CN113481659A - Method for regulating pore structure of nanofiber membrane - Google Patents
Method for regulating pore structure of nanofiber membrane Download PDFInfo
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- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
- D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
- D04H1/70—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres
- D04H1/72—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres the fibres being randomly arranged
- D04H1/728—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres the fibres being randomly arranged by electro-spinning
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- 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
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- 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
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- 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
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- 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
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- 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
Abstract
The invention is applicable to the technical field of nanofiber membranes, and provides a nanofiber membrane pore structure regulating method, which comprises the following steps: preparing a high-molecular spinning solution; adding a regulating agent into the macromolecular spinning solution for mixing and dispersing to obtain a regulating solution; the regulating agent comprises nano silicon dioxide, polydiethanol, myristic acid, isobutyl triethoxy silicon and water; and filtering the regulating solution, and then performing electrostatic spinning to obtain the nanofiber membrane. According to the invention, after the regulating agent is added into the polymer spinning solution, electrostatic spinning is carried out, and the pore structure of the nanofiber membrane can be regulated and controlled by regulating the addition amount of the regulating agent, so that the pore diameter and porosity of the nanofiber membrane can be changed. The regulation and control method can realize the regulation and control of the pore structure of the nanofiber membrane only by changing the addition amount of the regulating and control agent, and can realize the regulation and control of the pore diameter and the porosity of the nanofiber membrane in a larger range without changing the technological parameters of electrostatic spinning.
Description
Technical Field
The invention belongs to the technical field of nanofiber membranes, and particularly relates to a method for regulating and controlling a pore structure of a nanofiber membrane.
Background
Currently, there are many methods for producing nanofiber membranes, such as stretching, templated synthesis, self-assembly, microphase separation,Electrostatic spinningAnd the like. Wherein, high molecular polymer is used as raw materialElectrostatic spinningThe technology for manufacturing the nanofiber membrane is a common method, and the nanofiber membrane prepared by the method can be widely applied to the fields of water filtration, oil-water separation and the like. The pore structures of different nanofiber membranes can influence the functions and the purposes of the nanofiber membranes, so that the regulation of the pore structures of the nanofiber membranes is very important.
However, it is currently used for regulationElectrostatic spinningThe method for controlling the pore structure of the nanofiber membrane generally controls the technological parameters of electrostatic spinning, and not only is the pore structure difficult to control, but also the problem that the adjustable range of the pore size is small exists.
Disclosure of Invention
The embodiment of the invention aims to provide a method for regulating and controlling a pore structure of a nanofiber membrane, and aims to solve the problems in the background art.
The embodiment of the invention is realized in such a way that a method for regulating and controlling the pore structure of a nanofiber membrane comprises the following steps:
preparing a high-molecular spinning solution;
adding a regulating agent into the macromolecular spinning solution for mixing and dispersing to obtain a regulating solution; the regulating agent comprises the following components in parts by weight: 20-50 parts of nano silicon dioxide, 20-50 parts of polydiethylene alcohol, 10-30 parts of myristic acid, 1-10 parts of isobutyl triethoxy silicon and 200-500 parts of water;
and filtering the regulating solution, and then performing electrostatic spinning to obtain the nanofiber membrane.
As a preferable scheme of the embodiment of the invention, the regulating agent comprises the following components in parts by weight: 30-40 parts of nano silicon dioxide, 30-40 parts of polydiethylene alcohol, 15-25 parts of myristic acid, 4-6 parts of isobutyl triethoxy silicon and 300-400 parts of water.
In another preferable embodiment of the present invention, the added mass of the control agent is 0.1% to 5% of the mass of the polymer spinning solution.
As another preferable scheme of the embodiment of the invention, the particle size of the nano silicon dioxide is 50-150 nm.
In another preferable embodiment of the present invention, the average molecular weight of the polyethylene glycol is 400 to 1200.
As another preferable embodiment of the present invention, the method for preparing the polymer spinning solution comprises the following steps:
dissolving a high molecular polymer in a solvent to obtain a high molecular spinning solution; the mass ratio of the high molecular polymer to the solvent is (5-30) to (70-95).
