CN110253984B - Electrostatic spinning nanofiber membrane-fabric composite coating material and preparation method thereof - Google Patents
Electrostatic spinning nanofiber membrane-fabric composite coating material and preparation method thereof Download PDFInfo
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- CN110253984B CN110253984B CN201910533122.XA CN201910533122A CN110253984B CN 110253984 B CN110253984 B CN 110253984B CN 201910533122 A CN201910533122 A CN 201910533122A CN 110253984 B CN110253984 B CN 110253984B
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- fabric
- coating material
- composite coating
- nanofiber membrane
- polyvinylpyrrolidone
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- 239000004744 fabric Substances 0.000 title claims abstract description 51
- 239000002121 nanofiber Substances 0.000 title claims abstract description 46
- 239000002131 composite material Substances 0.000 title claims abstract description 44
- 239000011248 coating agent Substances 0.000 title claims abstract description 38
- 238000000576 coating method Methods 0.000 title claims abstract description 38
- 239000000463 material Substances 0.000 title claims abstract description 36
- 238000010041 electrostatic spinning Methods 0.000 title claims abstract description 26
- 238000002360 preparation method Methods 0.000 title claims abstract description 7
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims abstract description 59
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims abstract description 59
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims abstract description 59
- 229920005569 poly(vinylidene fluoride-co-hexafluoropropylene) Polymers 0.000 claims abstract description 38
- 239000012528 membrane Substances 0.000 claims abstract description 25
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- 235000013824 polyphenols Nutrition 0.000 claims abstract description 15
- 238000000034 method Methods 0.000 claims abstract description 11
- 238000001179 sorption measurement Methods 0.000 claims abstract description 10
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical group [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 12
- 238000006243 chemical reaction Methods 0.000 claims description 12
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- 238000001035 drying Methods 0.000 claims description 7
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- 229910001870 ammonium persulfate Inorganic materials 0.000 claims description 6
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
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- 229920004933 Terylene® Polymers 0.000 claims description 3
- 239000003937 drug carrier Substances 0.000 claims description 3
- 239000005020 polyethylene terephthalate Substances 0.000 claims description 3
- 239000002904 solvent Substances 0.000 claims description 2
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- 239000010410 layer Substances 0.000 abstract description 32
- 229920000523 polyvinylpolypyrrolidone Polymers 0.000 abstract description 20
- 235000013809 polyvinylpolypyrrolidone Nutrition 0.000 abstract description 20
- 238000004132 cross linking Methods 0.000 abstract description 14
- 238000001914 filtration Methods 0.000 abstract description 11
- 239000003381 stabilizer Substances 0.000 abstract description 8
- 239000000126 substance Substances 0.000 abstract description 7
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- JRKICGRDRMAZLK-UHFFFAOYSA-L peroxydisulfate Chemical compound [O-]S(=O)(=O)OOS([O-])(=O)=O JRKICGRDRMAZLK-UHFFFAOYSA-L 0.000 abstract description 3
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- 238000005516 engineering process Methods 0.000 description 1
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- 238000001728 nano-filtration Methods 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
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Abstract
The invention discloses an electrostatic spinning nanofiber membrane-fabric composite coating material and a preparation method thereof. The composite coating material is composed of a three-layer structure. The surface layer is cross-linked PVPP obtained by PVP persulfate free radical polymerization; the middle layer is a polyvinylidene fluoride-hexafluoropropylene (PVDF-HFP)/polyvinylpyrrolidone (PVP) needle-free electrostatic spinning nanofiber membrane; the bottom layer is a fabric. The surface layer is a functional layer, and the middle layer and the bottom layer are compounded together through PVP self-crosslinking and the cross-linking with PVDF-HFP in the PVP crosslinking process to jointly form a supporting layer of the composite coating material. The composite material prepared by the invention can be used for functional medical dressings and beer stabilizers, and has the double-layer functions of polyphenol substance adsorption and filtration.
Description
Technical Field
The invention belongs to the field of composite material preparation, and particularly relates to a preparation method for processing an electrostatic spinning/fabric binary composite material. Can be applied to the technical field of nano material analysis technology and membrane material application.
