WO2023273954A1 - Procédé de régulation et de commande de la structure des pores d'un film de nanofibres - Google Patents
Procédé de régulation et de commande de la structure des pores d'un film de nanofibres Download PDFInfo
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- WO2023273954A1 WO2023273954A1 PCT/CN2022/100093 CN2022100093W WO2023273954A1 WO 2023273954 A1 WO2023273954 A1 WO 2023273954A1 CN 2022100093 W CN2022100093 W CN 2022100093W WO 2023273954 A1 WO2023273954 A1 WO 2023273954A1
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- Prior art keywords
- regulating
- solution
- parts
- polyethylene glycol
- pore structure
- Prior art date
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- 230000001105 regulatory effect Effects 0.000 title claims abstract description 117
- 238000000034 method Methods 0.000 title claims abstract description 64
- 239000011148 porous material Substances 0.000 title claims abstract description 59
- 239000002121 nanofiber Substances 0.000 title claims abstract description 52
- 230000001276 controlling effect Effects 0.000 title abstract description 22
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 54
- 239000002202 Polyethylene glycol Substances 0.000 claims abstract description 51
- 229920001223 polyethylene glycol Polymers 0.000 claims abstract description 51
- 229920000642 polymer Polymers 0.000 claims abstract description 50
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 44
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 43
- 238000009987 spinning Methods 0.000 claims abstract description 41
- ALVYUZIFSCKIFP-UHFFFAOYSA-N triethoxy(2-methylpropyl)silane Chemical compound CCO[Si](CC(C)C)(OCC)OCC ALVYUZIFSCKIFP-UHFFFAOYSA-N 0.000 claims abstract description 21
- TUNFSRHWOTWDNC-HKGQFRNVSA-N tetradecanoic acid Chemical compound CCCCCCCCCCCCC[14C](O)=O TUNFSRHWOTWDNC-HKGQFRNVSA-N 0.000 claims abstract description 14
- 238000002156 mixing Methods 0.000 claims abstract description 13
- 239000012528 membrane Substances 0.000 claims description 73
- 238000001523 electrospinning Methods 0.000 claims description 37
- 239000002904 solvent Substances 0.000 claims description 32
- 239000002245 particle Substances 0.000 claims description 17
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical group CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- 239000005543 nano-size silicon particle Substances 0.000 claims description 12
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 12
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 12
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 12
- 235000012239 silicon dioxide Nutrition 0.000 claims description 11
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 5
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 5
- 239000001856 Ethyl cellulose Substances 0.000 claims description 4
- 229920001249 ethyl cellulose Polymers 0.000 claims description 4
- 235000019325 ethyl cellulose Nutrition 0.000 claims description 4
- 229920000896 Ethulose Polymers 0.000 claims description 2
- 239000001859 Ethyl hydroxyethyl cellulose Substances 0.000 claims description 2
- 235000019326 ethyl hydroxyethyl cellulose Nutrition 0.000 claims description 2
- 235000019422 polyvinyl alcohol Nutrition 0.000 claims description 2
- 239000000377 silicon dioxide Substances 0.000 abstract description 27
- 238000001914 filtration Methods 0.000 abstract description 14
- 238000010041 electrostatic spinning Methods 0.000 abstract 2
- 239000000243 solution Substances 0.000 description 90
- 230000000052 comparative effect Effects 0.000 description 31
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 13
- 239000011889 copper foil Substances 0.000 description 13
- 239000000203 mixture Substances 0.000 description 13
- 239000000706 filtrate Substances 0.000 description 12
- TWJNQYPJQDRXPH-UHFFFAOYSA-N 2-cyanobenzohydrazide Chemical compound NNC(=O)C1=CC=CC=C1C#N TWJNQYPJQDRXPH-UHFFFAOYSA-N 0.000 description 7
- TUNFSRHWOTWDNC-UHFFFAOYSA-N Myristic acid Natural products CCCCCCCCCCCCCC(O)=O TUNFSRHWOTWDNC-UHFFFAOYSA-N 0.000 description 7