In another preferred embodiment of the present invention, the high molecular polymer is at least one of polyvinyl alcohol, ethyl cellulose, hydroxyethyl cellulose, and polyvinyl pyrrolidone.
It should be noted that the high molecular polymer may adopt other water-soluble or alcohol-soluble high molecular materials, and is not limited to the above polymers, that is, the regulation method provided by the present invention is suitable for pore regulation of the nanofiber membrane of most water-soluble or alcohol-soluble high molecular materials.
As another preferable aspect of the embodiment of the present invention, the solvent is water and/or ethanol.
In another preferable scheme of the embodiment of the invention, in the step, the temperature for mixing and dispersing is 50-70 ℃.
In another preferable embodiment of the invention, in the step, the voltage is 10 to 20kV during electrostatic spinning.
According to the method for regulating and controlling the pore structure of the nanofiber membrane, provided by the embodiment of the invention, after the regulating and controlling agent containing nano silicon dioxide, polydiethylene alcohol, myristic acid and isobutyl triethoxy silicon is added into a high-molecular spinning solution, electrostatic spinning is carried out, so that the pore structure of the nanofiber membrane can be regulated and controlled by regulating the addition amount of the regulating and controlling agent, and the pore diameter and the porosity of the nanofiber membrane can be changed. The regulation and control method can realize the regulation and control of the pore structure of the nanofiber membrane only by changing the addition amount of the regulating and control agent, and can realize the regulation and control of the pore diameter and the porosity of the nanofiber membrane in a larger range without changing the technological parameters of electrostatic spinning.
Detailed Description
In order to clearly and completely describe the technical solutions in the embodiments of the present invention in combination with the embodiments of the present invention, it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
The embodiment provides a nanofiber membrane pore structure regulating method, which comprises the following steps:
s1, adding 5g of polyvinyl alcohol into 95g of solvent, and heating to 95 ℃ for dissolving to obtain a high-molecular spinning solution; wherein the solvent is water.
S2, adding 0.1g of regulating agent into 100g of the polymer spinning solution, placing the mixture at the temperature of 50 ℃, and mixing and dispersing the mixture for 20min at the rotating speed of 500rpm to obtain a regulating solution; wherein the regulating agent is prepared by mixing 20g of nano silicon dioxide, 20g of polydiethanol, 10g of myristic acid, 1g of isobutyl triethoxy silicon and 500g of water; the particle size of the nanosilica was 50nm, and the average molecular weight of the polyethylene glycol was 400.
And S3, filtering the regulating solution, and then performing electrostatic spinning on the filtrate to obtain the nanofiber membrane, thereby completing the regulation of the pore structure of the nanofiber membrane. The technical parameters of electrostatic spinning can refer to the prior art, specifically, a copper foil is used as a receiving device, the voltage is set to be 10kV, the pushing speed of the regulating solution is 1mL/h, and the distance between a needle point for pushing the regulating solution and the receiving device is 10 cm.
Example 2
The embodiment provides a nanofiber membrane pore structure regulating method, which comprises the following steps:
s1, adding 10g of ethyl cellulose and 20g of hydroxyethyl cellulose into 70g of solvent, and heating to 90 ℃ for dissolving to obtain a high-molecular spinning solution; wherein the solvent is a solution prepared by mixing water and ethanol according to an equal volume ratio.
S2, adding 5g of regulating agent into 100g of the polymer spinning solution, placing the mixture at the temperature of 70 ℃, and mixing and dispersing for 40min at the rotating speed of 1500rpm to obtain a regulating solution; wherein the regulating agent is prepared by mixing 50g of nano silicon dioxide, 50g of polydiethanol, 30g of myristic acid, 10g of isobutyl triethoxy silicon and 200g of water; the particle size of the nanosilica was 150nm, and the average molecular weight of the polyethylene glycol was 1200.
And S3, filtering the regulating solution, and then performing electrostatic spinning on the filtrate to obtain the nanofiber membrane, thereby completing the regulation of the pore structure of the nanofiber membrane. The technical parameters of electrostatic spinning can refer to the prior art, specifically, a copper foil is used as a receiving device, the voltage is set to be 20kV, the pushing speed of the regulating solution is 2mL/h, and the distance between a needle point for pushing the regulating solution and the receiving device is 15 cm.
