filter for infusion filtering with film become its current prior development direction.
Summary of the invention
The present 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 of separating layer and two layers of antibiotic layer, and preparation method is simple and convenient, the film good anti-bacterial effect, porosity
Greatly, pore size is adjustable, and retention range is wide, and flux is big, and drag minimization in filter process, good mechanical property meets bio-medical
The antibacterial and filtration of infusion Chinese medicine liquid.
A kind of filter for infusion filtering preparation method of nano fibrous membrane, comprising:
(1) polymer and electrolyte are added in solvent, heated at constant temperature is stirred to dissolution, and it is molten to obtain polymer spinning
Liquid；Nano-Ag particles are added in polymer spinning solution, antibacterial spinning solution is obtained；
The polymer is polyether sulfone, polyurethanes, polyacrylate, Polyhedral Oligomeric silsesquioxane, gathers
At least one of urethane, poly lactide-glycolide acid, polyacrylonitrile；In the polymer spinning solution, polymer
Mass percent concentration be 10~35%.
Polymer solution concentration is higher, and viscosity is bigger, and surface tension is bigger, and leave after nozzle drop breakup ability with
Surface tension increases and weakens.Usually when other conditions are constant, with the diameter of the increase fiber of polymer solution concentration
Increase.
Preferably, the polymer is polyether sulfone, polyacrylate or polyurethane；The polymer spinning solution
In, the mass percent concentration of polymer is 15~30%.
Similar to conventional solution-polymerized SBR, the property of solvent has the forming of electrospun fibers and structure and performance very big
Influence, the volatility of solvent plays an important role to the form of fiber.Preferably, the solvent is N, N- dimethyl methyl
One of amide, n,N-dimethylacetamide, N-Methyl pyrrolidone, tetrahydrofuran, acetone, ethyl alcohol, dimethyl sulfoxide or
It is several.
The electrolyte is lithium chloride, sodium chloride or potassium chloride, in the polymer spinning solution, the matter of electrolyte
Measuring percent concentration is 0.001~0.01%.
Polymer is dissolved in organic solvent, can form the solution of transparent stable homogeneous, and the mesh of qs Electrolyte is added
Be increase solution electric conductivity, make polymer solution in high voltage electric field be easier spray.
The partial size of the nano-Ag particles is 20~50nm；In the antibacterial spinning solution, the matter of nano-Ag particles
Amount is the 0.1~0.5% of the quality of polymer.
It is further preferred that the partial size of the nano-Ag particles is 20~30nm；In the antibacterial spinning solution, receive
The quality of rice Argent grain is the 0.1~0.5% of the quality of polymer.The partial size of 20~30nm nano-Ag particles doping effect compared with
Good, spinning is easy.If the partial size of nano-Ag particles is excessive, nanofiber is easy to produce defect, if the grain of nano-Ag particles
Diameter is too small, and nano silver is easy to be embedded in fiber, and antibacterial effect is bad.In addition, if the concentration of nano-Ag particles too Gao Shihui shadow
Film forming is rung, antibacterial effect is unobvious when concentration is too low.
The partial size of nano silver is mostly in 25 rans, all to a variety of pathogenic microorganisms such as bacillus, coccus, chlamydia trachomatis
There are strong inhibition and killing effect.
Preferably, being added into polymer spinning solution after nano-Ag particles ultrasound 2~4 hours.Using ultrasonic wave added
The method of dispersion make nano-Ag particles it is evenly dispersed with polymer spinning solution in, while may also function as the effect of defoaming.
(2) electrostatic spinning after polymer spinning solution deaeration is obtained into separating layer；It will divide after antibacterial spinning solution deaeration
Absciss layer surface electrostatic spinning obtains antibiotic layer；
The separating layer is the main body of filter for infusion filtering film, and the filtration in filter for infusion, described is anti-
Bacterium layer is a thin layer spun on separating layer, with a thickness of 10 μm or so, plays antibacterial action.
