CN111501136A - Preparation method of ozone catalytic nanofiber - Google Patents
Preparation method of ozone catalytic nanofiber Download PDFInfo
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- CN111501136A CN111501136A CN201910089418.7A CN201910089418A CN111501136A CN 111501136 A CN111501136 A CN 111501136A CN 201910089418 A CN201910089418 A CN 201910089418A CN 111501136 A CN111501136 A CN 111501136A
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- 239000002121 nanofiber Substances 0.000 title claims abstract description 42
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 title claims abstract description 26
- 238000002360 preparation method Methods 0.000 title claims abstract description 25
- 230000003197 catalytic effect Effects 0.000 title claims abstract description 13
- 239000000243 solution Substances 0.000 claims abstract description 64
- 229920000642 polymer Polymers 0.000 claims abstract description 28
- 239000002131 composite material Substances 0.000 claims abstract description 26
- 239000000835 fiber Substances 0.000 claims abstract description 24
- 239000003054 catalyst Substances 0.000 claims abstract description 22
- 238000010041 electrostatic spinning Methods 0.000 claims abstract description 19
- 238000003756 stirring Methods 0.000 claims abstract description 15
- 239000002904 solvent Substances 0.000 claims abstract description 13
- 150000002696 manganese Chemical class 0.000 claims abstract description 11
- 238000001354 calcination Methods 0.000 claims abstract description 9
- 229910052751 metal Inorganic materials 0.000 claims abstract description 8
- 239000002184 metal Substances 0.000 claims abstract description 8
- 238000002156 mixing Methods 0.000 claims abstract description 8
- 150000003839 salts Chemical class 0.000 claims abstract description 8
- 238000001035 drying Methods 0.000 claims abstract description 7
- 238000006555 catalytic reaction Methods 0.000 claims abstract description 5
- 238000010438 heat treatment Methods 0.000 claims abstract description 3
- 239000012266 salt solution Substances 0.000 claims abstract description 3
- 229910052723 transition metal Inorganic materials 0.000 claims abstract description 3
- -1 transition metal salt Chemical class 0.000 claims abstract description 3
- 238000009987 spinning Methods 0.000 claims description 16
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 12
- 229920002239 polyacrylonitrile Polymers 0.000 claims description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- 238000002347 injection Methods 0.000 claims description 8
- 239000007924 injection Substances 0.000 claims description 8
- VCJMYUPGQJHHFU-UHFFFAOYSA-N iron(3+);trinitrate Chemical compound [Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VCJMYUPGQJHHFU-UHFFFAOYSA-N 0.000 claims description 8
- 229910052782 aluminium Inorganic materials 0.000 claims description 6
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 6
- 239000011888 foil Substances 0.000 claims description 6
- 238000000034 method Methods 0.000 claims description 6
- 229910001961 silver nitrate Inorganic materials 0.000 claims description 6
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 5
- MIVBAHRSNUNMPP-UHFFFAOYSA-N manganese(2+);dinitrate Chemical compound [Mn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O MIVBAHRSNUNMPP-UHFFFAOYSA-N 0.000 claims description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 4
- 229910021380 Manganese Chloride Inorganic materials 0.000 claims description 4
- GLFNIEUTAYBVOC-UHFFFAOYSA-L Manganese chloride Chemical compound Cl[Mn]Cl GLFNIEUTAYBVOC-UHFFFAOYSA-L 0.000 claims description 4
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims description 4
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 4
- UFMZWBIQTDUYBN-UHFFFAOYSA-N cobalt dinitrate Chemical compound [Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O UFMZWBIQTDUYBN-UHFFFAOYSA-N 0.000 claims description 4
- 229910001981 cobalt nitrate Inorganic materials 0.000 claims description 4
- 235000002867 manganese chloride Nutrition 0.000 claims description 4
- 239000011565 manganese chloride Substances 0.000 claims description 4
- 229940099607 manganese chloride Drugs 0.000 claims description 4
- 229940099596 manganese sulfate Drugs 0.000 claims description 4
- 235000007079 manganese sulphate Nutrition 0.000 claims description 4
- 239000011702 manganese sulphate Substances 0.000 claims description 4
- SQQMAOCOWKFBNP-UHFFFAOYSA-L manganese(II) sulfate Chemical compound [Mn+2].[O-]S([O-])(=O)=O SQQMAOCOWKFBNP-UHFFFAOYSA-L 0.000 claims description 4