Example 3
The embodiment provides a nanofiber membrane pore structure regulating method, which comprises the following steps:
s1, adding 10g of polyvinylpyrrolidone into 90g of solvent, and heating to 92 ℃ for dissolving to obtain a high-molecular spinning solution; wherein the solvent is water.
S2, adding 1g of regulating agent into 100g of the polymer spinning solution, placing the mixture at a temperature of 55 ℃, and mixing and dispersing for 30min at a rotating speed of 800rpm to obtain a regulating solution; wherein the regulating agent is prepared by mixing 25g of nano silicon dioxide, 25g of polydiethanol, 12g of myristic acid, 2g of isobutyl triethoxy silicon and 450g of water; the particle size of the nanosilica was 80nm, and the average molecular weight of the polyethylene glycol was 600.
And S3, filtering the regulating solution, and then performing electrostatic spinning on the filtrate to obtain the nanofiber membrane, thereby completing the regulation of the pore structure of the nanofiber membrane. The technical parameters of electrostatic spinning can refer to the prior art, specifically, a copper foil is used as a receiving device, the voltage is set to be 15kV, the pushing speed of the regulating solution is 1.5mL/h, and the distance between the needle point for pushing the regulating solution and the receiving device is 15 cm.
Example 4
The embodiment provides a nanofiber membrane pore structure regulating method, which comprises the following steps:
s1, adding 10g of polyvinyl alcohol and 10g of polyvinylpyrrolidone into 80g of solvent, and heating to 95 ℃ for dissolving to obtain a high-molecular spinning solution; wherein the solvent is a solution prepared by mixing water and ethanol according to an equal volume ratio.
S2, adding 3g of regulating agent into 100g of the polymer spinning solution, placing the mixture at the temperature of 60 ℃, and mixing and dispersing for 30min at the rotating speed of 1200rpm to obtain a regulating solution; wherein the regulating agent is prepared by mixing 45g of nano silicon dioxide, 45g of polydiethanol, 28g of myristic acid, 8g of isobutyl triethoxy silicon and 250g of water; the particle size of the nanosilica was 120nm, and the average molecular weight of the polyethylene glycol was 1000.
And S3, filtering the regulating solution, and then performing electrostatic spinning on the filtrate to obtain the nanofiber membrane, thereby completing the regulation of the pore structure of the nanofiber membrane. The technical parameters of electrostatic spinning can refer to the prior art, specifically, a copper foil is used as a receiving device, the voltage is set to be 15kV, the pushing speed of the regulating solution is 1.5mL/h, and the distance between the needle point for pushing the regulating solution and the receiving device is 12 cm.
Example 5
The embodiment provides a nanofiber membrane pore structure regulating method, which comprises the following steps:
s1, adding 5g of polyvinyl alcohol, 5g of ethyl cellulose and 5g of hydroxyethyl cellulose into 85g of solvent, and heating to 95 ℃ for dissolving to obtain a polymer spinning solution; wherein the solvent is a solution prepared by mixing water and ethanol according to an equal volume ratio.
S2, adding 2g of regulating agent into 100g of the polymer spinning solution, placing the mixture at the temperature of 60 ℃, and mixing and dispersing for 30min at the rotating speed of 1000rpm to obtain a regulating solution; wherein the regulating agent is prepared by mixing 30g of nano silicon dioxide, 30g of polydiethanol, 15g of myristic acid, 4g of isobutyl triethoxy silicon and 400g of water; the particle size of the nanosilica was 100nm, and the average molecular weight of the polyethylene glycol was 800.
And S3, filtering the regulating solution, and then performing electrostatic spinning on the filtrate to obtain the nanofiber membrane, thereby completing the regulation of the pore structure of the nanofiber membrane. The technical parameters of electrostatic spinning can refer to the prior art, specifically, a copper foil is used as a receiving device, the voltage is set to be 15kV, the pushing speed of the regulating solution is 1.5mL/h, and the distance between the needle point for pushing the regulating solution and the receiving device is 12 cm.