Preferably, separating layer is identical as the procedure parameter of the electrostatic spinning of antibiotic layer, the procedure parameter: voltage is
6~50kV, the fltting speed of spinning solution are 0.3~5mL/min, and the relative humidity of spinning process air is 30~60%, ring
Border temperature is 10~35 DEG C, and electrostatic spinning syringe needle internal diameter is 0.06~1.55mm, needle point to receive the distance of roller for 5~
30cm, the revolving speed for receiving roller is 4~60r/min.
As the voltage applied to polymer solution increases, the electrostatic force of system increases, and the splitting ability of drop accordingly increases
By force, the diameter of gained fiber tends to reduce；Polymer drop is after nozzle sprays, in air along in solvent volatilization thread
While, polymer concentration is solidified into fiber, is finally received roller reception.
It is further preferred that the procedure parameter: voltage is 20~30kV, the fltting speed of spinning solution is 0.8~
1.2mL/min, the relative humidity of spinning process air are 40~50%, and environment temperature is 30~35 DEG C, in electrostatic spinning syringe needle
Diameter is 0.1~0.5mm, and needle point to the distance for receiving roller is 15~20cm, and the revolving speed for receiving roller is 30~60r/min.
Electrostatic spinning is carried out under the procedure parameter, fibre diameter, aperture, the porosity of obtained nano fibrous membrane 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 longer, and the thickness of resulting film is bigger, the nanofiber obtained under the electrostatic spinning time
The thickness of film, separating layer and antibiotic layer makes it with stronger mechanical strength and good antibacterial effect.
(3) by containing the static spinning membrane of separating layer and antibiotic layer, dry, hot pressing and sterilization disappear obtained in step (2)
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 the sterilizing can be gone out using hot-air sterilization, moist hear heat test, radiation sterilization, ultraviolet light
Bacterium method, ethylene oxide sterilizing method, ozone sterilization method etc..
Hot pressing is in order to which the nanofiber for 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.
The present invention also provides a kind of filter for infusion filtering nano fibrous membranes prepared using above-mentioned preparation method.
Preferably, the diameter of fiber is 0.1~5 μm in the filter for infusion filtering nano fibrous membrane, average hole
Diameter is 0.1~5 μm, and porosity is 70~90%, and film thickness is 70~200 μm, and water contact angle is 10 °~70 °.
The nanofiber membrane porosity is big, and retention range is wide, and flux is big, drag minimization in filter process, good mechanical property,
Meet the antibacterial and filtration of bio-medical infusion Chinese medicine liquid.
Preferably, a kind of filter for infusion filtering preparation method of nano fibrous membrane, comprising:
(1) polyether sulfone and electrolyte are added to the mixed solvent of N-Methyl pyrrolidone and n,N-Dimethylformamide
In, the mass ratio of N-Methyl pyrrolidone and n,N-Dimethylformamide is 1: 5~6.5, and heated at constant temperature is stirred to dissolution, is obtained
The polymer spinning solution that the mass percent concentration of polyether sulfone is 15~30%；
Nano-Ag particles are added in polymer spinning solution, antibacterial spinning solution, the quality of nano-Ag particles are 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；It will divide after antibacterial spinning solution deaeration
Absciss layer surface electrostatic spinning obtains antibiotic layer；
Separating layer is identical as the procedure parameter of the electrostatic spinning of antibiotic layer, the 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 is 30~35 DEG C, electrostatic spinning syringe needle internal diameter is 0.1~0.5mm, and needle point to the distance for receiving roller is 15~20cm, receives rolling
The revolving 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) by containing the static spinning membrane of separating layer and antibiotic layer, dry, hot pressing and sterilization disappear obtained in step (2)
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.
Using the preparation method can filter for infusion filtering nano fibrous membrane obtained separating layer with a thickness of 90~100 μ
M, for antibiotic layer with a thickness of 8~10 μm, average pore size is 5 μm, and pore-size distribution is 4.6~5.2 μm, and porosity is 85~90%.It can
Filtering for adult infusion medical fluid.