- 235000021360 Myristic acid Nutrition 0.000 description 7
- 229910052814 silicon oxide Inorganic materials 0.000 description 4
- 125000000959 isobutyl group Chemical group [H]C([H])([H])C([H])(C([H])([H])[H])C([H])([H])* 0.000 description 3
- 229910052710 silicon Inorganic materials 0.000 description 3
- 239000010703 silicon Substances 0.000 description 3
- ZZSNKZQZMQGXPY-UHFFFAOYSA-N Ethyl cellulose Chemical compound CCOCC1OC(OC)C(OCC)C(OCC)C1OC1C(O)C(O)C(OC)C(CO)O1 ZZSNKZQZMQGXPY-UHFFFAOYSA-N 0.000 description 2
- 229920000663 Hydroxyethyl cellulose Polymers 0.000 description 2
- 239000004354 Hydroxyethyl cellulose Substances 0.000 description 2
- 235000019447 hydroxyethyl cellulose Nutrition 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- HMUNWXXNJPVALC-UHFFFAOYSA-N 1-[4-[2-(2,3-dihydro-1H-inden-2-ylamino)pyrimidin-5-yl]piperazin-1-yl]-2-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)ethanone Chemical compound C1C(CC2=CC=CC=C12)NC1=NC=C(C=N1)N1CCN(CC1)C(CN1CC2=C(CC1)NN=N2)=O HMUNWXXNJPVALC-UHFFFAOYSA-N 0.000 description 1
- VWVRASTUFJRTHW-UHFFFAOYSA-N 2-[3-(azetidin-3-yloxy)-4-[2-(2,3-dihydro-1H-inden-2-ylamino)pyrimidin-5-yl]pyrazol-1-yl]-1-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)ethanone Chemical compound O=C(CN1C=C(C(OC2CNC2)=N1)C1=CN=C(NC2CC3=C(C2)C=CC=C3)N=C1)N1CCC2=C(C1)N=NN2 VWVRASTUFJRTHW-UHFFFAOYSA-N 0.000 description 1
- YJLUBHOZZTYQIP-UHFFFAOYSA-N 2-[5-[2-(2,3-dihydro-1H-inden-2-ylamino)pyrimidin-5-yl]-1,3,4-oxadiazol-2-yl]-1-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)ethanone Chemical compound C1C(CC2=CC=CC=C12)NC1=NC=C(C=N1)C1=NN=C(O1)CC(=O)N1CC2=C(CC1)NN=N2 YJLUBHOZZTYQIP-UHFFFAOYSA-N 0.000 description 1
- MGGVALXERJRIRO-UHFFFAOYSA-N 4-[2-(2,3-dihydro-1H-inden-2-ylamino)pyrimidin-5-yl]-2-[2-oxo-2-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)ethyl]-1H-pyrazol-5-one Chemical compound C1C(CC2=CC=CC=C12)NC1=NC=C(C=N1)C=1C(=NN(C=1)CC(=O)N1CC2=C(CC1)NN=N2)O MGGVALXERJRIRO-UHFFFAOYSA-N 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 1
- 229910052753 mercury Inorganic materials 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000001338 self-assembly Methods 0.000 description 1
- 238000005287 template synthesis Methods 0.000 description 1
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
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/0007—Electro-spinning
- D01D5/0015—Electro-spinning characterised by the initial state of the material
-
- 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
-
- 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
- D01F6/50—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 polyalcohols, polyacetals or polyketals
-
- 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
- D01F6/56—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 cyclic compounds with one carbon-to-carbon double bond in the side chain
-
- 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
- D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
- D01F8/02—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from cellulose, cellulose derivatives, or proteins
-
- 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
- D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
- D01F8/04—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
- D01F8/10—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one other macromolecular compound obtained by reactions only involving carbon-to-carbon unsaturated bonds as constituent
Definitions
- the present application relates to the technical field of nanofiber membranes, in particular to a method for regulating the pore structure of nanofiber membranes.
- nanofibrous membranes there are many methods for fabricating nanofibrous membranes, such as stretching method, template synthesis, self-assembly, microphase separation, electrospinning, etc.
- stretching method template synthesis
- self-assembly self-assembly
- microphase separation electrospinning
- electrospinning electrospinning technology
- the nanofiber membranes prepared by this method can be widely used in water filtration, oil-water separation and other fields.
