CN111549529B - Non-woven fabric material and preparation method and application thereof - Google Patents
Non-woven fabric material and preparation method and application thereof Download PDFInfo
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- CN111549529B CN111549529B CN202010404892.7A CN202010404892A CN111549529B CN 111549529 B CN111549529 B CN 111549529B CN 202010404892 A CN202010404892 A CN 202010404892A CN 111549529 B CN111549529 B CN 111549529B
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M14/00—Graft polymerisation of monomers containing carbon-to-carbon unsaturated bonds on to fibres, threads, yarns, fabrics, or fibrous goods made from such materials
- D06M14/08—Graft polymerisation of monomers containing carbon-to-carbon unsaturated bonds on to fibres, threads, yarns, fabrics, or fibrous goods made from such materials on to materials of synthetic origin
- D06M14/10—Graft polymerisation of monomers containing carbon-to-carbon unsaturated bonds on to fibres, threads, yarns, fabrics, or fibrous goods made from such materials on to materials of synthetic origin of macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D39/00—Filtering material for liquid or gaseous fluids
- B01D39/08—Filter cloth, i.e. woven, knitted or interlaced material
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M14/00—Graft polymerisation of monomers containing carbon-to-carbon unsaturated bonds on to fibres, threads, yarns, fabrics, or fibrous goods made from such materials
- D06M14/08—Graft polymerisation of monomers containing carbon-to-carbon unsaturated bonds on to fibres, threads, yarns, fabrics, or fibrous goods made from such materials on to materials of synthetic origin
- D06M14/12—Graft polymerisation of monomers containing carbon-to-carbon unsaturated bonds on to fibres, threads, yarns, fabrics, or fibrous goods made from such materials on to materials of synthetic origin of macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M14/14—Polyesters
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M16/00—Biochemical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. enzymatic
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M8/00—Fuel cells; Manufacture thereof
- H01M8/06—Combination of fuel cells with means for production of reactants or for treatment of residues
- H01M8/0662—Treatment of gaseous reactants or gaseous residues, e.g. cleaning
- H01M8/0687—Reactant purification by the use of membranes or filters
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2239/00—Aspects relating to filtering material for liquid or gaseous fluids
- B01D2239/04—Additives and treatments of the filtering material
- B01D2239/0442—Antimicrobial, antibacterial, antifungal additives
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2239/00—Aspects relating to filtering material for liquid or gaseous fluids
- B01D2239/06—Filter cloth, e.g. knitted, woven non-woven; self-supported material
- B01D2239/0604—Arrangement of the fibres in the filtering material
- B01D2239/0618—Non-woven
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/50—Fuel cells
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
Abstract
The invention provides a method for preparing a non-woven fabric material, the non-woven fabric material prepared by the method and application of the non-woven fabric material in a filter. Wherein the method for preparing the non-woven fabric material comprises the following steps: (1) adding a quaternary phosphonium salt monomer into deionized water, and uniformly stirring to ensure that the molar concentration of the quaternary phosphonium salt monomer is 0.5-1.0 mol/L so as to obtain a solution A; (2) adding an initiator into the solution A to obtain a solution B; (3) adding non-woven fabrics into the solution B and uniformly stirring to obtain a mixture C; (4) introducing nitrogen into the mixture C, bubbling for 10min, sealing, and carrying out redox grafting reaction in a constant-temperature water bath; and (5) washing a product after the oxidation-reduction grafting reaction with acetone, then extracting for 24 hours, and drying to obtain the non-woven fabric material. The non-woven fabric material prepared by the method has strong filtering performance and good antibacterial and antiseptic properties.
Description
Technical Field
The invention belongs to the field of materials, and particularly relates to a method for preparing a non-woven fabric material, the non-woven fabric material prepared by the method and application of the non-woven fabric material in a filter.
Background
With the continuous development of economy in China, automobiles are indispensable transportation means in daily life of people. With the increase of the possession of private automobiles in cities year by year, the air pollution condition on roads is increasingly serious, the space in the automobiles is narrow, the air circulation is poor, the diffusion of pollutants is not facilitated, bacteria are easy to breed, and great harm is brought to the health of automobile owners. How to improve the quality of air in the vehicle becomes a topic of close attention of the majority of vehicle owners, and an air conditioner filter with an antibacterial function is an effective means for solving the problem.
A Proton Exchange Membrane Fuel Cell (PEMFC) is a device that can directly convert chemical energy of fuel (usually hydrogen or methanol) and oxidant (oxygen or air) into electrical energy, and has the advantages of high energy conversion efficiency, no environmental pollution, simple structure, and low influence of load change on power generation efficiency, and is considered to be a type of cell with the greatest development prospect. In recent years, Fuel Cell Vehicles (FCV) and proton exchange membrane fuel cell (pem) technologies have been rapidly promoted along with the rapid development of new energy vehicles. An air filter with high efficiency and gas filtering and antibacterial functions is required to be used in the fuel cell system, and the device is an important accessory of the fuel cell system and directly influences the service life of the fuel cell.