Preferably, a kind of filter for infusion filtering preparation method of nano fibrous membrane, comprising:
(1) polymethylacrylic acid 2- hydroxyl ethyl ester and electrolyte are added in ethyl alcohol, or polyurethane and electrolyte is added
It being added in n,N-Dimethylformamide and tetrahydrofuran, the mass ratio of n,N-Dimethylformamide and tetrahydrofuran is 1: 1~2,
Heated at constant temperature is stirred to dissolution, and the mass percent concentration for obtaining polymethylacrylic acid 2- hydroxyl ethyl ester or polyurethane is 15~
25% polymer spinning solution；
Nano-Ag particles are added in polymer spinning solution, antibacterial spinning solution, the quality of nano-Ag particles are 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；It will divide after antibacterial spinning solution deaeration
Absciss layer surface electrostatic spinning obtains antibiotic layer；
Separating layer is identical as the procedure parameter of the electrostatic spinning of antibiotic layer, the 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 is 30~35 DEG C, electrostatic spinning syringe needle internal diameter is 0.1~0.5mm, and needle point to the distance for receiving roller is 15~20cm, receives rolling
The revolving 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) by containing the static spinning membrane of separating layer and antibiotic layer, dry, hot pressing and sterilization disappear obtained in step (2)
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.
Using the preparation method can filter for infusion filtering nano fibrous membrane obtained separating layer with a thickness of 100~110 μ
M, for antibiotic layer with a thickness of 8~10 μm, average pore size is 1.2 μm, and pore-size distribution is 1.0~1.4 μm, and porosity is 80~85%.
It can be used for the filtering of child infusion medical fluid.
Compared with prior art, the invention has the benefit that
(1) preparation method of the present invention is simple and easy to do, can facilitate and be accurately controlled the aperture of film, meet different situations
The filtering of lower infusion medical fluid, while being easily industrialized large-scale production；
(2) nanofiber film surface prepared by the present invention covers one layer of antibacterial film, can effectively kill in infusion medical fluid
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 what resistance was big lacks
It falls into, uses filter for infusion filtering in the case where not increasing extras with film.
Detailed description of the invention
Fig. 1 is the scanning electron microscope (SEM) photograph of separating layer in the nano fibrous membrane of the preparation of embodiment 1；
Fig. 2 is the scanning electron microscope (SEM) photograph of antibiotic layer in the nano fibrous membrane of the preparation of embodiment 1.
Specific embodiment
Embodiment 1
The present embodiment is prepared for a kind of filter for infusion filtering nano fibrous membrane with antibacterial action that aperture is 5 μm,
It can be used for the filtering of adult infusion medical fluid, specific preparation method comprises the following steps:
(1) 10 parts of N-Methyl pyrrolidones and 60 parts of N, N- dimethyl are dissolved in by 30 parts and 0.004 part of sodium chloride of polyether sulfone
The in the mixed solvent of formamide, constant temperature stirs 2 hours under 50 DEG C of water-baths, obtains the polymer spinning solution of stable homogeneous, will
The solution left standstill is overnight to remove bubble；
0.3% nano-Ag particles for being equivalent to polyether sulfone quality, nano-Ag particles are added into polymer spinning solution
Diameter be 30nm, by mixed liquor in ultrasonic pond ultrasound 2 hours, be completely dispersed nano-Ag particles therein in the solution
Obtain antibacterial spinning solution；
(2) polymer spinning solution is carried out the electrostatic spinning time 4.5 hours, nanofiber separating layer is made, by antibacterial
Spinning solution carries out the electrostatic spinning time 0.5 hour obtained nanofiber antibiotic layer；Wherein syringe needle is flat mouth syringe needle, needle
Head connects high-voltage power cathode, and electrostatic spinning liquid in medical injection pump by squeezing out.The procedure parameter of electrostatic spinning are as follows: 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%, made from this process
The thickness of polyether sulfone nano fibrous membrane containing antibiotic layer is total up to 100 μm, wherein separating layer with a thickness of 90 μm, antibiotic layer
With a thickness of 10 μm, mean flow pore diameter size is 5 μm, and pore size distribution range is 4.6~5.2 μm, porosity 90%；
(3) polyether sulfone nano fibrous membrane made from step (2) is 12 hours dry at 80 DEG C, keep solvent therein complete
After evaporating, polyether sulfone nano fibrous membrane is placed among two smooth stainless steel plates, 5Mpa is forced into, the hot pressing 2 at 220 DEG C
Hour takes out, through sterilizing to get filter for infusion filtering nano fibrous membrane.