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 4
- 229940071125 manganese acetate Drugs 0.000 claims description 3
- UOGMEBQRZBEZQT-UHFFFAOYSA-L manganese(2+);diacetate Chemical compound [Mn+2].CC([O-])=O.CC([O-])=O UOGMEBQRZBEZQT-UHFFFAOYSA-L 0.000 claims description 3
- 229920001661 Chitosan Polymers 0.000 claims description 2
- FXHOOIRPVKKKFG-UHFFFAOYSA-N N,N-Dimethylacetamide Chemical compound CN(C)C(C)=O FXHOOIRPVKKKFG-UHFFFAOYSA-N 0.000 claims description 2
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 claims description 2
- 229940011182 cobalt acetate Drugs 0.000 claims description 2
- QAHREYKOYSIQPH-UHFFFAOYSA-L cobalt(II) acetate Chemical compound [Co+2].CC([O-])=O.CC([O-])=O QAHREYKOYSIQPH-UHFFFAOYSA-L 0.000 claims description 2
- XTVVROIMIGLXTD-UHFFFAOYSA-N copper(II) nitrate Chemical compound [Cu+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XTVVROIMIGLXTD-UHFFFAOYSA-N 0.000 claims description 2
- OPQARKPSCNTWTJ-UHFFFAOYSA-L copper(ii) acetate Chemical compound [Cu+2].CC([O-])=O.CC([O-])=O OPQARKPSCNTWTJ-UHFFFAOYSA-L 0.000 claims description 2
- PVFSDGKDKFSOTB-UHFFFAOYSA-K iron(3+);triacetate Chemical compound [Fe+3].CC([O-])=O.CC([O-])=O.CC([O-])=O PVFSDGKDKFSOTB-UHFFFAOYSA-K 0.000 claims description 2
- 235000006748 manganese carbonate Nutrition 0.000 claims description 2
- 239000011656 manganese carbonate Substances 0.000 claims description 2
- 229940093474 manganese carbonate Drugs 0.000 claims description 2
- 229910000016 manganese(II) carbonate Inorganic materials 0.000 claims description 2
- XMWCXZJXESXBBY-UHFFFAOYSA-L manganese(ii) carbonate Chemical compound [Mn+2].[O-]C([O-])=O XMWCXZJXESXBBY-UHFFFAOYSA-L 0.000 claims description 2
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 2
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 2
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 2
- CQLFBEKRDQMJLZ-UHFFFAOYSA-M silver acetate Chemical compound [Ag+].CC([O-])=O CQLFBEKRDQMJLZ-UHFFFAOYSA-M 0.000 claims description 2
- 229940071536 silver acetate Drugs 0.000 claims description 2
- NUJOXMJBOLGQSY-UHFFFAOYSA-N manganese dioxide Chemical compound O=[Mn]=O NUJOXMJBOLGQSY-UHFFFAOYSA-N 0.000 description 18
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 9
- 238000001914 filtration Methods 0.000 description 8
- 239000012528 membrane Substances 0.000 description 8
- 239000008367 deionised water Substances 0.000 description 6
- 229910021641 deionized water Inorganic materials 0.000 description 6
- 239000002245 particle Substances 0.000 description 6
- 238000000354 decomposition reaction Methods 0.000 description 5
- 238000011068 loading method Methods 0.000 description 4
- 238000011056 performance test Methods 0.000 description 4
- 229910016978 MnOx Inorganic materials 0.000 description 3
- 239000000443 aerosol Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- 238000003421 catalytic decomposition reaction Methods 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- UXGNZZKBCMGWAZ-UHFFFAOYSA-N dimethylformamide dmf Chemical compound CN(C)C=O.CN(C)C=O UXGNZZKBCMGWAZ-UHFFFAOYSA-N 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000006864 oxidative decomposition reaction Methods 0.000 description 2
- 229920002125 Sokalan® Polymers 0.000 description 1
- 238000004887 air purification Methods 0.000 description 1
- HPXRVTGHNJAIIH-UHFFFAOYSA-N cyclohexanol Chemical compound OC1CCCCC1 HPXRVTGHNJAIIH-UHFFFAOYSA-N 0.000 description 1
- 238000000635 electron micrograph Methods 0.000 description 1
- 238000003837 high-temperature calcination Methods 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000011572 manganese Substances 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000004584 polyacrylic acid Substances 0.000 description 1
- 239000012286 potassium permanganate Substances 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
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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
- D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
- D01F9/08—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
- D01F9/12—Carbon filaments; Apparatus specially adapted for the manufacture thereof
- D01F9/14—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments
- D01F9/20—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from polyaddition, polycondensation or polymerisation products
- D01F9/21—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from polyaddition, polycondensation or polymerisation products from 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