- the pore structure of different nanofiber membranes will affect the function and application of nanofiber membranes, so it is very important to regulate the pore structure of nanofiber membranes.
- each exemplary embodiment of the present application is to provide a method for regulating the pore structure of a nanofiber membrane, which includes the following steps:
- the regulating agent includes the following components in parts by weight: 20-50 parts of nano silicon dioxide, 20-50 parts of polyethylene glycol, 10-30 parts of myristic acid, 1-10 parts of isobutyl triethoxy silicon, 200-500 parts of water; and
- control solution is filtered, electrospinning is performed to obtain a nanofiber membrane.
- the regulator includes the following components in parts by weight: 30-40 parts of nano-silica, 30-40 parts of polyethylene glycol, 15-25 parts of myristic acid, isobutyl triethyl 4-6 parts of silicon oxide, 300-400 parts of water.
- the added mass of the regulating agent is 0.1%-5% of the mass of the polymer spinning solution.
- the particle size of the nano silicon dioxide is 50nm-150nm.
- the average molecular weight of the polyethylene glycol is 400-1200.
- the preparation method of the polymer spinning solution comprises the following steps:
- the high molecular polymer is dissolved in a solvent to obtain the high molecular spinning solution; the mass ratio of the high molecular polymer to the solvent is (5-30):(70-95).
- the high molecular polymer is at least one of polyvinyl alcohol, ethyl cellulose, hydroxyethyl cellulose or polyvinyl pyrrolidone.
- water-soluble or alcohol-soluble polymer materials can be used for high-molecular polymers, and are not limited to the above-mentioned polymers, that is, the regulation method provided in this application is applicable to most water-soluble or alcohol-soluble polymers. Pore modulation of nanofibrous membranes of materials.
- the solvent is water and/or ethanol.
- the mixing and dispersing temperature is 50°C-70°C.
- the voltage in the step, during electrospinning, is 10kV-20kV.
- the current method for regulating the pore structure of electrospun nanofibrous membranes is generally to control the process parameters of electrospinning, which is not only difficult to control the pore structure, but also has a small adjustable range of pore size. question.
- Each exemplary embodiment of the present application provides a method for regulating the pore structure of a nanofiber membrane, by adding nano-silica, polyethylene glycol, myristic acid, and isobutyltriethoxysilane to the polymer spinning solution.
- the pore structure of the nanofiber membrane can be adjusted by adjusting the amount of the regulator to change the pore size and porosity of the nanofiber membrane.
- This control method can realize the control of the pore structure of the nanofiber membrane only by changing the addition amount of the regulator, and it can realize a wide range of control of the pore size and porosity of the nanofiber membrane without changing the process parameters of electrospinning .
- This embodiment provides a method for regulating and controlling the pore structure of a nanofibrous membrane, which includes the following steps:
- a regulating agent to the above-mentioned 100 g of polymer spinning solution, and place it at a temperature of 50° C., mix and disperse for 20 minutes at a speed of 500 rpm to obtain a regulating solution, wherein the regulating agent is made of nano-silica 20g, polyethylene glycol 20g, myristic acid 10g, isobutyltriethoxy silicon 1g, and water 500g.
- the particle size of the nano silicon dioxide is 50nm
- the average molecular weight of the polyethylene glycol is 400.
- the filtrate is taken for electrospinning to obtain a nanofiber membrane, and the regulation of the pore structure of the nanofiber membrane is completed.
- the process parameters of electrospinning can refer to the prior art. Specifically, copper foil was used as the receiving device, the voltage was set to 10 kV, the pushing speed of the regulating solution was 1 mL/h, and the distance between the needle tip for pushing the regulating solution and the receiving device was 10 cm.
- This embodiment provides a method for regulating and controlling the pore structure of a nanofibrous membrane, which includes the following steps:
- regulating agent Add 5 g of regulating agent to the above-mentioned 100 g of polymer spinning solution, and place it at a temperature of 70° C., mix and disperse for 40 minutes at a speed of 1500 rpm to obtain a regulating solution, wherein the regulating agent is made of 50 g of nano-silica , 50g of polyethylene glycol, 30g of myristic acid, 10g of isobutyl triethoxy silicon, and 200g of water are mixed.
- the particle size of the nano silicon dioxide is 150nm
- the average molecular weight of the polyethylene glycol is 1200.
- the filtrate is taken for electrospinning to obtain a nanofiber membrane, and the regulation of the pore structure of the nanofiber membrane is completed.
- the process parameters of electrospinning can refer to the prior art. Specifically, copper foil was used as the receiving device, the voltage was set to 20 kV, the pushing speed of the regulating solution was 2 mL/h, and the distance between the needle tip for pushing the regulating solution and the receiving device was 15 cm.
- This embodiment provides a method for regulating and controlling the pore structure of a nanofibrous membrane, which includes the following steps:
- regulating agent Add 1 g of regulating agent to the above-mentioned 100 g of polymer spinning solution, and place it at a temperature of 55° C., mix and disperse for 30 minutes at a speed of 800 rpm to obtain a regulating solution, wherein the regulating agent is made of 25 g of nano-silica , polyethylene glycol 25g, myristic acid 12g, isobutyltriethoxy silicon 2g, and water 450g; in addition, the particle size of nano-silica is 80nm, and the average molecular weight of polyethylene glycol is 600.
- the filtrate is taken for electrospinning to obtain a nanofiber membrane, and the regulation of the pore structure of the nanofiber membrane is completed.
- the process parameters of electrospinning can refer to the prior art. Specifically, copper foil was used as the receiving device, the voltage was set to 15kV, the pushing speed of the regulating solution was 1.5mL/h, and the distance between the needle tip for pushing the regulating solution and the receiving device was 15cm.
- This embodiment provides a method for regulating and controlling the pore structure of a nanofibrous membrane, which includes the following steps:
- regulating agent Add 3 g of regulating agent to the above-mentioned 100 g of polymer spinning solution, and place it at a temperature of 60° C., mix and disperse for 30 minutes at a speed of 1200 rpm to obtain a regulating solution, wherein the regulating agent is made of 45 g of nano-silica , 45g of polyethylene glycol, 28g of myristic acid, 8g of isobutyl triethoxy silicon, and 250g of water.
- the particle size of the nano silicon dioxide is 120nm, and the average molecular weight of the polyethylene glycol is 1000.
- the filtrate is taken for electrospinning to obtain a nanofiber membrane, and the regulation of the pore structure of the nanofiber membrane is completed.
- the process parameters of electrospinning can refer to the prior art. Specifically, copper foil was used as the receiving device, the voltage was set to 15kV, the pushing speed of the regulating solution was 1.5mL/h, and the distance between the needle tip for pushing the regulating solution and the receiving device was 12cm.
- This embodiment provides a method for regulating and controlling the pore structure of a nanofibrous membrane, which includes the following steps:
- regulating agent Add 2 g of regulating agent to the above-mentioned 100 g of polymer spinning solution, and place it at a temperature of 60° C., mix and disperse for 30 minutes at a speed of 1000 rpm to obtain a regulating solution, wherein the regulating agent is made of 30 g of nano-silicon dioxide , 30g of polyethylene glycol, 15g of myristic acid, 4g of isobutyl triethoxy silicon, and 400g of water are mixed.
- the particle diameter of the nano-silica is 100 nm
- the average molecular weight of the polyethylene glycol is 800.
- the filtrate is taken for electrospinning to obtain a nanofiber membrane, and the regulation of the pore structure of the nanofiber membrane is completed.
- the process parameters of electrospinning can refer to the prior art. Specifically, copper foil was used as the receiving device, the voltage was set to 15kV, the pushing speed of the regulating solution was 1.5mL/h, and the distance between the needle tip for pushing the regulating solution and the receiving device was 12cm.
- This embodiment provides a method for regulating and controlling the pore structure of a nanofibrous membrane, which includes the following steps:
- regulating agent Add 2 g of regulating agent to the above-mentioned 100 g of polymer spinning solution, and place it at a temperature of 60° C., mix and disperse for 30 minutes at a speed of 1200 rpm to obtain a regulating solution, wherein the regulating agent is made of 40 g of nano-silica , 40g of polyethylene glycol, 25g of myristic acid, 6g of isobutyl triethoxy silicon, and 300g of water are mixed.
- the particle diameter of the nano-silica is 100 nm
- the average molecular weight of the polyethylene glycol is 800.
- the process parameters of electrospinning can refer to the existing technology. Specifically, copper foil was used as the receiving device, the voltage was set to 15kV, the pushing speed of the regulating solution was 1.5mL/h, and the distance between the needle tip for pushing the regulating solution and the receiving device was 12cm.
- This embodiment provides a method for regulating and controlling the pore structure of a nanofibrous membrane, which includes the following steps:
- a regulating agent to the above-mentioned 100 g of polymer spinning solution, and place it at a temperature of 60° C., mix and disperse for 30 minutes at a speed of 1000 rpm to obtain a regulating solution, wherein the regulating agent is made of nano-silica 35g, 35g of polyethylene glycol, 20g of myristic acid, 5g of isobutyl triethoxy silicon, and 350g of water.
- the particle diameter of the nano-silica is 100 nm
- the average molecular weight of the polyethylene glycol is 800.
- the filtrate is taken for electrospinning to obtain a nanofiber membrane, and the regulation of the pore structure of the nanofiber membrane is completed.
- the process parameters of electrospinning can refer to the prior art. Specifically, copper foil was used as the receiving device, the voltage was set to 15kV, the pushing speed of the regulating solution was 1.5mL/h, and the distance between the needle tip for pushing the regulating solution and the receiving device was 12cm.
- This embodiment provides a method for regulating and controlling the pore structure of a nanofibrous membrane, which includes the following steps:
- a regulating agent to the above-mentioned 100 g of polymer spinning solution, and place it at a temperature of 60° C., mix and disperse for 30 minutes at a speed of 1000 rpm to obtain a regulating solution, wherein the regulating agent is made of nano-silica 35g, polyethylene glycol 35g, myristic acid 20g, isobutyl triethoxy silicon 5g, water 350g mixed.
- the particle diameter of the nano-silica is 100 nm
- the average molecular weight of the polyethylene glycol is 800.
- the filtrate is taken for electrospinning to obtain a nanofiber membrane, and the regulation of the pore structure of the nanofiber membrane is completed.
- the process parameters of electrospinning can refer to the prior art. Specifically, copper foil was used as the receiving device, the voltage was set to 15kV, the pushing speed of the regulating solution was 1.5mL/h, and the distance between the needle tip for pushing the regulating solution and the receiving device was 12cm.
- This embodiment provides a method for regulating and controlling the pore structure of a nanofibrous membrane, which includes the following steps:
- regulating agent Add 1 g of regulating agent to the above-mentioned 100 g of polymer spinning solution, and place it at a temperature of 60° C., mix and disperse for 30 minutes at a speed of 1000 rpm to obtain a regulating solution, wherein the regulating agent is composed of 35 g of nano-silica , 35g of polyethylene glycol, 20g of myristic acid, 5g of isobutyl triethoxy silicon, and 350g of water are mixed.
- the particle diameter of the nano-silica is 100 nm
- the average molecular weight of the polyethylene glycol is 800.
- the filtrate is taken for electrospinning to obtain a nanofiber membrane, and the regulation of the pore structure of the nanofiber membrane is completed.
- the process parameters of electrospinning can refer to the prior art. Specifically, copper foil was used as the receiving device, the voltage was set to 15kV, the pushing speed of the regulating solution was 1.5mL/h, and the distance between the needle tip for pushing the regulating solution and the receiving device was 12cm.
- This embodiment provides a method for regulating and controlling the pore structure of a nanofibrous membrane, which includes the following steps:
- regulating agent Add 2 g of regulating agent to the above-mentioned 100 g of polymer spinning solution, and place it at a temperature of 60° C., mix and disperse for 30 minutes at a speed of 1000 rpm to obtain a regulating solution, wherein the regulating agent is made of nano silicon dioxide 35 g , 35g of polyethylene glycol, 20g of myristic acid, 5g of isobutyl triethoxy silicon, and 350g of water are mixed.
- the particle diameter of the nano-silica is 100 nm
- the average molecular weight of the polyethylene glycol is 800.
- the filtrate is taken for electrospinning to obtain a nanofiber membrane, and the regulation of the pore structure of the nanofiber membrane is completed.
- the process parameters of electrospinning can refer to the prior art. Specifically, copper foil was used as the receiving device, the voltage was set to 15kV, the pushing speed of the regulating solution was 1.5mL/h, and the distance between the needle tip for pushing the regulating solution and the receiving device was 12cm.
- This embodiment provides a method for regulating and controlling the pore structure of a nanofibrous membrane, which includes the following steps:
- regulating agent Add 3 g of regulating agent to the above-mentioned 100 g of polymer spinning solution, and place it at a temperature of 60° C., mix and disperse for 30 minutes at a speed of 1000 rpm to obtain a regulating solution, wherein the regulating agent is made of 35 g of nano-silica , 35g of polyethylene glycol, 20g of myristic acid, 5g of isobutyl triethoxy silicon, and 350g of water are mixed.
- the particle diameter of the nano-silica is 100 nm
- the average molecular weight of the polyethylene glycol is 800.
- the filtrate is taken for electrospinning to obtain a nanofiber membrane, and the regulation of the pore structure of the nanofiber membrane is completed.
- the process parameters of electrospinning can refer to the prior art. Specifically, copper foil was used as the receiving device, the voltage was set to 15kV, the pushing speed of the regulating solution was 1.5mL/h, and the distance between the needle tip for pushing the regulating solution and the receiving device was 12cm.
- This embodiment provides a method for regulating and controlling the pore structure of a nanofibrous membrane, which includes the following steps:
- regulating agent Add 5 g of regulating agent to the above-mentioned 100 g of polymer spinning solution, and place it at a temperature of 60° C., mix and disperse for 30 minutes at a speed of 1000 rpm to obtain a regulating solution, wherein the regulating agent is made of nano silicon dioxide 35 g , 35g of polyethylene glycol, 20g of myristic acid, 5g of isobutyl triethoxy silicon, and 350g of water are mixed.
- the particle diameter of the nano-silica is 100 nm
- the average molecular weight of the polyethylene glycol is 800.
- the filtrate is taken for electrospinning to obtain a nanofiber membrane, and the regulation of the pore structure of the nanofiber membrane is completed.
- the process parameters of electrospinning can refer to the prior art. Specifically, copper foil was used as the receiving device, the voltage was set to 15kV, the pushing speed of the regulating solution was 1.5mL/h, and the distance between the needle tip for pushing the regulating solution and the receiving device was 12cm.
- This comparative example provides a method for regulating and controlling the pore structure of a nanofibrous membrane, which includes the following steps:
- Electrospinning the above-mentioned polymer spinning solution to obtain a nanofiber membrane the process parameters of electrospinning can refer to the prior art. Specifically, copper foil was used as the receiving device, the voltage was set to 15kV, the pushing speed of the regulating solution was 1.5mL/h, and the distance between the needle tip for pushing the regulating solution and the receiving device was 12cm.
- This comparative example provides a method for regulating the pore structure of a nanofibrous membrane.
- the only difference between it and Example 7 is that the regulating agent used is composed of polyethylene glycol 35g, myristic acid 20g, isobutyl triethoxy It is obtained by mixing 5g of base silicon and 385g of water.
- the average molecular weight of polyethylene glycol was 800.
- This comparative example provides a method for regulating the pore structure of a nanofibrous membrane.
- the only difference between it and Example 9 is that the regulating agent used is composed of polyethylene glycol 35g, myristic acid 20g, isobutyl triethoxy It is obtained by mixing 5g of base silicon and 385g of water.
- the average molecular weight of polyethylene glycol was 800.
- This comparative example provides a method for regulating the pore structure of a nanofibrous membrane.
- the only difference between it and Example 12 is that the regulating agent used is composed of polyethylene glycol 35g, myristic acid 20g, isobutyl triethoxy It is obtained by mixing 5g of base silicon and 385g of water.
- the average molecular weight of polyethylene glycol was 800.
- This comparative example provides a method for regulating the pore structure of a nanofibrous membrane.
- the regulating agent used is composed of nano-silica 35g, polyethylene glycol 35g, isobutyltriethyl Obtained by mixing 5g of silicon oxide and 370g of water.
- the particle diameter of the nano-silica is 100 nm, and the average molecular weight of the polyethylene glycol is 800.
- This comparative example provides a method for regulating the pore structure of a nanofibrous membrane.
- the regulating agent used is composed of nano-silica 35g, polyethylene glycol 35g, isobutyltriethyl Obtained by mixing 5g of silicon oxide and 370g of water.
- the particle diameter of the nano-silica is 100 nm, and the average molecular weight of the polyethylene glycol is 800.
- This comparative example provides a method for regulating the pore structure of a nanofibrous membrane.
- the regulating agent used is composed of nano-silica 35g, polyethylene glycol 35g, isobutyltriethyl Obtained by mixing 5g of silicon oxide and 370g of water.
- the particle diameter of the nano-silica is 100 nm, and the average molecular weight of the polyethylene glycol is 800.
- This comparative example provides a method for regulating the pore structure of a nanofibrous membrane.
- the only difference between it and Example 7 is that the regulating agent used is composed of polyethylene glycol 35g, isobutyl triethoxy silicon 5g, water 405g obtained by mixing.
- the average molecular weight of polyethylene glycol was 800.
- This comparative example provides a method for regulating the pore structure of a nanofibrous membrane.
- the only difference between it and Example 9 is that the regulating agent used is composed of polyethylene glycol 35g, isobutyl triethoxy silicon 5g, water 405g obtained by mixing.
- the average molecular weight of polyethylene glycol was 800.
- This comparative example provides a method for regulating the pore structure of a nanofiber membrane.
- the only difference between it and Example 12 is that the regulating agent used is a mixture of 35 g of polyethylene glycol, 5 g of isobutyl triethoxy silicon, and 405 g of water. And get. In addition, the average molecular weight of polyethylene glycol was 800.
- nanofibrous membranes obtained in Examples 7-12 and Comparative Examples 1-10 above were tested for pore size and porosity using commercially available AutoPore V series mercury porosimeters, and the test results are shown in Table 1.
- nanofiber membrane Regulator addition amount % Pore diameter, nm Porosity,% Comparative example 1 0 100.5 65.6
- Example 8 0.5 205.5 73.2 Example 9 1 281.4 76.5 Example 10 2 342.2 80.2 Example 11 3 400.7 83.8 Example 12 5 501.5 85.1 Comparative example 2 0.1 115.8 68.2 Comparative example 3 1 185.2 69.5 Comparative example 4 5 253.5 71.3 Comparative example 5 0.1 118.9 69.3 Comparative example 6 1 192.4 70.1 Comparative example 7 5 275.8 73.7 Comparative example 8 0.1 108.5 66.2 Comparative example 9 1 123.8 67.3 Comparative example 10 5 152.3 68.6
- the present application carries out electrospinning after adding regulators containing nano silicon dioxide, polyethylene glycol, myristic acid and isobutyl triethoxy silicon to the polymer spinning solution.
- the pore structure of the nanofiber membrane can be regulated by adjusting the addition amount of the regulator, so as to change the pore size and porosity of the nanofiber membrane.
- This control method can realize the control of the pore structure of the nanofiber membrane only by changing the addition amount of the regulator, and it can realize a wide range of control of the pore size and porosity of the nanofiber membrane without changing the process parameters of electrospinning .
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Abstract
Procédé de régulation et de commande d'une structure des pores d'un film de nanofibres. Le procédé consiste : à préparer une solution de filage de polymère ; à ajouter un agent de régulation et de commande à la solution de filage de polymère et à la mélanger et à la disperser pour obtenir une solution de régulation et de commande, l'agent de régulation et de commande comprenant de la nano-silice, du glycol polyéthylénique, de l'acide myristique, de l'isobutyltriéthoxysilane et de l'eau ; et à filtrer la solution de régulation et de commande, puis à la soumettre à un filage électrostatique pour obtenir le film de nanofibres. Au moyen de l'ajout de l'agent de régulation et de commande à la solution de filage de polymère, puis de la réalisation d'un filage électrostatique, la structure des pores du film de nanofibres peut être régulée et commandée par ajustement de la quantité ajoutée d'agent de régulation et de commande de façon à modifier le diamètre des pores et la porosité du film de nanofibres.
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