By the filter for infusion A of the filter for infusion filtering nano fibrous membrane prepared added with embodiment 1 and filter for infusion is not added
The filter for infusion B of filtering nano fibrous membrane does infusion contrast test, defeated compared with filter for infusion B under identical infusion height
The flow-reduction rate of liquid filter A is 100% to the impurity rejection for being wherein greater than 5 μm less than 10%；
The filter for infusion filtering prepared to embodiment 1 does tolerance test with nano fibrous membrane, after continuous filtering 10 times,
Flux and cutoff performance decline degree are respectively less than 1%；
The filter for infusion filtering prepared to embodiment 1 does antibiotic property test with nano fibrous membrane, finds under scanning electron microscope
The bacterial number ne ar and normal bacteria form phase seldom, and occur of filter for infusion filtering nanofiber film surface
Than being changed, indicate 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 of antibiotic layer is electric
Mirror figure is as shown in Figure 2.
Embodiment 2
The present embodiment is prepared for a kind of filter for infusion filtering nanofiber with antibacterial action that aperture is 1.2 μm
Film can be used for the filtering of child infusion medical fluid, and specific preparation method comprises the following steps:
(1) 25 parts and 0.002 part of lithium chloride of polymethylacrylic acid 2- hydroxyl ethyl ester are dissolved in 75 parts of ethyl alcohol, in 40 DEG C of water-baths
Lower constant temperature stirs 4 hours, obtains the polymer spinning solution of stable homogeneous, by the solution left standstill overnight to remove bubble；
0.5% nano silver for being equivalent to polymethylacrylic acid 2- hydroxyl ethyl ester quality is added into polymer spinning solution
Grain, the diameter of nano-Ag particles is 30nm, and mixed liquor is 2 hours ultrasonic in ultrasonic pond, keeps nano-Ag particles therein complete
Full dispersion obtains antibacterial spinning solution in the solution；
(2) polymer spinning solution is subjected to the electrostatic spinning time 5 hours obtained nanofiber separating layers, by antibacterial spinning
Solution carries out the electrostatic spinning time 0.5 hour obtained nanofiber antibiotic layer；Wherein syringe needle is flat mouth syringe needle, and syringe needle connects
High-voltage power cathode, electrostatic spinning liquid in medical injection pump by squeezing out.The procedure parameter of electrostatic spinning are as follows: 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%, made from this process
The thickness of polymethylacrylic acid 2- hydroxyl ethyl ester nano fibrous membrane containing antibiotic layer is total up to 110 μm, wherein the thickness of separating layer
Be 100 μm, antibiotic layer with a thickness of 10 μm, mean flow pore diameter 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 ester nano fibrous membrane made from step (2) is 12 hours dry at 80 DEG C, make
After solvent therein evaporates completely, polymethylacrylic acid 2- hydroxyl ethyl ester nano fibrous membrane is placed in two smooth stainless steel plates
Between, it is forced into 3Mpa, is taken out within hot pressing 2 hours at 120 DEG C, through sterilizing to get filter for infusion filtering nano fibrous membrane.