Background
With the continuous development of the textile industry and the continuous improvement of the requirements of people on the comprehensive performance of textiles, the multifunctional composite fabric undoubtedly occupies a place in the development of the fabric. In recent years, the application of electrostatic spinning nanofibers which are generally concerned at home and abroad in spinning is increasing, and particularly reports that nanofibers are combined with traditional fabrics and applied to special industrial materials are frequent.
PVPP is formed by cross-linking polymerization of a vinylpyrrolidone monomer under specific conditions, is a high-molecular fine chemical product with excellent properties, and is a novel pharmaceutic adjuvant which is popular in recent years. PVPP is mainly used as a disintegrant for tablets, and has been approved as a food additive, a stabilizer, a clarifier, and the like in the brewing industry of beer, fruit juice, and the like.
PVPP is widely applied in the field of domestic and foreign beer and is used as a beer colloid stabilizer. No matter how cool the beer is after filtration, the dissolved classified compounds and proteins are still contained, and the irreversible permanent polymers formed by the polyphenol substances and the proteins under the condition of oxygen are the main reasons for beer chaos. The PVPP can effectively remove polyphenol substances in the beer, improve the clarity of the beer and prolong the shelf life of the beer.
At present, in beer production, kieselguhr and PVPP are mixed and then quantitatively added into beer, and after filtration, the PVPP and the kieselguhr form a filter cake which is treated as waste. The process does not need separate PVPP filtering equipment, but has higher production cost.
Disclosure of Invention
In order to solve the problem of high-efficiency use of the PVPP as the beer stabilizer, the invention breaks through the use method that the conventional PVPP is adsorbed by a powdery intermediate in the beer stabilizer and is filtered and removed in the form of a filter cake, and prepares the composite material which takes the electrostatic spinning nanofiber membrane-fabric filter material as a supporting layer and the PVPP coating as a functional layer.
The electrostatic spinning nanofiber membrane-fabric composite coating material is of a three-layer structure consisting of a surface layer, a middle layer and a bottom layer, wherein the surface layer is a crosslinked polyvinyl pyrrolidone (PVPP) coating obtained by PVP persulfate free radical polymerization, the middle layer is a polyvinylidene fluoride-hexafluoropropylene (PVDF-HFP)/polyvinyl pyrrolidone (PVP) electrostatic spinning nanofiber membrane, preferably a polyvinylidene fluoride-hexafluoropropylene (PVDF-HFP)/polyvinyl pyrrolidone (PVP) needle-free electrostatic spinning nanofiber membrane obtained by needle-free electrostatic spinning, and the bottom layer is a fabric which is a woven fabric or a non-woven fabric.
As a preferable technical scheme, the thickness of the polyvinylidene fluoride-hexafluoropropylene/polyvinylpyrrolidone electrostatic spinning nanofiber membrane is 0.054-0.114 mm; the fabric is a woven fabric or a non-woven fabric of terylene, polypropylene or chinlon.
The invention also provides a preparation method of the electrostatic spinning nanofiber membrane-fabric composite coating material, which comprises the following steps:
(1) mixing polyvinylidene fluoride-hexafluoropropylene (PVDF-HFP) solution and polyvinylpyrrolidone (PVP) solution according to a volume ratio of (9:1-7:3) to obtain a composite spinning solution, and preparing a polyvinylidene fluoride-hexafluoropropylene (PVDF-HFP)/polyvinylpyrrolidone (PVP) electrospun nanofiber membrane by an electrostatic spinning method;
the concentration of the polyvinylidene fluoride-hexafluoropropylene (PVDF-HFP) solution is 14-20wt%, and the concentration of the polyvinylpyrrolidone solution is 6-8 wt%;
(2) placing the polyvinylidene fluoride-hexafluoropropylene (PVDF-HFP)/polyvinylpyrrolidone (PVP) electrostatic spinning nanofiber membrane and fabric obtained in the step (1) in parallel, mutually attaching, immersing the membrane and the fabric into an initiation system containing PVP, an initiator and water to perform polymerization (crosslinking) reaction, and drying after crosslinking to obtain a nanofiber membrane-fabric composite coating material;
the initiator in the initiation system is ammonium persulfate, the concentration of polyvinylpyrrolidone (PVP) is 5-10wt%, the concentration of ammonium persulfate is 0.5-1wt%, the reaction temperature is 90-95 ℃, and the reaction time is 6-8 h.
As a preferable technical scheme, a solvent of the polyvinylidene fluoride-hexafluoropropylene (PVDF-HFP) solution and the polyvinylpyrrolidone (PVP) solution in the step (1) is N-Dimethylacetamide (DMAC); as a preferred technical scheme, the electrostatic spinning method in the step (1) is needle-free electrostatic spinning.
As a preferred technical scheme, the needleless electrospinning conditions in the step (1) are as follows: the voltage is 60-80kV, the solution box speed is 80-150mm/s, and the spinning time is 40-120 min.
Preferably, the thickness of the polyvinylidene fluoride-hexafluoropropylene (PVDF-HFP)/polyvinylpyrrolidone (PVP) electrospun nanofiber membrane in the step (1) is 0.054-0.114 mm.
As a preferable technical scheme, the drying conditions in the step (2) are as follows: drying at 40-60 deg.C for 2-4 h.
As a preferable technical scheme, the fabric in the step (2) is a woven fabric or a non-woven fabric of terylene, polypropylene or chinlon.
The invention also provides application of the nanofiber membrane-fabric composite coating material in drug carriers, functional medical dressings and beer polyphenol adsorption. The product has double-layer functions of polyphenol adsorption and filtration, and can be used as beer stabilizer.
As a preferable technical scheme, when the electrostatic spinning nanofiber membrane-fabric composite coating material is applied to beer polyphenol adsorption, the fabric is a woven fabric or a non-woven fabric of polypropylene fibers.
The surface layer of the electrostatic spinning nanofiber membrane-fabric composite coating material is a functional layer, and the middle layer and the bottom layer are compounded together through PVP self-crosslinking and crosslinking with PVDF-HFP in the PVP crosslinking process to jointly form a supporting layer of the composite coating material. The surface coating of the composite coating material, the PVPP mutually crosslinked by the nano fibers and the PVPP adsorbed on the surfaces of the fibers in the fabric increase the contact area between the PVPP and the adsorbing material, play a role of a stabilizer, effectively remove polyphenol substances in beer and play a role in reinforcing and connecting the composite coating material. The intermediate layer and the bottom layer of the binary fabric are compounded to form a secondary filtering condition. The middle layer of the nano-fiber membrane is nano-grade filtration, and the fabric layer is micro-grade filtration. The composite coating material has the double-layer functions of polyphenol substance adsorption and filtration, shortens the process flow and saves the cost.
The invention has the beneficial effects that:
1. the composite coating material consists of three layers, wherein the surface is a PVPP coating, the middle is a PVDF-HFP/PVP nano fiber membrane, and the bottom layer is a fabric. In the presence of persulfate, PVDF-HFP can generate corresponding free radicals, and the cross-linking reaction of PVP and PFDF-HFP occurs to form a stable structure. By utilizing the self-crosslinking reaction of PVP and the cross-linking reaction of PVDF-HFP, the PVPP can firmly connect the coating with the nanofiber layer and the nanofiber layer with the fabric, the interface strength of the material is improved, and the problem that the membrane is easy to peel is solved.
2. In the beer polyphenol adsorption, the PVPP fixed on the surface coating of the composite material and the surface of the fiber improves the contact area of the material, plays a role of a stabilizer and effectively removes polyphenol substances in beer. The intermediate layer and the bottom layer of the binary fabric are compounded to form a secondary filtering condition. The nano-fiber layer is nano-filtration, and the fabric layer is micro-filtration. The composite material has the functions of filtering and adsorbing polyphenol substances, shortens the process flow and saves the cost.
3. Because the PVPP needs to be washed by alkali liquor in the recycling process, polypropylene fabrics are selected in the adsorption of the beer polyphenol. The polypropylene fabric and the PVDF-HFP nanofiber membrane have good acid and alkali resistance and water resistance. The composite material can work under acidic and alkaline conditions, and has a long service life.
4. The PVPP has the characteristics of physiological safety, liquid absorption capacity, drug carrying and releasing, water insolubility, complexation and the like, and the composite material prepared by the invention can also be prepared into a soft adhesive tape with certain strength and used as an ideal drug carrier or an ideal wound dressing. The functional layer provides drug loading and liquid absorption capacity, the middle nano layer is acid and alkali resistant and has good hydrophobicity, the product ventilation capacity is provided, and the bottom layer is a supporting layer and provides strength and flexibility.
Drawings
FIG. 1 is an SEM photograph of a 7:3PVDF-HFP/PVP nano-composite membrane in example 1;
FIG. 2 is an SEM photograph of a 9:1PVDF-HFP/PVP nano-composite membrane in example 2;
fig. 3 is SEM image of the nanofiber membrane-fabric composite coating material of example 2, wherein (a) is front side coating, (b) is back side fabric, and (c) is interface between nanofiber membrane and fabric.
Detailed Description
The following non-limiting examples will allow one of ordinary skill in the art to more fully understand the present invention, but are not intended to limit the invention in any way.
The embodiment of the invention selects the following materials and devices:
scanning Electron Microscope (SEM): a super-high resolution thermal field emission scanning electron microscope JSM-780DF, Japanese Electron JEDL;
needle-free electrospinning apparatus: nano spider silk electrostatic spinning machine, czech ELMARCO company;
and (3) a strength test device: LLY-06E model electronic single fiber strength tester, Leizhou electronic instruments, Inc. The test sample manufacturing process comprises the following steps: the specimens were cut out to a length of 5cm and a width of 0.6 cm. Testing at 20 deg.C and 65% humidity;
thickness test equipment: model YG141LA digital textile thickness meter, electronics ltd, lazhou.
Example 1
PVDF-HFP was dissolved in DMAC to give a 20wt% PVDF-HFP solution. PVP was dissolved in DMAC to give a 6 wt% PVP solution. And mixing the PVDF-HFP solution with the PVP solution according to the volume ratio of 7:3 to prepare the PVDF-HFP/PVP composite spinning solution. And (3) carrying out needleless electrostatic spinning on the PVDF-HFP/PVP composite spinning solution under the conditions of voltage of 80kV, solution box speed of 80mm/s and spinning time of 40min to obtain the PVDF-HFP/PVP nano composite membrane. The PVDF-HFP/PVP nano composite membrane has the breaking strength of 4.6202MPa, the average diameter of the nano fiber is 113nm, the thickness is 0.054mm, and SEM is shown in figure 1. The PVDF-HFP/PVP nano composite membrane and polyester woven fabric (polyester: polyester filament 300DX5, weft: polyester filament 300DX4, warp density: 307 pieces/10 cm, weft density: 122 pieces/10 cm, 2/2 twill) are placed in parallel up and down and are mutually attached, the peripheral edges are clamped by a mould and then immersed into an initiation system to initiate polymerization (crosslinking) reaction, the concentration of ammonium persulfate in the initiation system is 0.5 wt%, the concentration of PVP is 5 wt%, the reaction temperature is 90 ℃, the reaction time is 6 hours, and after the reaction is finished, the nano fiber membrane-fabric composite coating material is obtained after drying at 40 ℃ for 4 hours.