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/16—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/32—Manganese, technetium or rhenium
- B01J23/34—Manganese
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/50—Catalysts, in general, characterised by their form or physical properties characterised by their shape or configuration
- B01J35/58—Fabrics or filaments
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
- B01J37/082—Decomposition and pyrolysis
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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
- D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
- D01F9/08—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
- D01F9/12—Carbon filaments; Apparatus specially adapted for the manufacture thereof
- D01F9/14—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments
- D01F9/20—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from polyaddition, polycondensation or polymerisation products
- D01F9/21—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from polyaddition, polycondensation or polymerisation products from macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
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- D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
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- D01F9/12—Carbon filaments; Apparatus specially adapted for the manufacture thereof
- D01F9/14—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments
- D01F9/20—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from polyaddition, polycondensation or polymerisation products
- D01F9/24—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from polyaddition, polycondensation or polymerisation products from macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
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Abstract
The invention relates to a preparation method of ozone catalytic nanofiber, which is characterized by comprising the following steps: dissolving a polymer in a solvent, and stirring for 3-12 hours at the temperature of room temperature-80 ℃ to prepare a uniform and transparent polymer solution with the concentration of 5-20 wt%; dissolving manganese salt and transition metal salt in a solvent to prepare a catalyst solution with the manganese salt concentration of 2-20 wt% and the metal salt concentration of 0-1 wt%; mixing the polymer solution and the manganese salt solution, stirring for 5-12 h, and then standing or defoaming in vacuum to obtain a composite gel solution; putting the composite gel solution into electrostatic spinning equipment for electrostatic spinning to prepare a fiber web; drying the prepared fiber net at 50-120 ℃ for 5-12 h, and then raising the temperature to 300-1000 ℃ at a heating rate of 2-10 ℃/min and calcining for 3-10 h to obtain the nanofiber with the ozone catalysis function.
Description
Technical Field
The invention relates to the field of air purification, in particular to a preparation method of ozone catalytic nanofiber.
Background
CN201310309595.4 discloses an electrostatic spinning preparation method of manganese dioxide/polyacrylonitrile-based oxidative decomposition formaldehyde type nanofiber membrane, which comprises the following steps: (1) preparing nano manganese dioxide by using potassium permanganate and cyclohexanol through a hydrothermal method, wherein the diameter of the nano manganese dioxide is 50-600 nm; (2) mixing Polyacrylonitrile (PAN) and nano Manganese Dioxide (MD), dissolving in N-N Dimethylformamide (DMF), and stirring to obtain uniformly dispersed electrostatic spinning solution; wherein the mass ratio of MD to PAN is 0.01-0.5: 1; (3) and (3) performing electrostatic spinning by using the prepared electrostatic spinning solution to obtain the manganese dioxide/polyacrylonitrile (MD/PAN) based formaldehyde oxidative decomposition type nanofiber membrane. The nanofiber membrane has the function of oxidizing and decomposing formaldehyde.
However, in the nanofiber membrane, the nano manganese dioxide is directly added into the spinning solution, so that the spinnability of the original spinning solution is reduced, and a part of Mn ions are wrapped in the inside of the fiber, so that the effective utilization rate is reduced.
Disclosure of Invention
The invention aims to solve the technical problem of providing a preparation method of ozone catalytic nanofiber, which has high effective utilization rate and can remove particles and decompose ozone, aiming at the current situation of the prior art.