By the filter for infusion A of the filter for infusion filtering nano fibrous membrane prepared added with embodiment 2 and filter for infusion is not added
The filter for infusion B of filtering nano fibrous membrane does infusion contrast test, defeated compared with filter for infusion B under identical infusion height
The flow-reduction rate of liquid filter A is 100% to the impurity rejection for being wherein greater than 1.2 μm less than 10%；
The filter for infusion filtering prepared to embodiment 2 does tolerance test with nano fibrous membrane, after continuous filtering 10 times,
Flux and cutoff performance decline degree are respectively less than 1%；
The filter for infusion filtering prepared to embodiment 2 does antibiotic property test with nano fibrous membrane, finds under scanning electron microscope
The bacterial number ne ar and normal bacteria form phase seldom, and occur of filter for infusion filtering nanofiber film surface
Than being changed, indicate that bacterium has been killed.
Embodiment 3
The present embodiment is prepared for a kind of filter for infusion filtering nanofiber with antibacterial action that aperture is 1.2 μm
Film can be used for the filtering of child infusion medical fluid, and specific preparation method comprises the following steps:
(1) 27 parts of n,N-Dimethylformamide and 54 parts of tetrahydro furans are dissolved in by 19 parts and 0.004 part of lithium chloride of polyurethane
In muttering, constant temperature is stirred 4 hours under 45 DEG C of water-baths, obtains the polymer spinning solution of stable homogeneous, which is stayed overnight
To remove bubble；
0.4% nano-Ag particles for being equivalent to polyurethane quality, nano silver are added into polymer spinning solution
The diameter of grain is 25nm, and mixed liquor is 2 hours ultrasonic in ultrasonic pond, and nano-Ag particles therein is made to be thoroughly dispersed in solution
In obtain antibacterial spinning solution；
(2) polymer spinning solution is subjected to the electrostatic spinning time 5 hours obtained nanofiber separating layers, by antibacterial spinning
Solution carries out the electrostatic spinning time 0.5 hour obtained nanofiber antibiotic layer；Wherein syringe needle is flat mouth syringe needle, and syringe needle connects
High-voltage power cathode, electrostatic spinning liquid in medical injection pump by squeezing out.The procedure parameter of electrostatic spinning are as follows: 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%, made from this process
The thickness of polyurethane nano fibrous membrane containing antibiotic layer is total up to 110 μm, wherein separating layer with a thickness of 100 μm, antibacterial
Layer with a thickness of 10 μm, mean flow pore diameter size is 1.2 μm, and pore size distribution range is 1.0~1.3 μm, porosity 85%；
(3) polyurethane nano fibrous membrane made from step (2) is 12 hours dry at 60 DEG C, keep solvent therein complete
After evaporating entirely, polymethylacrylic acid 2- hydroxyl ethyl ester nano fibrous membrane is placed among two smooth stainless steel plates, is forced into
5Mpa takes out, through sterilizing to get filter for infusion filtering nano fibrous membrane for hot pressing 2 hours at 80 DEG C.
By the filter for infusion A of the filter for infusion filtering nano fibrous membrane prepared added with embodiment 3 and filter for infusion is not added
The filter for infusion B of filtering nano fibrous membrane does infusion contrast test, defeated compared with filter for infusion B under identical infusion height
The flow-reduction rate of liquid filter A is 100% to the impurity rejection for being wherein greater than 1.2 μm less than 10%；
The filter for infusion filtering prepared to embodiment 3 does tolerance test with nano fibrous membrane, after continuous filtering 10 times,
Flux and cutoff performance decline degree are respectively less than 1%；
The filter for infusion filtering prepared to embodiment 3 does antibiotic property test with nano fibrous membrane, finds under scanning electron microscope
The bacterial number ne ar and normal bacteria form phase seldom, and occur of filter for infusion filtering nanofiber film surface
Than being changed, indicate that bacterium has been killed.