Therefore, it is highly desirable to develop a material suitable for an air filter and having both filtering and antibacterial functions.
Disclosure of Invention
The present invention is directed to solving, at least to some extent, one of the technical problems in the related art. Therefore, one object of the present invention is to provide a non-woven fabric material for a vehicle air conditioner filter and a preparation method thereof, wherein the non-woven fabric material has antibacterial and antifungal properties on the premise of maintaining its own filtering performance, and therefore can be used in the application fields of vehicle air conditioner filters, proton exchange membrane fuel cell air filters, and the like, so as to effectively improve the quality of air in vehicles and prolong the service life of fuel cells.
According to one aspect of the invention, there is provided a method of making a nonwoven material, the method comprising:
(1) adding a quaternary phosphonium salt monomer into deionized water, and uniformly stirring to ensure that the molar concentration of the quaternary phosphonium salt monomer is 0.5-1.0 mol/L so as to obtain a solution A;
(2) adding an initiator into the solution A to ensure that the molar concentration of the initiator is 0.02-0.05 mol/L so as to obtain a solution B;
(3) adding non-woven fabrics into the solution B, and uniformly stirring to ensure that the mass ratio of the non-woven fabrics to the solution B is 1: 20-1: 100 so as to obtain a mixture C;
(4) filling nitrogen into the mixture C, bubbling for 10min, sealing, and carrying out redox grafting reaction in a constant-temperature water bath; and
(5) and washing a product after the oxidation-reduction grafting reaction with acetone, extracting for 24 hours, and drying to obtain the non-woven fabric material.
Therefore, the non-woven fabric material with both filtering performance and antibacterial and mildewproof performance can be prepared by adopting the method for preparing the non-woven fabric material provided by the embodiment of the invention, the preparation method is simple and feasible, the cost is low, and quaternary phosphonium salt can be effectively grafted on the surface of the non-woven fabric, so that the non-woven fabric has good antibacterial and mildewproof performance, and the application range of the non-woven fabric is expanded. Therefore, the non-woven fabric product prepared by the method can be used for an air filter in an automobile and an air filter in a fuel cell system, so that the quality of air in the automobile can be effectively improved, and the service life of the fuel cell can be effectively prolonged.
In addition, the method for preparing a nonwoven material according to the above embodiment of the present invention may also have the following additional technical features:
in some embodiments of the present invention, the quaternary phosphonium salt monomer is methacryloyloxyheptyl-tributylphosphonium chloride.
In some embodiments of the invention, the initiator is cerium ammonium nitrate, cerium ammonium sulfate, or ammonium thiosulfate.
In some embodiments of the invention, the non-woven fabric is a polypropylene filter cloth or a polyethylene terephthalate filter cloth.
In some embodiments of the present invention, the redox grafting reaction is performed at a reaction temperature of 30 ℃ to 60 ℃ for a reaction time of 60min to 120 min.
According to another aspect of the present invention, there is also provided a nonwoven material prepared by the method of the preceding embodiment, which, according to an embodiment of the present invention, comprises: the non-woven fabric comprises a non-woven fabric substrate and a quaternary phosphonium salt monomer layer, wherein the quaternary phosphonium salt monomer layer is formed on the surface of the non-woven fabric substrate through oxidation-reduction grafting reaction.
According to a further aspect of the invention, the invention further provides the use of the nonwoven material according to the preceding embodiment in a filter, which is a filter for an air conditioner for a vehicle or a filter for a fuel cell.
Drawings
FIG. 1 is a schematic diagram of a grafting reaction in the preparation of a nonwoven material in accordance with one embodiment of the present invention.
FIG. 2 is a graph of the EDS element distribution of a nonwoven fabric material prepared in example 3 of the present invention, the presence of elements N, O and Cl indicating that quaternary phosphonium salt monomers have been grafted to the surface of the nonwoven fabric material.
Detailed Description
The following detailed description of the embodiments of the invention, which is intended to be illustrative and not to be construed as limiting the invention.
According to one aspect of the invention, there is provided a method of making a nonwoven material, the method comprising:
(1) adding a quaternary phosphonium salt monomer into deionized water, and uniformly stirring to ensure that the molar concentration of the quaternary phosphonium salt monomer is 0.5-1.0 mol/L so as to obtain a solution A;
(2) adding an initiator into the solution A to ensure that the molar concentration of the initiator is 0.02-0.05 mol/L so as to obtain a solution B;
(3) adding a non-woven fabric into the solution B, and uniformly stirring to ensure that the mass ratio of the non-woven fabric to the solution B is 1: 20-1: 100 so as to obtain a mixture C;
(4) filling nitrogen into the mixture C, bubbling for 10min, sealing, and carrying out redox grafting reaction in a constant-temperature water bath; and
(5) washing the product after the oxidation-reduction grafting reaction with acetone, then extracting for 24 hours, and drying at the temperature of below 60 ℃ so as to obtain the non-woven fabric material.
Therefore, the non-woven fabric material with both filtering performance and antibacterial and mildewproof performance can be prepared by adopting the method for preparing the non-woven fabric material provided by the embodiment of the invention, the preparation method is simple and easy to implement, and the quaternary phosphonium salt can be effectively grafted on the surface of the non-woven fabric, so that the non-woven fabric has good antibacterial and mildewproof performance, and the application range of the non-woven fabric is expanded. Therefore, the non-woven fabric product prepared by the method can be used for an air filter in an automobile and an air filter in a fuel cell system, so that the quality of air in the automobile can be effectively improved, and the service life of the fuel cell can be effectively prolonged.
The method of preparing the nonwoven material according to the above embodiment of the present invention will be described in detail.
(1) Firstly, adding a quaternary phosphonium salt monomer into deionized water, and uniformly stirring to ensure that the molar concentration of the quaternary phosphonium salt monomer is 0.5-1.0 mol/L so as to obtain a solution A. Thereby preparing a quaternary phosphonium salt monomer solution.
According to a specific embodiment of the present invention, the quaternary phosphonium salt monomer is preferably methacryloyloxyheptyl-tributylphosphonium chloride. Because, the inventors found that by grafting a nonwoven fabric with methacryloyloxyheptyl-tributylphosphine chloride as a quaternary phosphonium salt monomer, it can be judged from the change in air permeability and filtration efficiency of the nonwoven fabric that there is no reduction in filtration performance of the nonwoven fabric. In addition, methacryloxypentyl heptyl-tributyl phosphine chloride is used as the quaternary phosphonium salt monomer grafted non-woven fabric, antibacterial performance evaluation is carried out on the non-woven fabric, evaluation results on escherichia coli and staphylococcus aureus are good, and the antibacterial effect is achieved. The antibacterial and mildewproof grade can reach 0 grade by testing, which shows that the mildewproof effect is good. Therefore, the inventor thinks that aiming at the non-woven fabric material, the methacrylatioheptyl-tributyl phosphonium chloride is adopted as the best choice for the quaternary phosphonium salt monomer, and the performance of the methacrylatioheptyl-tributyl phosphonium chloride and the quaternary phosphonium salt monomer can be exerted, and the performance of the methacrylatioheptyl-tributyl phosphonium chloride and the quaternary phosphonium salt monomer can not be influenced, so that the filterability and the mildew-proof and antibacterial performance of the prepared non-woven fabric material are improved to the maximum extent.
In addition, the molar concentration of the quaternary phosphonium salt monomer in the solution A prepared is 0.5-1.0 mol/L. Therefore, the concentration of the quaternary phosphonium salt monomer can be ensured to be enough to improve the grafting rate, so that the sufficient mildew-proof antibacterial performance is obtained, and in addition, the concentration is not easy to be too high, so that the influence of grafting too much quaternary phosphonium salt monomer on the filtering performance of the non-woven fabric is avoided. Specifically, the quaternary phosphonium salt monomer molar concentration in the solution A can be 0.5mol/L, 0.6mol/L, 0.7mol/L, 0.8mol/L, 0.9mol/L or 1.0 mol/L. And then the non-woven fabric material with good filtering property, antibacterial property and mildew resistance can be prepared.
(2) Then, an initiator is added to the solution A so that the molar concentration of the initiator is 0.02mol/L to 0.05mol/L, thereby obtaining a solution B.
According to a specific embodiment of the present invention, the initiator is cerium ammonium nitrate, cerium ammonium sulfate or ammonium thiosulfate. The inventors have found that the grafting efficiency and grafting yield of the quaternary phosphonium salt monomer can be significantly improved by employing several of the above initiators. Therefore, in order to effectively graft the quaternary phosphonium salt monomer with antibacterial activity on the non-woven fabric, the inventor optimizes the combination of the initiator of ammonium cerium nitrate, ammonium cerium sulfate or ammonium thiosulfate and methacryloyloxyheptyl-tributylphosphine chloride, and further ensures that the quaternary phosphonium salt monomer can be effectively grafted on the surface of the non-woven fabric.
In addition, in the solution B containing the quaternary phosphonium salt monomer and the initiator prepared in the above way, the concentrations of the quaternary phosphonium salt monomer and the initiator are respectively 0.5mol/L to 1.0mol/L of the molar concentration of the quaternary phosphonium salt monomer and 0.02mol/L to 0.05mol/L of the molar concentration of the initiator. Therefore, the grafting efficiency and the grafting rate of the quaternary phosphonium salt monomer can be obviously improved by adopting the concentration ratio. The mass percentage concentration of the photoinitiator is obtained by matching according to the molar concentration of the pyridinium monomer, and the photoinitiator has the most appropriate initiation effect in the solution B, so that the grafting efficiency can be effectively improved. If the initiator concentration is too high, two problems arise:
1. the grafting reaction speed is too high, the grafting reaction is incomplete, the degradation and chain scission of a polymer chain can be caused, the grafting efficiency is reduced, and the antibacterial effect is influenced;
2. the cost of the initiator is increased, so that the cost of the grafted non-woven fabric is increased, and the product application is not facilitated.
(3) And then adding a non-woven fabric into the solution B containing the quaternary phosphonium salt monomer and the initiator, and uniformly stirring to ensure that the mass ratio of the non-woven fabric to the solution B is 1: 20-1: 100 so as to obtain a mixture C.
According to the specific embodiment of the invention, the mass ratio of the non-woven fabric to the solution B is controlled to be 1: 20-1: 100, so that the moderate ratio of the quaternary phosphonium salt monomer to the non-woven fabric can be ensured, and the prepared non-woven fabric monomer can maintain the filtering performance to the maximum extent and simultaneously increase the effective antibacterial and antiseptic performance. According to a specific example of the present invention, the mass ratio of the non-woven fabric to the solution B may be 1:20, 1:25, 1:30, 1:35, 1:40, 1:45, 1:50, 1:55, 1:60, 1:65, 1:70, 1:75, 1:80, 1:85, 1:90, 1:95, or 1: 100. Therefore, the quaternary phosphonium salt monomer with enough quantity can be grafted on the surface of the non-woven fabric, so that the prepared non-woven fabric monomer has good antibacterial effect and 0-grade mildew-proof grade. In addition, the inventor also finds that in the mixture C, the addition amount of the non-woven fabric is not easy to be too large or too small, because the addition amount is too small, the yield of the grafted non-woven fabric is reduced, the production efficiency and the cost are influenced, a multi-graft network is easy to form on the surface of the non-woven fabric, and the phenomenon of barrier of a penetration step caused by similar long molecular chains occurs, so that the antibacterial performance is reduced; and too large addition can lead to the non-woven fabric not to effectively unfold in the solution, and phenomena such as lamination shielding, winding and the like are easily generated, and grafting reaction can not be carried out on the surface of the non-woven fabric, so that the antibacterial performance is reduced, and the product performance and the production efficiency of the grafted non-woven fabric are influenced.
In addition, according to an embodiment of the present invention, the non-woven fabric used may be a polypropylene (PP) filter cloth or a polyethylene terephthalate (PET) filter cloth. Because the polypropylene filter cloth and the polyethylene glycol terephthalate filter cloth have good filtering performance, the polypropylene filter cloth and the polyethylene glycol terephthalate filter cloth can be used for a filter element of a filter, and the filtering effect can be obviously improved. The invention adopts polypropylene (PP) filter cloth or polyethylene terephthalate (PET) filter cloth, and quaternary phosphonium salt monomer is grafted on the surface of the PP filter cloth or the PET filter cloth, so that the non-woven fabric can be further endowed with excellent antibacterial and antiseptic properties, and the filtering effect and the service life of the non-woven fabric material are further obviously improved. In addition, the polypropylene (PP) filter cloth or the polyethylene terephthalate (PET) filter cloth is adopted for grafting the quaternary phosphonium salt monomer, so that the original filtering performance can be easily maintained, and the influence of the grafted quaternary phosphonium salt monomer on the filtering performance is reduced. In addition, the inventor finds that the non-woven fabric material prepared by the non-woven fabric is more suitable for an air filter in an automobile and an air filter in a fuel cell system, and further can effectively improve the quality of air in the automobile and prolong the service life of a fuel cell.
(4) And then, filling nitrogen into the mixture C, bubbling for 10min, sealing, and carrying out redox grafting reaction in a constant-temperature water bath.
According to the specific embodiment of the invention, the initiator in the mixture C enables the surface of the non-woven fabric to form carbon free radicals, and the quaternary phosphonium salt monomer and the carbon free radicals undergo redox grafting reaction and are grafted on the non-woven fabric.
According to the specific embodiment of the present invention, the inventors have found that when the quaternary phosphonium salt monomer is preferably methacryloyloxyheptyl-tributylphosphine chloride, the formula of which is shown in the specification
The grafting reaction with the nonwoven fabric is shown in FIG. 1. When the methacryloyloxyheptyl-tributylphosphine chloride is adopted, the inventor finds that the length of a molecular chain of the methacryloyloxyheptyl-tributylphosphine salt is moderate from the antibacterial mechanism analysis of the quaternary phosphonium salt antibacterial agent, so that the antibacterial group density can be improved, the antibacterial performance of a grafted non-woven fabric product can be improved, the gas penetration step blockage caused by a high-molecular-weight long molecular chain can be avoided, and the high molecular chain can be prevented from being broken under the actions of high temperature, illumination and oxygen to form harmful gases such as acetaldehyde and formaldehyde and the like, so that the air quality in the whole vehicle can be influenced. In addition, the adoption of the tributyl can not only improve the antibacterial property, but also reduce the toxicity of the quaternary phosphonium salt antibacterial agent, so that compared with other types of quaternary phosphonium salt antibacterial agents and the like, the methacryloxypropyl-tributyl phosphine chloride is more suitable for being used in vehicle air conditioner filters and fuel cell filters.
According to the specific embodiment of the present invention, the inventor further studied the reaction conditions for grafting the quaternary phosphonium salt monomer on the surface of the non-woven fabric, and when the reaction temperature of the redox grafting reaction is controlled to be 30 ℃ to 60 ℃, specifically 30 ℃, 35 ℃, 40 ℃, 45 ℃, 50 ℃, 55 ℃ or 60 ℃, the reaction time is 60min to 120min, specifically 60min, 65min, 70min, 75min, 80min, 85min, 90min, 95min, 100min, 105min, 110min, 115min or 120 min. Therefore, the grafting reaction can be further ensured to be smooth, the optimal grafting effect is achieved, namely the finally obtained non-woven fabric material basically keeps the original filtering performance and effectively increases the antibacterial and anticorrosive performance, the antibacterial effect is good through testing, the anticorrosive grade reaches 0 grade, and the filtering performance is hardly influenced.
(5) And finally, washing the product after the redox grafting reaction by using acetone, extracting for 24 hours, and drying at the temperature of below 60 ℃ so as to obtain the non-woven fabric material.
According to a particular embodiment of the invention, the method for preparing the nonwoven material proposed by the invention is preferably:
(1) adding methacryloxy heptyl-tributyl phosphine chloride into deionized water, and uniformly stirring to ensure that the molar concentration of the methacryloxy heptyl-tributyl phosphine chloride is 0.5-1.0 mol/L so as to obtain a solution A;
(2) adding ammonium ceric nitrate, ammonium ceric sulfate or ammonium thiosulfate into the solution A, wherein the molar concentration is 0.02-0.05 mol/L, so as to obtain a solution B;
(3) adding polypropylene spray-melted non-woven fabric into the solution B, and uniformly stirring to ensure that the mass ratio of the non-woven fabric to the solution B is 1: 20-1: 100 so as to obtain a mixture C;
(4) filling nitrogen into the mixture C, bubbling for 10min, sealing, and carrying out oxidation-reduction grafting reaction in a constant-temperature water bath at the reaction temperature of 30-60 ℃ for 60-120 min; and
(5) washing the product after the oxidation-reduction grafting reaction with acetone, extracting for 24 hours, and drying at the temperature of below 60 ℃ to obtain the non-woven fabric material.
Therefore, by adopting the method, a proper amount of methacryloyloxyheptyl-tributylphosphine chloride can be effectively grafted on the surface of the non-woven fabric, so that the finally obtained non-woven fabric material basically keeps the original filtering performance and effectively increases the antibacterial and anticorrosive performances, and the antibacterial effect is good through tests, and the anticorrosive grade reaches 0 level.
According to another aspect of the present invention, there is also provided a nonwoven material prepared by the method of the preceding embodiment, which, according to an embodiment of the present invention, comprises: the quaternary phosphonium salt non-woven fabric comprises a non-woven fabric substrate and a quaternary phosphonium salt monomer layer, wherein the quaternary phosphonium salt monomer layer is grafted on the surface of the non-woven fabric substrate through an oxidation-reduction reaction. The non-woven fabric material basically keeps the original filtering performance, meanwhile, the antibacterial and anticorrosive performance is effectively improved, the antibacterial effect is good through tests, and the anticorrosive grade reaches 0 grade.
According to a further aspect of the invention, the invention further provides the use of the nonwoven material according to the preceding embodiment in a filter, which is a filter for an air conditioner for a vehicle or a filter for a fuel cell. The non-woven fabric material has strong filtering performance and good antibacterial and anticorrosive performance, so that the non-woven fabric material can be used for an air conditioner filter or a fuel cell filter for a vehicle, and the quality of air in the vehicle and the service life of the fuel cell can be obviously improved.
Example 1
The invention provides a grafted quaternary phosphonium salt non-woven fabric material for an air-conditioning filter for a vehicle and a preparation method thereof, which are characterized in that the surface of the non-woven fabric for the air-conditioning filter is modified by oxidation-reduction grafting, and a grafted layer is formed by a grafted quaternary phosphonium salt monomer, and the method comprises the following steps:
(1) adding a quaternary phosphonium salt monomer material (methacryloyloxyheptyl-tributyl phosphonium chloride) into deionized water, and uniformly stirring to ensure that the molar concentration of the quaternary phosphonium salt monomer is 0.5mol/L, which is defined as a solution A;
(2) adding a cerium ammonium nitrate initiator into the solution A to ensure that the molar concentration of the cerium ammonium nitrate initiator is 0.02mol/L, and defining the solution A as a solution B;
(3) placing the solution B into the solution B with an area of 100cm 2 PP non-woven material (gram weight 120 g/m) 2 ) Uniformly stirring to ensure that the mass ratio of the non-woven fabric to the solution B is 1:20, and defining the mixture as a mixture C;
(4) introducing nitrogen into the mixture C, bubbling for 10min, exhausting air, sealing, and carrying out oxidation-reduction grafting reaction in a constant-temperature water bath at the reaction temperature of 60 ℃ for 60 min;
(5) the grafted non-woven fabric is washed by acetone, then extracted for 10 hours and dried.
The results of the tests carried out on the nonwoven materials obtained in steps (1) to (5) are as follows: the air permeability of the non-woven fabric material before surface grafting treatment is 3000mm/s, and the PM2.5 filtration efficiency is 80%; after the surface grafting treatment, the air permeability of the nonwoven material was 2953mm/s and the PM2.5 filtration efficiency was 80%. The change in air permeability and filtration efficiency was used to determine that the nonwoven fabric had not degraded filtration performance. In addition, the non-woven fabric material for in-vehicle air purification has good antibacterial and mildewproof effects, and is prepared according to GB/T20944.1-2007 evaluation part 1 of antibacterial properties of textiles: the evaluation results of the agar plate diffusion method are good, which shows that the antibacterial effect is achieved; the test is carried out according to the GB/T24346-one 2009 evaluation of the mildew-proof performance of the textile, the mildew-proof grade is 0 grade, and the good mildew-proof effect is shown.
Example 2
The invention provides a grafted quaternary phosphonium salt non-woven fabric material for an air-conditioning filter for a vehicle and a preparation method thereof, which are characterized in that the surface of the non-woven fabric for the air-conditioning filter is modified by oxidation-reduction grafting, and a grafted layer is formed by a grafted quaternary phosphonium salt monomer, and the grafted quaternary phosphonium salt non-woven fabric material comprises the following steps:
(1) adding a quaternary phosphonium salt monomer material (methacryloyloxyheptyl-tributylphosphine chloride) into deionized water, and uniformly stirring to ensure that the molar concentration of the quaternary phosphonium salt monomer is 1.0mol/L, which is defined as a solution A;
(2) adding a cerium ammonium sulfate initiator into the solution A to ensure that the molar concentration of the cerium ammonium sulfate initiator is 0.04mol/L, and defining the solution A as a solution B;
(3) placing the solution B into the solution B with an area of 100cm 2 PET non-woven material (gram weight 150 g/m) 2 ) Uniformly stirring to ensure that the mass ratio of the non-woven fabric to the solution B is 1:60, and defining the mixture as a mixture C;
(4) introducing nitrogen into the mixture C, bubbling for 10min, exhausting air, sealing, and carrying out oxidation-reduction grafting reaction in a constant-temperature water bath at the reaction temperature of 50 ℃ for 60 min;
(5) the grafted non-woven fabric is washed by acetone, then extracted for 10 hours and dried.
The results of the tests carried out on the nonwoven materials obtained in steps (1) to (5) are as follows: the air permeability of the non-woven fabric material before surface grafting treatment is 2800mm/s, and the PM2.5 filtration efficiency is 85%; after the surface grafting treatment, the air permeability of the non-woven material is 2721mm/s, and the PM2.5 filtration efficiency is 83%. From the changes in air permeability and filtration efficiency, it was judged that the nonwoven fabric had little decrease in filtration performance. In addition, the non-woven fabric material for in-vehicle air purification has good antibacterial and mildewproof effects, and is prepared according to GB/T20944.1-2007 evaluation part 1 of antibacterial properties of textiles: the evaluation results of the agar plate diffusion method are good, which shows that the antibacterial effect is achieved; the test is carried out according to the GB/T24346-one 2009 evaluation of the mildew resistance of textiles, the mildew resistance grade is 0, and the good mildew resistance effect is shown.
Example 3
The invention provides a grafted quaternary phosphonium salt non-woven fabric material for an air-conditioning filter for a vehicle and a preparation method thereof, which are characterized in that the surface of the non-woven fabric for the air-conditioning filter is modified by oxidation-reduction grafting, and a grafted layer is formed by a grafted quaternary phosphonium salt monomer, and the method comprises the following steps:
(1) adding a quaternary phosphonium salt monomer material (methacryloyloxyheptyl-tributyl phosphonium chloride) into deionized water, and uniformly stirring to ensure that the molar concentration of the quaternary phosphonium salt monomer is 1.0mol/L, which is defined as a solution A;
(2) adding an ammonium thiosulfate initiator into the solution A to ensure that the molar concentration of the ammonium thiosulfate initiator is 0.05mol/L, and defining the solution A as a solution B;
(3) placing the solution B into the solution B with an area of 100cm 2 PP nonwoven material (gram weight 100 g/m) 2 ) Uniformly stirring to ensure that the mass ratio of the non-woven fabric to the solution B is 1:100 and defining the mixture as a mixture C;
(4) filling nitrogen into the mixture C, bubbling for 10min, exhausting air, sealing, and performing oxidation-reduction grafting reaction in a constant-temperature water bath at the reaction temperature of 30 ℃ for 120 min;
(5) the grafted non-woven fabric is washed by acetone, then extracted for 10 hours and dried.
The results of the tests carried out on the nonwoven materials obtained in steps (1) to (5) are as follows: the air permeability of the non-woven fabric material before surface grafting treatment is 3000mm/s, and the PM2.5 filtration efficiency is 92%; after the surface grafting treatment, the air permeability of the non-woven material is 2859mm/s, and the PM2.5 filtration efficiency is 92%. The change in air permeability and filtration efficiency was used to determine that the nonwoven fabric had not degraded filtration performance. In addition, the non-woven fabric material for in-vehicle air purification has good antibacterial and mildewproof effects, and is prepared according to GB/T20944.1-2007 evaluation part 1 of antibacterial properties of textiles: the evaluation results of the agar plate diffusion method are good, which shows that the antibacterial effect is achieved; the test is carried out according to the GB/T24346-one 2009 evaluation of the mildew-proof performance of the textile, the mildew-proof grade is 0 grade, and the good mildew-proof effect is shown. The EDS elemental profile of the nonwoven material produced is shown in fig. 2.
Comparative example 1
A comparative experiment was carried out with respect to example 1 using the other type of quaternary phosphonium salt monomer acryloyloxycetanyl-trimethyl phosphonium chloride, comprising the following steps:
(1) adding a quaternary phosphonium salt monomer material (acryloyl hexadecyl-trimethyl phosphine chloride) into deionized water, and uniformly stirring to ensure that the molar concentration of the quaternary phosphonium salt monomer is 0.5mol/L, which is defined as a solution A;
(2) adding a cerium ammonium nitrate initiator into the solution A to ensure that the molar concentration of the cerium ammonium nitrate initiator is 0.02mol/L, and defining the solution A as a solution B;
(3) placing the solution B into the solution B with an area of 100cm 2 PP non-woven material (gram weight 120 g/m) 2 ) Uniformly stirring to ensure that the mass ratio of the non-woven fabric to the solution B is 1:20, and defining the mixture as a mixture C;
(4) introducing nitrogen into the mixture C, bubbling for 10min, exhausting air, sealing, and carrying out oxidation-reduction grafting reaction in a constant-temperature water bath at the reaction temperature of 60 ℃ for 60 min;
(5) the grafted non-woven fabric is washed by acetone, then extracted for 10 hours and dried.
The results of the tests carried out on the nonwoven materials obtained in steps (1) to (5) are as follows: the air permeability of the non-woven fabric material of the comparative example before surface grafting treatment is 3000mm/s, and the PM2.5 filtration efficiency is 80%; after the surface grafting treatment, the air permeability of the non-woven fabric material is 2860mm/s, and the PM2.5 filtration efficiency is 80%. The change in air permeability and filtration efficiency was used to determine that the nonwoven fabric had not degraded filtration performance. The grafted non-woven fabric material obtained by the process has good antibacterial and mildewproof effects, and is prepared according to GB/T20944.1-2007 evaluation part 1 of antibacterial performance of textiles: when the evaluation results of escherichia coli and staphylococcus aureus are better when the standard of agar plate diffusion method is tested, the antibacterial effect is shown, but the antibacterial effect is reduced compared with that of the example 1; the test is carried out according to the GB/T24346-one 2009 evaluation of the mildew-proof performance of the textile, the mildew-proof grade is grade 1, which shows that the mildew-proof effect is better, but the effect is reduced compared with the embodiment 1. In addition, the grafted nonwoven material obtained by this process has a greatly increased toxicity compared to the grafted nonwoven material obtained in example 1, and is not suitable for use in grafted nonwoven materials.
Comparative example 2
A comparative experiment was carried out with respect to example 1, using other temperature conditions, comprising the following steps:
(1) adding a quaternary phosphonium salt monomer material (methacryloyloxyheptyl-tributyl phosphonium chloride) into deionized water, and uniformly stirring to ensure that the molar concentration of the quaternary phosphonium salt monomer is 0.5mol/L, which is defined as a solution A;
(2) adding a cerium ammonium nitrate initiator into the solution A to ensure that the molar concentration of the cerium ammonium nitrate initiator is 0.02mol/L, and defining the solution A as a solution B;
(3) placing the solution B into the solution B with an area of 100cm 2 PP non-woven material (gram weight 120 g/m) 2 ) Uniformly stirring to ensure that the mass ratio of the non-woven fabric to the solution B is 1:20, and defining the mixture as a mixture C;
(4) introducing nitrogen into the mixture C, bubbling for 10min, exhausting air, sealing, and carrying out oxidation-reduction grafting reaction in a constant-temperature water bath at the reaction temperature of 90 ℃ for 60 min;
(5) the grafted non-woven fabric is washed by acetone, then extracted for 10 hours and dried.
The results of the tests carried out on the nonwoven materials obtained in steps (1) to (5) are as follows: the air permeability of the non-woven fabric material of the comparative example before surface grafting treatment is 3000mm/s, and the PM2.5 filtration efficiency is 80 percent; after the surface grafting treatment, the air permeability of the nonwoven material was 2657mm/s, and the PM2.5 filtration efficiency was 78%. From the change in air permeability and filtration efficiency, it was judged that the filtration performance of the nonwoven fabric was slightly lowered. The grafted activated carbon material obtained by the process has good antibacterial and mildewproof effects, and is prepared according to GB/T20944.1-2007 evaluation part 1 of antibacterial properties of textiles: the evaluation results of Escherichia coli and Staphylococcus aureus are good when tested according to the standard of agar plate diffusion method, which shows that the antibacterial effect is achieved, but the effect is reduced compared with that of example 1; the test is carried out according to the GB/T24346-one 2009 evaluation on the mildew resistance of textiles, the mildew resistance grade is grade 1, which shows that the mildew resistance effect is better, but the effect is reduced compared with the example 1.
In the description herein, references to the description of the term "one embodiment," "some embodiments," "an example," "a specific example," or "some examples," etc., mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above are not necessarily intended to refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples. Furthermore, various embodiments or examples and features of different embodiments or examples described in this specification can be combined and combined by one skilled in the art without contradiction.
Although embodiments of the present invention have been shown and described above, it is understood that the above embodiments are exemplary and should not be construed as limiting the present invention, and that variations, modifications, substitutions and alterations can be made to the above embodiments by those of ordinary skill in the art within the scope of the present invention.
Claims (6)
1. A method of making a nonwoven material, comprising:
(1) adding a quaternary phosphonium salt monomer into deionized water, and uniformly stirring to ensure that the molar concentration of the quaternary phosphonium salt monomer is 0.5-1.0 mol/L so as to obtain a solution A; the quaternary phosphonium salt monomer is methacryloyloxyheptyl-tributylphosphine chloride;
(2) adding an initiator into the solution A to ensure that the molar concentration of the initiator is 0.02-0.05 mol/L so as to obtain a solution B;
(3) adding a non-woven fabric into the solution B, and uniformly stirring to ensure that the mass ratio of the non-woven fabric to the solution B is 1: 20-1: 100 so as to obtain a mixture C;
(4) filling nitrogen into the mixture C, bubbling for 10min, sealing, and carrying out redox grafting reaction in a constant-temperature water bath; the reaction temperature of the oxidation-reduction grafting reaction is 30-60 ℃; and
(5) and washing the product after the oxidation-reduction grafting reaction with acetone, extracting for 24 hours, and drying to obtain the non-woven fabric material.
2. The method of claim 1, wherein the initiator is cerium ammonium nitrate, cerium ammonium sulfate, or ammonium thiosulfate.
3. The method according to claim 1 or 2, wherein the non-woven fabric is a polypropylene filter cloth or a polyethylene terephthalate filter cloth.
4. The method according to claim 3, wherein the reaction time of the redox grafting reaction is 60 to 120 min.
5. A nonwoven material made by the method of any of claims 1-4, comprising: the non-woven fabric comprises a non-woven fabric substrate and a quaternary phosphonium salt monomer layer, wherein the quaternary phosphonium salt monomer layer is formed on the surface of the non-woven fabric substrate through oxidation-reduction grafting reaction.
6. Use of the nonwoven fabric material according to claim 5 in a filter, which is a filter for an air conditioner for a vehicle or a filter for a fuel cell.
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| CN103289015A (en) * | 2012-02-26 | 2013-09-11 | 河南工业大学 | Method for preparing quaternary phosphonium salt type cationic starch |
| KR101330571B1 (en) * | 2012-06-12 | 2013-11-19 | (주) 시온텍 | Manufacturing method of hybride ion exchange membrane |
| CN110938992A (en) * | 2019-11-04 | 2020-03-31 | 仪征金泰化纤无纺布有限公司 | Antibacterial non-woven fabric and preparation method thereof |
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| CN1400355A (en) * | 2002-09-20 | 2003-03-05 | 清华大学 | Preparation method of macromolecular sterilization fibre with grafted antibacterial monomer on its surface |
| CN103289015A (en) * | 2012-02-26 | 2013-09-11 | 河南工业大学 | Method for preparing quaternary phosphonium salt type cationic starch |
| KR101330571B1 (en) * | 2012-06-12 | 2013-11-19 | (주) 시온텍 | Manufacturing method of hybride ion exchange membrane |
| CN110938992A (en) * | 2019-11-04 | 2020-03-31 | 仪征金泰化纤无纺布有限公司 | Antibacterial non-woven fabric and preparation method thereof |
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