The technical scheme adopted by the invention for solving the technical problems is as follows: the preparation method of the ozone catalytic nanofiber is characterized by comprising the following steps of:
1) preparing a polymer solution
Dissolving a polymer in a solvent, and stirring for 3-12 hours at the temperature of room temperature-80 ℃ to prepare a uniform and transparent polymer solution with the concentration of 5-20 wt%;
the polymer is selected from at least one of polyvinylpyrrolidone, polyvinyl alcohol, polyacrylonitrile, polyethylene oxide and chitosan;
the solvent is at least one selected from water, ethanol, N-dimethylformamide, N-dimethylacetamide and N-methylpyrrolidone;
2) preparation of catalyst solution
Dissolving manganese salt and transition metal salt in a solvent to prepare a catalyst solution with the manganese salt concentration of 2-20 wt% and the metal salt concentration of 0-1 wt%;
the manganese salt is selected from at least one of manganese nitrate, manganese acetate, manganese sulfate, manganese chloride and manganese carbonate;
the metal salt is selected from at least one of copper nitrate, silver nitrate, cobalt nitrate, ferric nitrate, copper acetate, silver acetate, cobalt acetate and ferric acetate;
the solvent is the same as the solvent used for the polymer solution;
3) mixing the polymer solution and the manganese salt solution, stirring for 5-12 h, and then standing or defoaming in vacuum to obtain a composite gel solution;
4) nanofiber preparation
Putting the composite gel solution into electrostatic spinning equipment for electrostatic spinning to prepare a fiber web;
5) post-treatment
Drying the prepared fiber net at 50-120 ℃ for 5-12 h, and then raising the temperature to 300-1000 ℃ at a heating rate of 2-10 ℃/min and calcining for 3-10 h to obtain the nanofiber with the ozone catalysis function.
Preferably, the concentration of the metal salt in the catalyst solution is 0.05-1 wt%. The metal salt plays a role in promoting catalysis, so that the ozone decomposition effect can be greatly improved, and the moisture resistance of the fiber can be provided; can keep the ozone decomposition function in a humid environment.
Further, when the electrostatic spinning is carried out, the flow speed of an injection pump in the electrostatic spinning equipment is controlled to be 3-200 mu L/min, the distance between a needle and a collector is 5-25 cm, the voltage is 8-30 KV, the preferred voltage is 15-25 KV, the rotating speed of the collector is 300-3000rpm, the spinning temperature is 20-30 ℃, the humidity is 40-70%, and a compact fiber net is collected on an aluminum foil.
Preferably, the flow rate of the injection pump is 5-20 mu L/min, and the voltage is 15-25 KV.
Preferably, the diameter of the nanofiber obtained after calcination is 50-500 nm.
Compared with the prior art, the preparation method has the advantages that after the high molecular polymer and the catalytic precursor solution are blended, the composite nanofiber is directly prepared by an electrostatic spinning method, high molecular components in the fiber are burnt by a high-temperature calcination method, so that MnOx forms a nanofiber shape at high temperature, and the MnOx is made into a nanofiber-shaped material and used as an active catalyst for ozone decomposition to improve the specific surface area and the reaction contact point of the MnOx catalyst, so that the reaction activity and the effective utilization rate of the catalyst are improved; and the fiber is made into a net shape and also has the function of particle filtration.
Drawings
FIG. 1 is an electron micrograph of a nanofiber web prepared in step 4 of example 1 of the present invention;
FIG. 2 is an SEM photograph of calcined nanofibers obtained in step 5 of example 1 of the present invention;
fig. 3 is a partially enlarged view of fig. 2.
Detailed Description
The present invention will be described in further detail with reference to examples.
Example 1
(1) Preparation of Polymer solutions
Dissolving 15g of polyvinyl alcohol (PVA) in 75g of deionized water, stirring for 3h at the water bath temperature of 60 ℃ and the rotating speed of 500rpm to prepare a uniform and transparent polymer solution;
(2) preparation of catalyst solution
Adding manganese nitrate and silver nitrate into deionized water to prepare a catalyst solution with the concentration of 10m L manganese nitrate being 5 wt% and the concentration of silver nitrate being 1 wt%;
(3) preparing composite gel solution
Adding the catalyst solution into a polymer solution, mixing, stirring for 5 hours, standing and defoaming to obtain a composite gel solution;
(4) nanofiber preparation
And (3) loading the composite gel solution into electrostatic spinning equipment, adjusting the flow rate of an injection pump to be 10 mu L/min, adjusting the distance between a needle and a collector to be 15cm, applying a voltage of 15KV, setting the rotating speed of the collector to be 500rpm, setting the spinning temperature to be 25 ℃ and the spinning humidity to be 50%, and collecting and spinning on an aluminum foil to obtain a dense fiber web.
(5) Nanofiber post-treatment
Drying the fiber net at 60 ℃ for 5h, then raising the temperature to 400 ℃ at the speed of 5 ℃/min, calcining at 400 ℃ and keeping the temperature for 3 hours to obtain the composite nanofiber membrane with the fiber diameter of 500 nm.
And carrying out performance test on the prepared composite nanofiber.
Firstly, ozone catalytic performance, wherein the size of a sample is 15cm × 15cm, the sample is placed into a testing device, and the space velocity is adjusted to 150000h-1The ozone inlet gas concentration is c0Was 10 ppm. Detecting the concentration c of ozone at the outlet of the pipeline by adopting a Model 202 Serial ozone analyzer, detecting the stable concentration of the outlet, and calculating the ozone removal rate according to the following formula:
secondly, the filtering performance of the particulate matters is as follows:
the filtering performance of the composite nanofiber membrane is tested by adopting a TSI 8130 type automatic filter material tester, the sample size is 15cm × 15cm, NaCl aerosol with the mass median diameter of particle particles of 0.26um is generated, and the air flow speed is 32L/min.
The filtering efficiency η of the particles is obtained by testing the concentration of the particles at two ends of the membrane
C1 is outlet aerosol concentration and C2 is inlet aerosol concentration.
And (3) testing results:
space velocity of 150000h-1When the inlet concentration is 10ppm, the catalytic ozone decomposition efficiency of the sample is 84 percent, and the filtering performance of PM0.3 is 91 percent.
Example 2:
(1) preparation of Polymer solutions
Dissolving 12g of polyacrylonitrile in 78g of N, N-dimethylformamide DMF solvent, stirring for 3h at 40 ℃ and the rotating speed of 500rpm to prepare uniform and transparent polymer solution;
(2) preparation of catalyst solution
Adding manganese acetate and silver nitrate into N, N-dimethylformamide DMF to prepare a catalyst solution with the concentration of 10m L manganese nitrate of 5 wt% and the concentration of silver nitrate of 0.2 wt%;
(3) preparing composite gel solution
Adding the catalyst solution into a polymer solution, mixing, stirring for 5 hours, standing and defoaming to obtain a composite gel solution;
(4) nanofiber preparation
And (3) loading the composite gel solution into electrostatic spinning equipment, adjusting the flow rate of an injection pump to be 10 mu L/min, adjusting the distance between a needle and a collector to be 15cm, applying a voltage of 18KV, setting the rotating speed of the collector to be 500rpm, setting the spinning temperature to be 25 ℃ and the spinning humidity to be 50%, and collecting and spinning on an aluminum foil to obtain a dense fiber web.
(5) Nanofiber post-treatment
Drying the fiber net at 60 ℃ for 5h, then raising the temperature to 600 ℃ at the speed of 5 ℃/min, calcining at 600 ℃ and keeping the temperature for 3 hours to obtain the composite nanofiber membrane with the fiber diameter of 200 nm.
And carrying out performance test on the prepared composite nanofiber.
Space velocity of 150000h-1When the inlet concentration is 10ppm,the catalytic ozone decomposition efficiency of the sample is 87%, and the filtering performance of PM0.3 is 93%.
Example 3:
(1) preparation of Polymer solutions
Dissolving 20g of polyethylene oxide (PEO) in 70g of deionized water, stirring for 2h at the temperature of 60 ℃ and the rotating speed of 300rpm, and preparing a uniform and transparent polymer solution;
(2) preparation of catalyst solution
Manganese sulfate and cobalt nitrate are added into deionized water to prepare a catalyst solution with the concentration of 10 wt% of manganese sulfate and 0.5 wt% of cobalt nitrate being 10m L;
(3) preparing composite gel solution
Adding the catalyst solution into a polymer solution, mixing, stirring for 5 hours, standing and defoaming to obtain a composite gel solution;
(4) nanofiber preparation
And (3) loading the composite gel solution into electrostatic spinning equipment, adjusting the flow rate of an injection pump to be 50 mu L/min, adjusting the distance between a needle and a collector to be 15cm, applying a voltage of 20KV, controlling the rotating speed of the collector to be 500rpm, controlling the spinning temperature to be 25 ℃ and the spinning humidity to be 50%, and collecting and spinning on an aluminum foil to obtain a dense fiber web.
(5) Nanofiber post-treatment
Drying the fiber web at 60 ℃ for 5h, then raising the temperature to 750 ℃ at the speed of 8 ℃/min, calcining at 750 ℃ and keeping the temperature for 3 hours to obtain the nanofiber with the fiber diameter of 90 nm.
And carrying out performance test on the prepared composite nanofiber.
Space velocity of 150000h-1When the inlet concentration is 10ppm, the catalytic decomposition efficiency of ozone of the sample is 90 percent, and the filtering performance of PM0.3 is 95 percent.