Claims (4)
1. the preparation method that nano fibrous membrane is used in a kind of filter for infusion filtering characterized by comprising
(1) polymer and electrolyte are added in solvent, heated at constant temperature is stirred to dissolution, obtains polymer spinning solution；It will
Nano-Ag particles are added in polymer spinning solution, obtain antibacterial spinning solution；
The partial size of the nano-Ag particles is 20 ~ 50nm；In the antibacterial spinning solution, the quality of nano-Ag particles is poly-
Close the 0.1 ~ 0.5% of the quality of object；
(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；
Separating layer is identical as the procedure parameter of the electrostatic spinning of antibiotic layer, the procedure parameter: voltage is 20 ~ 30kV, spinning
The fltting speed of solution is 0.8 ~ 1.2mL/min, and the relative humidity of spinning process air is 40 ~ 50%, and environment temperature is 30 ~ 35
DEG C, electrostatic spinning syringe needle internal diameter is 0.1 ~ 0.5mm, and needle point to the distance for receiving roller is 15 ~ 20cm, and the revolving speed for receiving roller is
30~60r/min；
(3) it is obtained obtained in step (2) containing the drying of the static spinning membrane of separating layer and antibiotic layer, hot pressing and sterilizing
To the filter for infusion filtering nano fibrous membrane with antibacterial action；
Hot pressing time is 1 ~ 4h, and hot pressing temperature is 60 ~ 250 DEG C, and hot pressing pressure is 0.1 ~ 5Mpa.
2. the preparation method that nano fibrous membrane is used in filter for infusion filtering according to claim 1, which is characterized in that described
Polymer is polyether sulfone, polyurethanes, polyacrylate, Polyhedral Oligomeric silsesquioxane, polyurethane, polylactic acid-glycolic
At least one of acetic acid copolymer, polyacrylonitrile；In the polymer spinning solution, the mass percent of polymer is dense
Degree is 10 ~ 35%.
3. the preparation method that nano fibrous membrane is used in filter for infusion filtering according to claim 1, which is characterized in that separating layer
The electrostatic spinning time be 4 ~ 8 hours, electrostatic spinning time of antibiotic layer is 0.2 ~ 1 hour.
4. a kind of filter for infusion filtering nano fibrous membrane, which is characterized in that described in any item infusions according to claim 1 ~ 3
It is prepared by the preparation method of filter filtering nano fibrous membrane.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611213539.0A CN106757788B (en) | 2016-12-23 | 2016-12-23 | A kind of filter for infusion filtering nano fibrous membrane and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611213539.0A CN106757788B (en) | 2016-12-23 | 2016-12-23 | A kind of filter for infusion filtering nano fibrous membrane and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN106757788A CN106757788A (en) | 2017-05-31 |
| CN106757788B true CN106757788B (en) | 2019-07-30 |
Family
ID=58920601
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201611213539.0A Active CN106757788B (en) | 2016-12-23 | 2016-12-23 | A kind of filter for infusion filtering nano fibrous membrane and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106757788B (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113279139B (en) * | 2021-04-26 | 2022-06-17 | 杭州诗蓝过滤科技有限公司 | Preparation method of high-strength fluffy melt-blown fabric |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1953286A1 (en) * | 2007-02-01 | 2008-08-06 | Nisshinbo Industries, Inc. | Fabric and mask |
| CN101559327A (en) * | 2009-05-08 | 2009-10-21 | 东华大学 | Nanometre-sized fibre liquid separation composite film and preparation method thereof |
| CN102425039A (en) * | 2011-09-26 | 2012-04-25 | 常州绿之源高分子材料有限公司 | Method for preparing water-soluble chitosan fibrous membrane |
| CN103361885A (en) * | 2013-06-28 | 2013-10-23 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of antibacterial silk fibroin fibrous membrane |
| CN103451849A (en) * | 2012-05-30 | 2013-12-18 | 中国科学院理化技术研究所 | Nano-silver containing polybutylene succinate nano-fiber membrane, preparation method thereof and application |