Example 2
PVDF-HFP was dissolved in DMAC to give a 20wt% solution of PVDF-HFP. 6 wt% of PVP was dissolved in DMAC to obtain a PVP solution. And mixing the PVDF-HFP solution with the PVP solution according to the volume ratio of 9:1 to prepare the PVDF-HFP/PVP composite spinning solution. And (3) carrying out needleless electrostatic spinning on the PVDF-HFP/PVP composite spinning solution under the conditions of voltage 80kV, solution box speed 80mm/s and spinning time 40min to obtain the PVDF-HFP/PVP nano composite membrane. The PVDF-HFP/PVP nano composite membrane has the breaking strength of 9.1565MPa, the average diameter of the nano fiber is 156nm, the thickness is 0.114mm, and SEM is shown in figure 2. The PVDF-HFP/PVP nano composite membrane and a polyester woven fabric (warp yarn: polyester filament 300DX5, weft yarn: polyester filament 300DX4, warp density: 307 pieces/10 cm, weft density: 122 pieces/10 cm, 2/2 twill) are placed in parallel up and down and are mutually attached, the peripheral edge is clamped by a mould and then is immersed into an initiation system to initiate polymerization (crosslinking) reaction, the concentration of ammonium persulfate in the initiation system is 1wt%, the concentration of PVP is 10wt%, the reaction temperature is 95 ℃, the reaction time is 8 hours, and after the reaction is finished, the nano fiber membrane-fabric composite coating material is dried at 40 ℃ for 4 hours to obtain the nano fiber membrane-fabric composite coating material, wherein SEM of the nano fiber membrane-fabric composite coating material is shown in figure 3, wherein (a) is a front side coating, (b) is a fabric, and (c) is an interface of the nano.
Claims (8)
1. An electrostatic spinning nanofiber membrane-fabric composite coating material for beer polyphenol adsorption is characterized in that the preparation method comprises the following steps:
(1) mixing a polyvinylidene fluoride-hexafluoropropylene solution and a polyvinylpyrrolidone solution according to a volume ratio of 9:1-7:3 to obtain a composite spinning solution, and preparing a polyvinylidene fluoride-hexafluoropropylene/polyvinylpyrrolidone electrospun nanofiber membrane by an electrostatic spinning method;
the concentration of the polyvinylidene fluoride-hexafluoropropylene solution is 14-20wt%, and the concentration of the polyvinylpyrrolidone solution is 6-8 wt%;
(2) placing the polyvinylidene fluoride-hexafluoropropylene/polyvinylpyrrolidone electrostatic spinning nanofiber membrane and the fabric prepared in the step (1) in parallel, mutually attaching, immersing into an initiation system, and drying after polymerization reaction to obtain an electrostatic spinning nanofiber membrane-fabric composite coating material;
the fabric is woven fabric;
the initiating system is an initiating system containing polyvinylpyrrolidone, an initiating agent and water, wherein the initiating agent is ammonium persulfate, the concentration of the polyvinylpyrrolidone is 5-10wt%, the concentration of the ammonium persulfate is 0.5-1wt%, the reaction temperature is 90-95 ℃, and the reaction time is 6-8 h.
2. The nanofiber membrane-fabric composite coating material according to claim 1, wherein the thickness of the polyvinylidene fluoride-hexafluoropropylene/polyvinylpyrrolidone electrospun nanofiber membrane is 0.054-0.114 mm; the fabric is a woven fabric of terylene, polypropylene or chinlon.
3. The nanofiber film-fabric composite coating material according to claim 1, wherein the electrospinning method in step (1) is needle-free electrospinning.
4. The nanofiber film-fabric composite coating material according to claim 3, wherein the needle-free electrospinning conditions in step (1) are: the voltage is 60-80kV, the solution box speed is 80-150mm/s, and the spinning time is 40-120 min.
5. The nanofiber film-fabric composite coating material according to claim 1, wherein the drying conditions in step (2) are as follows: drying at 40-60 deg.C for 2-4 h.
6. The nanofiber membrane-fabric composite coating material according to claim 1, wherein the solvent of the polyvinylidene fluoride-hexafluoropropylene solution and the polyvinylpyrrolidone solution in step (1) is N, N-dimethylacetamide.
7. Use of the electrospun nanofiber membrane-fabric composite coating material of any one of claims 1 to 6 in drug carriers, medical dressings, beer polyphenol adsorption.
8. The use according to claim 7, wherein the fabric is a woven fabric of polypropylene when the electrospun nanofiber membrane-fabric composite coating material is used in beer polyphenol adsorption.
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