Example 6
The embodiment provides a nanofiber membrane pore structure regulating method, which comprises the following steps:
s1, adding 15g of polyvinylpyrrolidone into 85g of solvent, and heating to 92 ℃ for dissolving to obtain a high-molecular spinning solution; wherein the solvent is water.
S2, adding 2g of regulating agent into 100g of the polymer spinning solution, placing the mixture at the temperature of 60 ℃, and mixing and dispersing for 30min at the rotating speed of 1200rpm to obtain a regulating solution; wherein the regulating agent is prepared by mixing 40g of nano silicon dioxide, 40g of polydiethanol, 25g of myristic acid, 6g of isobutyl triethoxy silicon and 300g of water; the particle size of the nanosilica was 100nm, and the average molecular weight of the polyethylene glycol was 800.
And S3, filtering the regulating solution, and then performing electrostatic spinning on the filtrate to obtain the nanofiber membrane, thereby completing the regulation of the pore structure of the nanofiber membrane. The technical parameters of electrostatic spinning can refer to the prior art, specifically, a copper foil is used as a receiving device, the voltage is set to be 15kV, the pushing speed of the regulating solution is 1.5mL/h, and the distance between the needle point for pushing the regulating solution and the receiving device is 12 cm.
Example 7
The embodiment provides a nanofiber membrane pore structure regulating method, which comprises the following steps:
s1, adding 15g of polyvinylpyrrolidone into 85g of solvent, and heating to 92 ℃ for dissolving to obtain a high-molecular spinning solution; wherein the solvent is water.
S2, adding 0.1g of regulating agent into 100g of the polymer spinning solution, placing the mixture at the temperature of 60 ℃, and mixing and dispersing the mixture for 30min at the rotating speed of 1000rpm to obtain a regulating solution; wherein the regulating agent is prepared by mixing 35g of nano silicon dioxide, 35g of polydiethanol, 20g of myristic acid, 5g of isobutyl triethoxy silicon and 350g of water; the particle size of the nanosilica was 100nm, and the average molecular weight of the polyethylene glycol was 800.
And S3, filtering the regulating solution, and then performing electrostatic spinning on the filtrate to obtain the nanofiber membrane, thereby completing the regulation of the pore structure of the nanofiber membrane. The technical parameters of electrostatic spinning can refer to the prior art, specifically, a copper foil is used as a receiving device, the voltage is set to be 15kV, the pushing speed of the regulating solution is 1.5mL/h, and the distance between the needle point for pushing the regulating solution and the receiving device is 12 cm.
Example 8
The embodiment provides a nanofiber membrane pore structure regulating method, which comprises the following steps:
s1, adding 15g of polyvinylpyrrolidone into 85g of solvent, and heating to 92 ℃ for dissolving to obtain a high-molecular spinning solution; wherein the solvent is water.
S2, adding 0.5g of regulating agent into 100g of the polymer spinning solution, placing the mixture at the temperature of 60 ℃, and mixing and dispersing the mixture for 30min at the rotating speed of 1000rpm to obtain a regulating solution; wherein the regulating agent is prepared by mixing 35g of nano silicon dioxide, 35g of polydiethanol, 20g of myristic acid, 5g of isobutyl triethoxy silicon and 350g of water; the particle size of the nanosilica was 100nm, and the average molecular weight of the polyethylene glycol was 800.
And S3, filtering the regulating solution, and then performing electrostatic spinning on the filtrate to obtain the nanofiber membrane, thereby completing the regulation of the pore structure of the nanofiber membrane. The technical parameters of electrostatic spinning can refer to the prior art, specifically, a copper foil is used as a receiving device, the voltage is set to be 15kV, the pushing speed of the regulating solution is 1.5mL/h, and the distance between the needle point for pushing the regulating solution and the receiving device is 12 cm.
Example 9
The embodiment provides a nanofiber membrane pore structure regulating method, which comprises the following steps:
s1, adding 15g of polyvinylpyrrolidone into 85g of solvent, and heating to 92 ℃ for dissolving to obtain a high-molecular spinning solution; wherein the solvent is water.
S2, adding 1g of regulating agent into 100g of the polymer spinning solution, placing the mixture at the temperature of 60 ℃, and mixing and dispersing for 30min at the rotating speed of 1000rpm to obtain a regulating solution; wherein the regulating agent is prepared by mixing 35g of nano silicon dioxide, 35g of polydiethanol, 20g of myristic acid, 5g of isobutyl triethoxy silicon and 350g of water; the particle size of the nanosilica was 100nm, and the average molecular weight of the polyethylene glycol was 800.
And S3, filtering the regulating solution, and then performing electrostatic spinning on the filtrate to obtain the nanofiber membrane, thereby completing the regulation of the pore structure of the nanofiber membrane. The technical parameters of electrostatic spinning can refer to the prior art, specifically, a copper foil is used as a receiving device, the voltage is set to be 15kV, the pushing speed of the regulating solution is 1.5mL/h, and the distance between the needle point for pushing the regulating solution and the receiving device is 12 cm.
Example 10
The embodiment provides a nanofiber membrane pore structure regulating method, which comprises the following steps:
s1, adding 15g of polyvinylpyrrolidone into 85g of solvent, and heating to 92 ℃ for dissolving to obtain a high-molecular spinning solution; wherein the solvent is water.
S2, adding 2g of regulating agent into 100g of the polymer spinning solution, placing the mixture at the temperature of 60 ℃, and mixing and dispersing for 30min at the rotating speed of 1000rpm to obtain a regulating solution; wherein the regulating agent is prepared by mixing 35g of nano silicon dioxide, 35g of polydiethanol, 20g of myristic acid, 5g of isobutyl triethoxy silicon and 350g of water; the particle size of the nanosilica was 100nm, and the average molecular weight of the polyethylene glycol was 800.
And S3, filtering the regulating solution, and then performing electrostatic spinning on the filtrate to obtain the nanofiber membrane, thereby completing the regulation of the pore structure of the nanofiber membrane. The technical parameters of electrostatic spinning can refer to the prior art, specifically, a copper foil is used as a receiving device, the voltage is set to be 15kV, the pushing speed of the regulating solution is 1.5mL/h, and the distance between the needle point for pushing the regulating solution and the receiving device is 12 cm.
Example 11
The embodiment provides a nanofiber membrane pore structure regulating method, which comprises the following steps:
s1, adding 15g of polyvinylpyrrolidone into 85g of solvent, and heating to 92 ℃ for dissolving to obtain a high-molecular spinning solution; wherein the solvent is water.
S2, adding 3g of regulating agent into 100g of the polymer spinning solution, placing the mixture at the temperature of 60 ℃, and mixing and dispersing for 30min at the rotating speed of 1000rpm to obtain a regulating solution; wherein the regulating agent is prepared by mixing 35g of nano silicon dioxide, 35g of polydiethanol, 20g of myristic acid, 5g of isobutyl triethoxy silicon and 350g of water; the particle size of the nanosilica was 100nm, and the average molecular weight of the polyethylene glycol was 800.
And S3, filtering the regulating solution, and then performing electrostatic spinning on the filtrate to obtain the nanofiber membrane, thereby completing the regulation of the pore structure of the nanofiber membrane. The technical parameters of electrostatic spinning can refer to the prior art, specifically, a copper foil is used as a receiving device, the voltage is set to be 15kV, the pushing speed of the regulating solution is 1.5mL/h, and the distance between the needle point for pushing the regulating solution and the receiving device is 12 cm.
Example 12
The embodiment provides a nanofiber membrane pore structure regulating method, which comprises the following steps:
s1, adding 15g of polyvinylpyrrolidone into 85g of solvent, and heating to 92 ℃ for dissolving to obtain a high-molecular spinning solution; wherein the solvent is water.
S2, adding 5g of regulating agent into 100g of the polymer spinning solution, placing the mixture at the temperature of 60 ℃, and mixing and dispersing for 30min at the rotating speed of 1000rpm to obtain a regulating solution; wherein the regulating agent is prepared by mixing 35g of nano silicon dioxide, 35g of polydiethanol, 20g of myristic acid, 5g of isobutyl triethoxy silicon and 350g of water; the particle size of the nanosilica was 100nm, and the average molecular weight of the polyethylene glycol was 800.
And S3, filtering the regulating solution, and then performing electrostatic spinning on the filtrate to obtain the nanofiber membrane, thereby completing the regulation of the pore structure of the nanofiber membrane. The technical parameters of electrostatic spinning can refer to the prior art, specifically, a copper foil is used as a receiving device, the voltage is set to be 15kV, the pushing speed of the regulating solution is 1.5mL/h, and the distance between the needle point for pushing the regulating solution and the receiving device is 12 cm.
Comparative example 1
This comparative example provides a nanofiber membrane comprising the steps of:
s1, adding 15g of polyvinylpyrrolidone into 85g of solvent, and heating to 92 ℃ for dissolving to obtain a high-molecular spinning solution; wherein the solvent is water.
And S2, carrying out electrostatic spinning on the polymer spinning solution to obtain the nanofiber membrane. The technical parameters of electrostatic spinning can refer to the prior art, specifically, a copper foil is used as a receiving device, the voltage is set to be 15kV, the pushing speed of the regulating solution is 1.5mL/h, and the distance between the needle point for pushing the regulating solution and the receiving device is 12 cm.
Comparative example 2
The comparative example provides a method for regulating and controlling the pore structure of a nanofiber membrane, and the only difference between the method and the example 7 is that the adopted regulating and controlling agent is prepared by mixing 35g of polyethylene glycol, 20g of myristic acid, 5g of isobutyl triethoxy silicon and 385g of water; in addition, the average molecular weight of the polyethylene glycol was 800.
Comparative example 3
The comparative example provides a method for regulating and controlling the pore structure of a nanofiber membrane, and the only difference between the method and the example 9 is that the adopted regulating and controlling agent is prepared by mixing 35g of polyethylene glycol, 20g of myristic acid, 5g of isobutyl triethoxy silicon and 385g of water; in addition, the average molecular weight of the polyethylene glycol was 800.
Comparative example 4
The comparative example provides a method for regulating and controlling the pore structure of a nanofiber membrane, and the only difference between the method and the example 12 is that the adopted regulating and controlling agent is prepared by mixing 35g of polyethylene glycol, 20g of myristic acid, 5g of isobutyl triethoxy silicon and 385g of water; in addition, the average molecular weight of the polyethylene glycol was 800.
Comparative example 5
The comparative example provides a method for regulating and controlling the pore structure of a nanofiber membrane, and the only difference between the method and the embodiment 7 is that the adopted regulating and controlling agent is prepared by mixing 35g of nano silicon dioxide, 35g of polydiethanol, 5g of isobutyl triethoxy silicon and 370g of water; the particle size of the nanosilica was 100nm, and the average molecular weight of the polyethylene glycol was 800.
Comparative example 6
The comparative example provides a method for regulating and controlling the pore structure of a nanofiber membrane, and the only difference between the method and the example 9 is that the adopted regulating and controlling agent is prepared by mixing 35g of nano silicon dioxide, 35g of polydiethanol, 5g of isobutyl triethoxy silicon and 370g of water; the particle size of the nanosilica was 100nm, and the average molecular weight of the polyethylene glycol was 800.
Comparative example 7
The comparative example provides a method for regulating and controlling the pore structure of a nanofiber membrane, and the only difference between the method and the example 12 is that the adopted regulating and controlling agent is prepared by mixing 35g of nano silicon dioxide, 35g of polydiethylene alcohol, 5g of isobutyl triethoxy silicon and 370g of water; the particle size of the nanosilica was 100nm, and the average molecular weight of the polyethylene glycol was 800.
Comparative example 8
The comparative example provides a method for regulating and controlling the pore structure of a nanofiber membrane, and the only difference between the method and the embodiment 7 is that the adopted regulating and controlling agent is prepared by mixing 35g of polydiethylene alcohol, 5g of isobutyl triethoxy silicon and 405g of water; in addition, the average molecular weight of the polyethylene glycol was 800.
Comparative example 9
The comparative example provides a method for regulating and controlling the pore structure of a nanofiber membrane, and the only difference between the method and the example 9 is that the adopted regulating and controlling agent is prepared by mixing 35g of polydiethylene alcohol, 5g of isobutyl triethoxy silicon and 405g of water; in addition, the average molecular weight of the polyethylene glycol was 800.
Comparative example 10
The comparative example provides a method for regulating and controlling the pore structure of a nanofiber membrane, and the only difference between the method and the example 12 is that the adopted regulating and controlling agent is prepared by mixing 35g of polydiethylene alcohol, 5g of isobutyl triethoxy silicon and 405g of water; in addition, the average molecular weight of the polyethylene glycol was 800.
The pore size and porosity of the nanofiber membranes obtained in examples 7 to 12 and comparative examples 1 to 10 were measured by a commercially available AutoPore V series mercury porosimeter, and the results are shown in table 1.
TABLE 1
As can be seen from table 1, in the present invention, after a control agent containing nano-silica, polydiethylene alcohol, myristic acid, and isobutyl triethoxy silicon is added to a polymer spinning solution, electrostatic spinning is performed, so that the pore structure of the nanofiber membrane can be controlled by adjusting the addition amount of the control agent, so as to change the pore diameter and porosity of the nanofiber membrane. The regulation and control method can realize the regulation and control of the pore structure of the nanofiber membrane only by changing the addition amount of the regulating and control agent, and can realize the regulation and control of the pore diameter and the porosity of the nanofiber membrane in a larger range without changing the technological parameters of electrostatic spinning.
Furthermore, it should be understood that although the present description refers to embodiments, not every embodiment may contain only a single embodiment, and such description is for clarity only, and those skilled in the art should integrate the description, and the embodiments may be combined as appropriate to form other embodiments understood by those skilled in the art.
Claims (10)
1. A nanofiber membrane pore structure regulating method is characterized by comprising the following steps:
preparing a high-molecular spinning solution;
adding a regulating agent into the macromolecular spinning solution for mixing and dispersing to obtain a regulating solution; the regulating agent comprises the following components in parts by weight: 20-50 parts of nano silicon dioxide, 20-50 parts of polydiethylene alcohol, 10-30 parts of myristic acid, 1-10 parts of isobutyl triethoxy silicon and 200-500 parts of water;
and filtering the regulating solution, and then performing electrostatic spinning to obtain the nanofiber membrane.
2. The method for regulating the pore structure of the nanofiber membrane as claimed in claim 1, wherein the regulating agent comprises the following components in parts by weight: 30-40 parts of nano silicon dioxide, 30-40 parts of polydiethylene alcohol, 15-25 parts of myristic acid, 4-6 parts of isobutyl triethoxy silicon and 300-400 parts of water.
3. The method for regulating the pore structure of the nanofiber membrane as claimed in claim 1 or 2, wherein the addition mass of the regulating agent is 0.1-5% of the mass of the polymer spinning solution.
4. The method for regulating and controlling the pore structure of the nanofiber membrane as claimed in claim 1 or 2, wherein the particle size of the nano silica is 50-150 nm.
5. The method for regulating and controlling the pore structure of the nanofiber membrane as claimed in claim 1 or 2, wherein the average molecular weight of the polyethylene glycol is 400-1200.
6. The method for regulating and controlling the pore structure of the nanofiber membrane as claimed in claim 1, wherein the preparation method of the polymer spinning solution comprises the following steps:
dissolving a high molecular polymer in a solvent to obtain a high molecular spinning solution; the mass ratio of the high molecular polymer to the solvent is (5-30) to (70-95).
7. The method for regulating the pore structure of the nanofiber membrane as claimed in claim 6, wherein the high molecular polymer is at least one of polyvinyl alcohol, ethyl cellulose, hydroxyethyl cellulose and polyvinylpyrrolidone.
8. The method for regulating the pore structure of the nanofiber membrane as claimed in claim 6 or 7, wherein the solvent is water and/or ethanol.
9. The method for regulating and controlling the pore structure of the nanofiber membrane as claimed in claim 1, wherein in the step, the temperature for mixing and dispersing is 50-70 ℃.
10. The method for regulating the pore structure of the nanofiber membrane as claimed in claim 1, wherein in the step, the voltage is 10-20 kV during electrostatic spinning.
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