Example 4:
(1) preparation of Polymer solutions
Dissolving 20g of polyacrylic acid in 70g of deionized water, stirring for 4h at 80 ℃ and the rotating speed of 500rpm, and preparing a uniform and transparent polymer solution;
(2) preparation of catalyst solution
Adding manganese chloride and ferric nitrate into deionized water to prepare a catalyst solution with the concentration of 10m L manganese chloride being 20 wt% and the concentration of ferric nitrate being 0.6 wt%;
(3) preparing composite gel solution
Adding the catalyst solution into a polymer solution, mixing, stirring for 6 hours, standing and defoaming to obtain a composite gel solution;
(4) nanofiber preparation
And (3) loading the composite gel solution into electrostatic spinning equipment, adjusting the flow rate of an injection pump to be 100 mu L/min, adjusting the distance between a needle and a collector to be 20cm, applying a voltage of 20KV, controlling the rotating speed of the collector to be 500rpm, controlling the spinning temperature to be 25 ℃ and the spinning humidity to be 50%, and collecting and spinning on an aluminum foil to obtain a dense fiber web.
(5) Nanofiber post-treatment
Drying the fiber web at 60 ℃ for 5h, then raising the temperature to 750 ℃ at the speed of 10 ℃/min, calcining at 750 ℃ and keeping the temperature for 3 hours to obtain the nanofiber with the fiber diameter of 100 nm.
And carrying out performance test on the prepared composite nanofiber.
Space velocity of 150000h-1When the inlet concentration is 10ppm, the catalytic decomposition efficiency of ozone of the sample is 92 percent, and the filtering performance of PM0.3 is 95.3 percent.
Claims (5)
1. The preparation method of the ozone catalytic nanofiber is characterized by comprising the following steps of:
1) preparing a polymer solution
Dissolving a polymer in a solvent, and stirring for 3-12 hours at the temperature of room temperature-80 ℃ to prepare a uniform and transparent polymer solution with the concentration of 5-20 wt%;
the polymer is selected from at least one of polyvinylpyrrolidone, polyvinyl alcohol, polyacrylonitrile, polyethylene oxide and chitosan;
the solvent is at least one selected from water, ethanol, N-dimethylformamide, N-dimethylacetamide and N-methylpyrrolidone;
2) preparation of catalyst solution
Dissolving manganese salt and transition metal salt in a solvent to prepare a catalyst solution with the manganese salt concentration of 2-20 wt% and the metal salt concentration of 0-1 wt%;
the manganese salt is selected from at least one of manganese nitrate, manganese acetate, manganese sulfate, manganese chloride and manganese carbonate;
the metal salt is selected from at least one of copper nitrate, silver nitrate, cobalt nitrate, ferric nitrate, copper acetate, silver acetate, cobalt acetate and ferric acetate;
the solvent is the same as the solvent used for the polymer solution;
3) mixing the polymer solution and the manganese salt solution, stirring for 5-12 h, and then standing or defoaming in vacuum to obtain a composite gel solution;
4) nanofiber preparation
Putting the composite gel solution into electrostatic spinning equipment for electrostatic spinning to prepare a fiber web;
5) post-treatment
Drying the prepared fiber net at 50-120 ℃ for 5-12 h, and then raising the temperature to 300-1000 ℃ at a heating rate of 2-10 ℃/min and calcining for 3-10 h to obtain the nanofiber with the ozone catalysis function.
2. The method of claim 1, wherein the concentration of the metal salt in the catalyst solution is 0.05-1 wt%.
3. The method for preparing the ozone catalysis nanofiber as claimed in claim 1 or 2, wherein during the electrostatic spinning, the flow rate of an injection pump in the electrostatic spinning device is controlled to be 3-200 μ L/min, the distance between a needle and a collector is controlled to be 5-25 cm, the voltage is 8-30 KV, preferably 15-25 KV, the rotating speed of the collector is 300-3000rpm, the spinning temperature is 20-30 ℃, the humidity is 40-70%, and a dense fiber web is collected on an aluminum foil.
4. The method for preparing the ozone catalytic nanofiber according to claim 3, wherein the flow rate of the injection pump is 5-20 μ L/min, and the voltage is 15-25 KV.
5. The method for preparing the ozone catalytic nanofiber as claimed in claim 4, wherein the diameter of the nanofiber obtained after calcination is 50-500 nm.
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| CN115672349A (en) * | 2022-11-09 | 2023-02-03 | 沈阳师范大学 | Metal oxide catalyst with hollow nanotube structure and preparation method and application thereof |
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