| CN103520999A (en) * | 2012-07-06 | 2014-01-22 | 北京服装学院 | Antibacterial composite nanometer fiber high-efficiency air filtering material and preparation method thereof |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20130033794A (en) * | 2011-09-27 | 2013-04-04 | 한국전자통신연구원 | Filter fabrication method and the filter fomred thereby |
-
2016
- 2016-12-23 CN CN201611213539.0A patent/CN106757788B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1953286A1 (en) * | 2007-02-01 | 2008-08-06 | Nisshinbo Industries, Inc. | Fabric and mask |
| CN101559327A (en) * | 2009-05-08 | 2009-10-21 | 东华大学 | Nanometre-sized fibre liquid separation composite film and preparation method thereof |
| CN102425039A (en) * | 2011-09-26 | 2012-04-25 | 常州绿之源高分子材料有限公司 | Method for preparing water-soluble chitosan fibrous membrane |
| CN103451849A (en) * | 2012-05-30 | 2013-12-18 | 中国科学院理化技术研究所 | Nano-silver containing polybutylene succinate nano-fiber membrane, preparation method thereof and application |
| CN103520999A (en) * | 2012-07-06 | 2014-01-22 | 北京服装学院 | Antibacterial composite nanometer fiber high-efficiency air filtering material and preparation method thereof |
| CN103361885A (en) * | 2013-06-28 | 2013-10-23 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of antibacterial silk fibroin fibrous membrane |
Also Published As
| Publication number | Publication date |
|---|---|
| CN106757788A (en) | 2017-05-31 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Aruchamy et al. | Electrospun nanofibers, nanocomposites and characterization of art: Insight on establishing fibers as product | |
| Stojanovska et al. | A review on non-electro nanofibre spinning techniques | |
| Rodríguez et al. | Electrospinning cellulosic nanofibers for biomedical applications: structure and in vitro biocompatibility | |
| Feng et al. | Recent progress in the preparation, characterization, and applications of nanofibers and nanofiber membranes via electrospinning/interfacial polymerization | |
| Shepa et al. | Electrospinning through the prism of time | |
| AK S et al. | Fabrication of poly (Caprolactone) nanofibers by electrospinning | |
| Yousefzadeh et al. | A note on the 3D structural design of electrospun nanofibers | |
| WO2015027769A1 (en) | Novel enhancing electrostatic spinning nanofiber membrane, producing method thereof, and device applied to method | |
| El Fawal | Polymer nanofibers electrospinning: A review | |
| CN106702598B (en) | A kind of preparation method of degradable graphene composite electrospun tunica fibrosa | |
| CN102086565A (en) | Polylactic acid antibacterial nanofiber membrane and preparation method thereof | |
| Yadav et al. | Electrospinning: an efficient biopolymer-based micro-and nanofibers fabrication technique | |
| Chen et al. | Review of the principles, devices, parameters, and applications for centrifugal electrospinning | |
| Hu et al. | A biodegradable composite filter made from electrospun zein fibers underlaid on the cellulose paper towel | |
| Fu et al. | Building bimodal structures by a wettability difference-driven strategy for high-performance protein air-filters | |
| CN101538776A (en) | Coaxial polyphosphazene nanofiber composite membrane and preparation method thereof | |
| CN112956764B (en) | Biodegradable mask and preparation method thereof | |
| CN107747165A (en) | A kind of super hydrophilic polyester nano tunica fibrosa and preparation method thereof | |
| Kalluri et al. | Effect of electrospinning parameters on the fiber diameter and morphology of PLGA nanofibers | |
| CN106757788B (en) | A kind of filter for infusion filtering nano fibrous membrane and preparation method thereof | |
| Wang et al. | Hydro‐spinning: A novel technology for making alginate/chitosan fibrous scaffold | |
| Zheng et al. | Effects of cylindrical-electrode-assisted solution blowing spinning process parameters on polymer nanofiber morphology and microstructure | |
| CN105561371B (en) | It is a kind of with network can broken off by water flush abandon dressing and its preparation process | |
| KR20100138503A (en) | Improved preparation method of pva nanofiber membrane using electrospinning | |
| Liu et al. | Electrospinning assisted by gas jet for preparing ultrafine poly (vinyl alcohol) fibres |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |