CN111495348A - Preparation method of porous photocatalyst filter screen - Google Patents
Preparation method of porous photocatalyst filter screen Download PDFInfo
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- CN111495348A CN111495348A CN202010325046.6A CN202010325046A CN111495348A CN 111495348 A CN111495348 A CN 111495348A CN 202010325046 A CN202010325046 A CN 202010325046A CN 111495348 A CN111495348 A CN 111495348A
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- 239000011941 photocatalyst Substances 0.000 title claims abstract description 49
- 238000002360 preparation method Methods 0.000 title claims abstract description 32
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 86
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 85
- 239000010936 titanium Substances 0.000 claims abstract description 85
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 71
- 239000004408 titanium dioxide Substances 0.000 claims abstract description 34
- 239000002071 nanotube Substances 0.000 claims abstract description 23
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 16
- 238000000137 annealing Methods 0.000 claims abstract description 8
- 238000004140 cleaning Methods 0.000 claims abstract description 8
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 8
- 238000010438 heat treatment Methods 0.000 claims description 42
- 239000000843 powder Substances 0.000 claims description 40
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 33
- 238000000034 method Methods 0.000 claims description 29
- 229910001069 Ti alloy Inorganic materials 0.000 claims description 12
- 239000003792 electrolyte Substances 0.000 claims description 12
- 230000003647 oxidation Effects 0.000 claims description 12
- 238000007254 oxidation reaction Methods 0.000 claims description 12
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 10
- 239000012298 atmosphere Substances 0.000 claims description 10
- 239000012153 distilled water Substances 0.000 claims description 10
- 238000001035 drying Methods 0.000 claims description 10
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 10
- 239000003795 chemical substances by application Substances 0.000 claims description 9
- 238000003825 pressing Methods 0.000 claims description 9
- 238000010146 3D printing Methods 0.000 claims description 8
- 238000001816 cooling Methods 0.000 claims description 8
- 230000005672 electromagnetic field Effects 0.000 claims description 8
- LYCAIKOWRPUZTN-UHFFFAOYSA-N ethylene glycol Natural products OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 8
- 238000005238 degreasing Methods 0.000 claims description 7
- 239000002002 slurry Substances 0.000 claims description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 claims description 5
- 239000011737 fluorine Substances 0.000 claims description 5
- 229910052731 fluorine Inorganic materials 0.000 claims description 5
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 5
- 229910052697 platinum Inorganic materials 0.000 claims description 5
- 238000004321 preservation Methods 0.000 claims description 5
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims description 5
- 229910010271 silicon carbide Inorganic materials 0.000 claims description 5
- 239000002904 solvent Substances 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 4
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical group [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 4
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 4
- 239000004202 carbamide Substances 0.000 claims description 4
- 238000009694 cold isostatic pressing Methods 0.000 claims description 4
- 229910002804 graphite Inorganic materials 0.000 claims description 4
- 239000010439 graphite Substances 0.000 claims description 4
- 239000011261 inert gas Substances 0.000 claims description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M sodium hydroxide Inorganic materials [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 4
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 2
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 2
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims description 2
- 229910052581 Si3N4 Inorganic materials 0.000 claims description 2
- 229920002472 Starch Polymers 0.000 claims description 2
- 229910000831 Steel Inorganic materials 0.000 claims description 2
- CZMRCDWAGMRECN-UGDNZRGBSA-N Sucrose Chemical compound O[C@H]1[C@H](O)[C@@H](CO)O[C@@]1(CO)O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 CZMRCDWAGMRECN-UGDNZRGBSA-N 0.000 claims description 2
- 229930006000 Sucrose Natural products 0.000 claims description 2
- 239000000853 adhesive Substances 0.000 claims description 2
- 230000001070 adhesive effect Effects 0.000 claims description 2
- 239000002518 antifoaming agent Substances 0.000 claims description 2
- 229910052786 argon Inorganic materials 0.000 claims description 2
- 239000011230 binding agent Substances 0.000 claims description 2
- 238000005097 cold rolling Methods 0.000 claims description 2
- 229910052802 copper Inorganic materials 0.000 claims description 2
- 239000010949 copper Substances 0.000 claims description 2
- 238000007598 dipping method Methods 0.000 claims description 2
- 239000002270 dispersing agent Substances 0.000 claims description 2
- 125000003827 glycol group Chemical group 0.000 claims description 2
- 239000001307 helium Substances 0.000 claims description 2
- 229910052734 helium Inorganic materials 0.000 claims description 2
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 2
- 230000006698 induction Effects 0.000 claims description 2
- 238000001746 injection moulding Methods 0.000 claims description 2
- 229910052749 magnesium Inorganic materials 0.000 claims description 2
- 239000011777 magnesium Substances 0.000 claims description 2
- 229910052750 molybdenum Inorganic materials 0.000 claims description 2
- 239000011733 molybdenum Substances 0.000 claims description 2
- 229910017604 nitric acid Inorganic materials 0.000 claims description 2
- 239000003960 organic solvent Substances 0.000 claims description 2
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 2
- 230000001681 protective effect Effects 0.000 claims description 2
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 claims description 2
- 239000011780 sodium chloride Substances 0.000 claims description 2
- 239000010935 stainless steel Substances 0.000 claims description 2
- 229910001220 stainless steel Inorganic materials 0.000 claims description 2
- 239000008107 starch Substances 0.000 claims description 2
- 235000019698 starch Nutrition 0.000 claims description 2
- 239000010959 steel Substances 0.000 claims description 2
- 238000003756 stirring Methods 0.000 claims description 2
- 239000005720 sucrose Substances 0.000 claims description 2
- 239000000375 suspending agent Substances 0.000 claims description 2
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims description 2
- 229910052721 tungsten Inorganic materials 0.000 claims description 2
- 239000010937 tungsten Substances 0.000 claims description 2
- 230000001699 photocatalysis Effects 0.000 abstract description 16
- 238000007743 anodising Methods 0.000 abstract description 7
- 238000007146 photocatalysis Methods 0.000 abstract description 7
- 239000000758 substrate Substances 0.000 abstract description 2
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 15
- 239000000463 material Substances 0.000 description 8
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 description 8
- 230000000694 effects Effects 0.000 description 7
- 238000005245 sintering Methods 0.000 description 7
- DDFHBQSCUXNBSA-UHFFFAOYSA-N 5-(5-carboxythiophen-2-yl)thiophene-2-carboxylic acid Chemical compound S1C(C(=O)O)=CC=C1C1=CC=C(C(O)=O)S1 DDFHBQSCUXNBSA-UHFFFAOYSA-N 0.000 description 6
- 238000000746 purification Methods 0.000 description 6
- STZCRXQWRGQSJD-GEEYTBSJSA-M methyl orange Chemical compound [Na+].C1=CC(N(C)C)=CC=C1\N=N\C1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-GEEYTBSJSA-M 0.000 description 5
- 229940012189 methyl orange Drugs 0.000 description 5
- 239000003344 environmental pollutant Substances 0.000 description 4
- 235000019441 ethanol Nutrition 0.000 description 4
- 231100000719 pollutant Toxicity 0.000 description 4
- 239000011148 porous material Substances 0.000 description 4
- 238000003980 solgel method Methods 0.000 description 4
- 241000894006 Bacteria Species 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- 239000011248 coating agent Substances 0.000 description 3
- 238000000576 coating method Methods 0.000 description 3
- 238000003912 environmental pollution Methods 0.000 description 3
- 239000000835 fiber Substances 0.000 description 3
- 238000005187 foaming Methods 0.000 description 3
- 239000011521 glass Substances 0.000 description 3
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical class C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 238000003786 synthesis reaction Methods 0.000 description 3
- 241000282414 Homo sapiens Species 0.000 description 2
- 229910052921 ammonium sulfate Inorganic materials 0.000 description 2
- 238000003491 array Methods 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 238000005266 casting Methods 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 2
- 230000000593 degrading effect Effects 0.000 description 2
- 238000010894 electron beam technology Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000005284 excitation Effects 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 238000009776 industrial production Methods 0.000 description 2
- 230000001678 irradiating effect Effects 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 2
- 229910052753 mercury Inorganic materials 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 239000012299 nitrogen atmosphere Substances 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 238000013032 photocatalytic reaction Methods 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- STZCRXQWRGQSJD-UHFFFAOYSA-M sodium;4-[[4-(dimethylamino)phenyl]diazenyl]benzenesulfonate Chemical compound [Na+].C1=CC(N(C)C)=CC=C1N=NC1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-UHFFFAOYSA-M 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 1
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 description 1
- 229910000013 Ammonium bicarbonate Inorganic materials 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 235000012538 ammonium bicarbonate Nutrition 0.000 description 1
- 239000001099 ammonium carbonate Substances 0.000 description 1
- LDDQLRUQCUTJBB-UHFFFAOYSA-N ammonium fluoride Chemical compound [NH4+].[F-] LDDQLRUQCUTJBB-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000000498 cooling water Substances 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000000499 gel Substances 0.000 description 1
- TUJKJAMUKRIRHC-UHFFFAOYSA-N hydroxyl Chemical compound [OH] TUJKJAMUKRIRHC-UHFFFAOYSA-N 0.000 description 1
- 239000007943 implant Substances 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 231100000053 low toxicity Toxicity 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000000399 orthopedic effect Effects 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 238000004663 powder metallurgy Methods 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 239000000741 silica gel Substances 0.000 description 1
- 229910002027 silica gel Inorganic materials 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- LLZRNZOLAXHGLL-UHFFFAOYSA-J titanic acid Chemical compound O[Ti](O)(O)O LLZRNZOLAXHGLL-UHFFFAOYSA-J 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 238000007740 vapor deposition Methods 0.000 description 1
Classifications
-
- 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
- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/06—Silicon, titanium, zirconium or hafnium; Oxides or hydroxides thereof
- B01J21/063—Titanium; Oxides or hydroxides thereof
-
- 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
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/24—Nitrogen compounds
-
- B01J35/39—
-
- B01J35/60—
Abstract
The invention belongs to the technical field of photocatalysis, and particularly relates to a preparation method of a porous photocatalyst filter screen. The technical scheme is as follows: a preparation method of a porous photocatalyst filter screen, wherein the porous photocatalyst filter screen is porous titanium loaded with titanium dioxide or a nitrogen-doped titanium dioxide nanotube array, and the preparation method specifically comprises the following steps: 1) cleaning the surface; 2) anodizing; 3) annealing treatment: obtaining porous titanium loaded with a titanium dioxide nanotube array; 4) nitrogen doping: and preparing the porous titanium loaded with the nitrogen-doped titanium dioxide nanotube array. According to the preparation method of the porous photocatalyst filter screen, the porous photocatalyst filter screen has a high surface area, has a strong photocatalytic effect under ultraviolet light or visible light conditions, and is high in bonding strength between the titanium dioxide nanotube and the substrate and not easy to fall off.
Description
Technical Field
The invention belongs to the technical field of photocatalysis, and particularly relates to a preparation method of a porous photocatalyst filter screen.
Background
In recent years, with the progress and industrial development of human society, environmental pollution is increasingly remarkable, especially chemical pollution becomes more common, which seriously threatens the environment which people do not live in, including water resources, soil and atmospheric environment, and how to effectively control and treat environmental pollution has become a great challenge for human beings. Since the 70 s in the 20 th century, semiconductor photocatalytic materials have wide application prospects in the aspect of treating environmental pollution, particularly organic pollution, due to the characteristics of simple preparation process, low energy consumption, no secondary pollution and the like. The photocatalysis uses visible light and ultraviolet light as light sources to irradiate the semiconductor photocatalysis material, induces electrons to be excited to a conduction band, generates corresponding holes, generates active oxygen and hydroxyl radical with extremely strong oxidation, can oxidize and decompose organic matters, pollutants, bacteria and the like, and realizes the purification effect on water and air. The nano titanium dioxide is regarded as a photocatalytic material with wide application prospect due to the advantages of high photocatalytic activity, low toxicity, low price, super-hydrophilicity and the like, and can be coated on the surfaces of materials such as glass, metal, ceramic, silica gel and the like.
At present, methods for preparing the nano titanium dioxide coating include a sol-gel method, a vapor deposition method, a powder sintering method and the like. The sol-gel method is the most common method for preparing the nano titanium dioxide coating because of simple process and low equipment cost. Patent No. CN1511630A discloses a preparation method of porous ceramic-supported high-activity nano titanium dioxide, wherein titanium dioxide sol prepared by a sol-gel method is mixed with titanium dioxide powder, and the nano titanium dioxide is coated on the surface of porous ceramic through high-temperature sintering. The patent number CN1943852A discloses an activated carbon fiber loaded titanium dioxide film photocatalyst and a preparation method and an application method thereof, wherein the activated carbon fiber is immersed into an absolute ethyl alcohol solution containing tetra-n-butyl titanate, taken out, heated to 180-700 ℃ in a high-purity nitrogen atmosphere, introduced with superheated steam, and calcined at 550-700 ℃ in the nitrogen atmosphere to prepare the activated carbon fiber loaded with the nano titanium dioxide film. The nano titanium dioxide coating prepared by the sol-gel method has low bonding strength with a matrix, is easy to fall off, and forms secondary pollution of titanium dioxide powder.
Among the currently used nano titanium dioxide photocatalytic materials, anatase titanium dioxide has the strongest photocatalytic effect, the forbidden bandwidth of which is 3.2Ev, and only under the excitation of ultraviolet rays with the wavelength λ of 387.5nm or less, electrons can be induced to be excited to a conduction band to generate corresponding holes, and the light source of the part only accounts for about 4% of the total amount of visible light.1986,123,126) first proposed using NH4Cl or NH4The nitrogen-doped titanium dioxide prepared from the mixture of OH and titanium hydroxide has a photocatalytic effect under the condition of visible light, but the process is complex and industrial production is not easy to realize.
Porous titanium has been used for orthopedic implant materials, battery electrode materials, sound absorption materials and sewage treatment materials due to its high surface area, low modulus, excellent corrosion resistance and excellent biocompatibility. At present, porous titanium is prepared by a powder metallurgy method, which comprises loose sintering, hollow sphere powder sintering, a pore-forming agent adding method, slurry foaming, gel casting, freeze casting, 3D printing, fiber sintering, dealloying, self-propagating high-temperature synthesis and other preparation methods. The preparation method of the porous titanium with high porosity and high porosity mainly comprises a pore-forming agent adding method, slurry foaming, 3D printing, fiber sintering, self-propagating high-temperature synthesis and the like. C.e.wen et al prepared porous titanium (j.mater.res.,2002,17,2633) with 80% porosity by adding a pore-forming agent using ammonium bicarbonate as a pore-forming agent. Patent nos. CN102747245A and CN104357700A disclose two methods for preparing porous titanium by adding pore-forming agent. Manonukul et al prepared 84% pore porosity porous titanium by slurry foaming (Powder technol.,2014,266,129). Parthasarathy et al prepared porous titanium with 70% pore gas content by 3D printing method (j. mech. behav. biomed. mater, 2010,3, 249). Patent No. CN103495731A discloses a method for 3D printing of pure titanium porous structure. C.m.zou et al prepared 84% porosity porous titanium by fiber sintering (Rare Metal mat. eng.,2007,36, 1394). S.Z.Xing et al prepared porous titanium with 70% porosity using a self-propagating high temperature synthesis (Shanghai J.biomed.Eng.,1999,20, 3).
Disclosure of Invention
The invention provides a preparation method of a porous photocatalyst filter screen, wherein the porous photocatalyst filter screen has a high surface area, has a strong photocatalytic effect under the conditions of ultraviolet light or visible light, and is high in bonding strength of a titanium dioxide nanotube and a substrate and not easy to fall off.
The technical scheme of the invention is as follows:
a preparation method of a porous photocatalyst filter screen, wherein the porous photocatalyst filter screen is porous titanium loaded with titanium dioxide or a nitrogen-doped titanium dioxide nanotube array, and the preparation method specifically comprises the following steps:
1) surface cleaning: sequentially ultrasonically cleaning porous titanium in distilled water, alcohol and acetone for 5-30 minutes, and drying; the porosity of the porous titanium is 40-98%, the through porosity is 60-100%, the aperture is 1-20mm, and the thickness is 5-100 cm;
2) anodic oxidation: preparing fluorine-containing electrolyte according to a certain proportion, putting the porous titanium serving as an anode and a platinum sheet, a titanium sheet, stainless steel or graphite serving as a cathode into the fluorine-containing electrolyte, introducing constant voltage, and carrying out anodic oxidation treatment in a constant-temperature water bath at the temperature of 0-50 ℃; then taking out and washing with distilled water, and drying;
3) annealing treatment: placing the anodized porous titanium into a muffle furnace, heating in the air atmosphere, preserving heat, annealing in the air, and air-cooling to room temperature to obtain porous titanium loaded with a titanium dioxide nanotube array;
4) nitrogen doping: putting porous titanium loaded with a titanium dioxide nanotube array in NH3And carrying out nitrogen doping heat treatment in the atmosphere, keeping the temperature, and then air-cooling to room temperature to prepare the porous titanium loaded with the nitrogen-doped titanium dioxide nanotube array.
Further, the preparation method of the porous photocatalyst filter screen comprises the following steps: HF 0-2 wt%, NaF 0-2 wt%, NH 0-2 wt%4F、0-2wt％KF、0-5wt％HNO3Matched with 0-2mol of L mol per liter-1HPO3、0-2mol.L-1H2SO4、0-2mol.L-1Na2SO4、0-2mol.L-1(NH4)2SO4、0-2mol.L-1Na2HPO4、0-2mol.L-1(NH4)2HPO4、0-2mol.L-1NaOH,、NH4H3COOH, and the solvent is glycol, water or the mixture of glycol and water.
Further, the preparation method of the porous photocatalyst filter screen is characterized in that the constant voltage is a stabilized direct current voltage, and the value is 1-200V; the distance between the cathode and the anode is controlled to be 0.1cm-20 cm; the anodic oxidation time is 0.1-24 h.
Further, the preparation method of the porous photocatalyst filter screen comprises the steps of annealing at the temperature of 250-700 ℃ and keeping the temperature for 0.5-48 h.
Further, the preparation method of the porous photocatalyst filter screen comprises the steps of carrying out nitrogen doping heat treatment at the temperature of 250-750 ℃ and carrying out heat preservation for 0.5-24 h.
The diameter of the titanium dioxide nanotube or the nitrogen-doped titanium dioxide nanotube is 10-200nm, the wall thickness is 5-100nm, and the length is 1-250 mu m.
Further, the preparation method of the porous photocatalyst filter screen comprises the following steps:
(1) preparing powder; preparing titanium or titanium alloy powder into powder;
(2) the heating body heats the powder; under the protective atmosphere of vacuum or inert gas, the powder is contacted with a heating body to be rapidly heated;
(3) heating the powder by an electromagnetic field; the heating body heats the powder through heat conduction, and simultaneously, the powder is quickly heated through an electromagnetic field to prepare a sintered body.
Further, in the preparation method of the porous photocatalyst filter screen, the powder preparation mode in the step (1) is as follows: mixing titanium or titanium alloy powder with the granularity of less than 1000 mu m with a pore-forming agent and an organic adhesive, preparing a green body by cold pressing, warm pressing, 3D printing, cold isostatic pressing, cold rolling or injection molding, and degreasing the green body to obtain the titanium or titanium alloy powder.
Further, in the preparation method of the porous photocatalyst filter screen, the powder preparation mode in the step (1) is as follows: adding titanium or titanium alloy powder with the granularity of less than 1000 mu m, a binder, a dispersant, a suspending agent, a defoaming agent, a titrant, water or an organic solvent into a container in proportion, preparing powder slurry by stirring, dipping an organic template into the powder slurry, and carrying out curing and degreasing treatment to obtain the titanium or titanium alloy powder.
Further, in the preparation method of the porous photocatalyst filter screen, the pore-forming agent is NaCl, sucrose, magnesium, urea or starch; the heating body is made of silicon carbide, silicon nitride, aluminum oxide, graphite, tungsten, molybdenum, steel, copper, titanium or titanium alloy.
Further, the preparation method of the porous photocatalyst filter screen is characterized in that the pressure for preparing the green body by the cold pressing or cold isostatic pressing process is 0.1-1500 MPa; the pressure of the green blank prepared by the warm pressing process is 0.1-1500MPa, and the temperature is 50-500 ℃; in the step 2), the vacuum condition is as follows: degree of vacuum 10-2～10-5Pa, inert gas is: argon or helium, wherein the heating temperature of the heating body is 200-1500 ℃; the electromagnetic field heating mode is as follows: microwave heating, induction heating, plasma heating or pulse heating; the heating temperature of the electromagnetic field is 600-1500 ℃, and the heat preservation time is 0.01-2400 minutes.
The invention has the beneficial effects that:
1. the porous titanium is subjected to anodic oxidation treatment to grow a titanium dioxide nanotube array on the surface of the porous titanium, an anatase type titanium dioxide nanotube array is prepared on the surface of the porous titanium through subsequent crystal form transformation annealing treatment, and the porous titanium loaded with the nitrogen-doped titanium dioxide nanotube array is prepared through a subsequent nitrogen doping process.
2. Porous titanium loaded with titanium dioxide or nitrogen-doped titanium dioxide nanotube arrays is used as a porous photocatalyst filter screen to decompose organic matters, pollutants, bacteria and the like in air and water through photocatalysis. The application method comprises the following steps: ultraviolet light or visible light is used as an excitation light source to irradiate porous titanium loaded with a titanium dioxide or nitrogen-doped titanium dioxide nanotube array, electrons are induced to be excited to a conduction band to generate corresponding holes, active oxygen and hydroxyl radicals with extremely strong oxidation effects are generated, air and organic matters, pollutants, bacteria and the like in water are oxidized and decomposed, the purification effect on the water and the air is realized, the pollutants in the air and the water can be effectively removed, and secondary pollution can not be caused
3. Titanium dioxide or nitrogen-doped titanium dioxide nanotube arrays grow on the surface of the porous titanium, and the titanium dioxide nanotubes are firmly combined with the surface of the porous titanium and are not easy to fall off; meanwhile, due to the high surface area of the porous titanium, the photocatalysis effect of the photocatalyst filter screen is enhanced, the purification efficiency of water and air is improved, and the effect of rapid purification is realized. The different pore rates of the porous titanium can control the flow speed of water and air, thereby improving the purification efficiency of the water and the air. The porous photocatalyst filter screen manufactured by the invention can realize double effects of chemical purification and physical filtration by utilizing the photocatalysis of the nano titanium oxide and the structure of the porous titanium, and has long service life and high mechanical strength.
4. The preparation method of the porous photocatalyst filter screen has the advantages of simple process, low equipment cost and low cost of the used electrolyte, and can realize large-scale industrial production.
Detailed Description
Example 1
A preparation method of a porous photocatalyst filter screen comprises the following steps:
step 1, melting the porous titanium with the net structure prepared by the 3D printing technology through the selective electron beam region, wherein the purity of the porous titanium is more than 99.3%, the porosity is 70%, the through porosity is 100%, the aperture is 5mm, and the thickness is 10 cm. Sequentially cleaning porous titanium with distilled water, alcohol and acetone for 30 minutes by ultrasonic waves, taking out and drying;
step 2, mixing the solute with mass fraction of 0.2NH4F+0.5mol/L(NH4)2SO4Preparing ammonium fluoride electrolyte with water as solvent; anodizing porous titanium in ammonium fluoride electrolyte, introducing constant voltage of 40V by using the porous titanium as an anode and a platinum sheet as a cathode, anodizing the porous titanium in water bath at constant temperature of 25 ℃ for 2h, taking out the porous titanium, washing the porous titanium with distilled water, and drying the porous titanium;
step 3, placing the anodic oxidation porous titanium into a muffle furnace, heating to 450 ℃ in the air atmosphere, preserving heat for 3 hours, and air-cooling to room temperature;
step 4, putting the prepared porous titanium loaded with the titanium dioxide nanotube array in NH3Heating to 500 ℃ in the atmosphere, preserving heat for 6h, and cooling to room temperature in air.
The photocatalytic activity of the porous photocatalyst filter screen under gas phase and liquid phase is measured by the following two evaluation systems:
and (3) degrading formaldehyde in the air, namely placing the porous photocatalyst filter screen in a closed space, introducing 6ppm of formaldehyde, irradiating the porous photocatalyst filter screen by using a high-pressure mercury lamp as an ultraviolet light source or using an L ED lamp as a visible light source, carrying out photocatalytic reaction for 30min, and analyzing by an instrument to obtain the removal rate of the porous photocatalyst filter screen on the formaldehyde.
And (3) degrading methyl orange, namely placing the porous photocatalyst filter screen in a glass container, adding the glass container into 100ml of methyl orange solution (20 mg/L), irradiating the porous photocatalyst filter screen by using a high-pressure mercury lamp as an ultraviolet light source or a L ED lamp as a visible light source, carrying out photocatalytic reaction for 30min, continuously introducing cooling water in the reaction process, and analyzing by measuring the methyl orange solution to obtain the removal rate of the porous photocatalyst filter screen on the methyl orange.
The formaldehyde removal rate of the porous photocatalyst filter screen of the embodiment reaches 90%, and the methyl orange removal rate reaches 95%.
Example 2
Step 1, melting the porous titanium with the net structure prepared by the 3D printing technology through the selective electron beam region, wherein the purity of the porous titanium is more than 99.3%, the porosity is 70%, the through porosity is 100%, the aperture is 5mm, and the thickness is 10 cm. Sequentially cleaning porous titanium with distilled water, alcohol and acetone for 30 minutes by ultrasonic waves, taking out and drying;
step 2, mixing the solute with mass fraction of 0.2NH4F+0.5mol/L(NH4)2SO4Preparing ammonium fluoride electrolyte with water as solvent; anodizing porous titanium in ammonium fluoride electrolyte, introducing constant voltage of 40V by using the porous titanium as an anode and a platinum sheet as a cathode, anodizing the porous titanium in water bath at constant temperature of 25 ℃ for 2h, taking out the porous titanium, washing the porous titanium with distilled water, and drying the porous titanium;
and 3, placing the anodic oxidation porous titanium into a muffle furnace, heating to 450 ℃ in the air atmosphere, preserving heat for 3 hours, and cooling to room temperature in air.
The formaldehyde removal rate of the prepared porous photocatalyst filter screen reaches 88%, and the methyl orange removal rate reaches 90%.
Example 3
Step 1, uniformly mixing pure titanium powder with the particle size of less than 45 mu m and urea particles with the particle size of less than 1000 mu m according to the volume ratio of 3:7, putting 100 g of the mixture into a mold, cold-pressing the mixture into a green body under the pressure of 100MPa, and putting the green body under the vacuum condition with the vacuum degree of less than 10-2Pa, degreasing to remove urea to obtain powder, wherein the degreasing temperature is 350 ℃, the heating rate is 10 ℃/min, and the degreasing time is 2 h. And placing the powder on a silicon carbide heating body, and heating the silicon carbide heating body under a vacuum condition, wherein the surface temperature of the silicon carbide heating body reaches 1000 ℃, and the heating rate is 500 ℃/min. Pulse current is introduced to heat the powder to 1000 ℃, and the temperature is kept for 5 minutes to prepare the porous titanium with the purity>99.0%, porosity of 67%, porosity of 99%, pore diameter of 1mm, and thickness of 10 cm. Sequentially cleaning porous titanium with distilled water, alcohol and acetone for 30 minutes by ultrasonic waves, taking out and drying;
step 2, using solute mass fraction of 0.2 wt% NH4F, the solvent is water and glycol solution (containing 10 vol% of H by volume fraction)2O), preparing an ammonium fluoride electrolyte; anodizing porous titanium in ammonium fluoride electrolyte, introducing constant voltage of 40V by using the porous titanium as an anode and a platinum sheet as a cathode, anodizing the porous titanium in water bath at constant temperature of 25 ℃ for 2h, taking out the porous titanium, washing the porous titanium with distilled water, and drying the porous titanium;
and 3, placing the anodic oxidation porous titanium into a muffle furnace, heating to 450 ℃ in the air atmosphere, preserving the heat for 3 hours, and air-cooling to room temperature to prepare the porous photocatalyst filter screen.
The formaldehyde removal rate of the prepared porous photocatalyst filter screen reaches 80%, and the methyl orange removal rate reaches 83%.
The above description describes only a few embodiments of the invention, and does not limit the scope of the invention. All changes and modifications that come within the spirit of the invention are desired to be protected.
Claims (10)
1. A preparation method of a porous photocatalyst filter screen is characterized in that the porous photocatalyst filter screen is porous titanium loaded with titanium dioxide or a nitrogen-doped titanium dioxide nanotube array, and specifically comprises the following steps:
1) surface cleaning: sequentially ultrasonically cleaning porous titanium in distilled water, alcohol and acetone for 5-30 minutes, and drying; the porosity of the porous titanium is 40-98%, the through porosity is 60-100%, the aperture is 1-20mm, and the thickness is 5-100 cm;
2) anodic oxidation: preparing fluorine-containing electrolyte according to a certain proportion, putting the porous titanium serving as an anode and a platinum sheet, a titanium sheet, stainless steel or graphite serving as a cathode into the fluorine-containing electrolyte, introducing constant voltage, and carrying out anodic oxidation treatment in a constant-temperature water bath at the temperature of 0-50 ℃; then taking out and washing with distilled water, and drying;
3) annealing treatment: placing the anodized porous titanium into a muffle furnace, heating in the air atmosphere, preserving heat, annealing in the air, and air-cooling to room temperature to obtain porous titanium loaded with a titanium dioxide nanotube array;
4) nitrogen doping: putting porous titanium loaded with a titanium dioxide nanotube array in NH3And carrying out nitrogen doping heat treatment in the atmosphere, keeping the temperature, and then air-cooling to room temperature to prepare the porous titanium loaded with the nitrogen-doped titanium dioxide nanotube array.
2. The method for preparing the porous photocatalyst filter screen according to claim 1, wherein the fluorine-containing electrolyte comprises: HF 0-2 wt%, NaF 0-2 wt%, NH 0-2 wt%4F、0-2wt％KF、0-5wt％HNO3Matched with 0-2mol of L mol per liter-1HPO3、0-2mol.L-1H2SO4、0-2mol.L-1Na2SO4、0-2mol.L-1(NH4)2SO4、0-2mol.L-1Na2HPO4、0-2mol.L-1(NH4)2HPO4、0-2mol.L-1NaOH,、NH4H3COOH, and the solvent is glycol, water or the mixture of glycol and water.
3. The method for preparing the porous photocatalyst filter screen according to claim 1, wherein the constant voltage is a stabilized dc voltage with a value of 1-200V; the distance between the cathode and the anode is controlled to be 0.1cm-20 cm; the anodic oxidation time is 0.1-24 h.
4. The method for preparing the porous photocatalyst filter screen according to claim 1, wherein the annealing temperature is 250-700 ℃ and the heat preservation time is 0.5-48 h.
5. The method for preparing the porous photocatalyst filter screen according to claim 1, wherein the temperature of the nitrogen doping heat treatment is 250-750 ℃, and the heat preservation time is 0.5-24 h.
6. The method for preparing the porous photocatalyst filter screen according to claim 1, wherein the method for preparing the porous titanium comprises the following steps:
(1) preparing powder; preparing titanium or titanium alloy powder into powder;
(2) the heating body heats the powder; under the protective atmosphere of vacuum or inert gas, the powder is contacted with a heating body to be rapidly heated;
(3) heating the powder by an electromagnetic field; the heating body heats the powder through heat conduction, and simultaneously, the powder is quickly heated through an electromagnetic field to prepare a sintered body.
7. The method for preparing the porous photocatalyst filter screen according to claim 6, wherein the powder preparation mode in the step (1) is as follows: mixing titanium or titanium alloy powder with the granularity of less than 1000 mu m with a pore-forming agent and an organic adhesive, preparing a green body by cold pressing, warm pressing, 3D printing, cold isostatic pressing, cold rolling or injection molding, and degreasing the green body to obtain the titanium or titanium alloy powder.
8. The method for preparing the porous photocatalyst filter screen according to claim 6, wherein the powder preparation mode in the step (1) is as follows: adding titanium or titanium alloy powder with the granularity of less than 1000 mu m, a binder, a dispersant, a suspending agent, a defoaming agent, a titrant, water or an organic solvent into a container in proportion, preparing powder slurry by stirring, dipping an organic template into the powder slurry, and carrying out curing and degreasing treatment to obtain the titanium or titanium alloy powder.
9. The method for preparing the porous photocatalyst filter screen according to claim 7, wherein the pore-forming agent is NaCl, sucrose, magnesium, urea or starch; the heating body is made of silicon carbide, silicon nitride, aluminum oxide, graphite, tungsten, molybdenum, steel, copper, titanium or titanium alloy.
10. The preparation method of the porous photocatalyst filter screen according to claim 6, wherein the pressure of the green body prepared by the cold pressing or cold isostatic pressing process is 0.1-1500 MPa; the pressure of the green blank prepared by the warm pressing process is 0.1-1500MPa, and the temperature is 50-500 ℃; in the step 2), the vacuum condition is as follows: degree of vacuum 10-2～10-5Pa, inert gas is: argon or helium, wherein the heating temperature of the heating body is 200-1500 ℃; the electromagnetic field heating mode is as follows: microwave heating, induction heating, plasma heating or pulse heating; the heating temperature of the electromagnetic field is 600-1500 ℃, and the heat preservation time is 0.01-2400 minutes.
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