CN109174071A - A kind of preparation method of ceramic base nano titanium dioxide film - Google Patents
A kind of preparation method of ceramic base nano titanium dioxide film Download PDFInfo
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- CN109174071A CN109174071A CN201811140036.4A CN201811140036A CN109174071A CN 109174071 A CN109174071 A CN 109174071A CN 201811140036 A CN201811140036 A CN 201811140036A CN 109174071 A CN109174071 A CN 109174071A
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- 239000000919 ceramic Substances 0.000 title claims abstract description 51
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 title claims abstract description 33
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 239000007788 liquid Substances 0.000 claims abstract description 63
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 52
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 47
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 43
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 31
- 238000010438 heat treatment Methods 0.000 claims abstract description 30
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical class [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 28
- 235000019813 microcrystalline cellulose Nutrition 0.000 claims abstract description 25
- 239000003085 diluting agent Substances 0.000 claims abstract description 24
- 229920000168 Microcrystalline cellulose Polymers 0.000 claims abstract description 23
- 239000008108 microcrystalline cellulose Substances 0.000 claims abstract description 22
- 229940016286 microcrystalline cellulose Drugs 0.000 claims abstract description 22
- 239000011261 inert gas Substances 0.000 claims abstract description 20
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 19
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 claims abstract description 16
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 claims abstract description 16
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 claims abstract description 16
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000005642 Oleic acid Substances 0.000 claims abstract description 16
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 claims abstract description 16
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 claims abstract description 16
- 229920001467 poly(styrenesulfonates) Polymers 0.000 claims abstract description 13
- 238000007599 discharging Methods 0.000 claims abstract description 12
- 238000003756 stirring Methods 0.000 claims abstract description 9
- 238000001914 filtration Methods 0.000 claims abstract description 8
- 238000010792 warming Methods 0.000 claims abstract description 8
- 238000001816 cooling Methods 0.000 claims abstract description 6
- 235000019441 ethanol Nutrition 0.000 claims description 33
- 239000000758 substrate Substances 0.000 claims description 13
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 8
- XGZNHFPFJRZBBT-UHFFFAOYSA-N ethanol;titanium Chemical compound [Ti].CCO.CCO.CCO.CCO XGZNHFPFJRZBBT-UHFFFAOYSA-N 0.000 claims description 8
- 125000005909 ethyl alcohol group Chemical group 0.000 claims description 8
- JMXKSZRRTHPKDL-UHFFFAOYSA-N titanium(IV) ethoxide Substances [Ti+4].CC[O-].CC[O-].CC[O-].CC[O-] JMXKSZRRTHPKDL-UHFFFAOYSA-N 0.000 claims description 8
- 239000001307 helium Substances 0.000 claims description 7
- 229910052734 helium Inorganic materials 0.000 claims description 7
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 7
- 238000006116 polymerization reaction Methods 0.000 claims description 7
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 6
- 239000007789 gas Substances 0.000 claims description 5
- 239000000377 silicon dioxide Substances 0.000 claims description 5
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 4
- 239000002253 acid Substances 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- 229910052708 sodium Inorganic materials 0.000 claims description 4
- 239000011734 sodium Substances 0.000 claims description 4
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 claims description 4
- 150000001298 alcohols Chemical class 0.000 claims description 3
- 229910052786 argon Inorganic materials 0.000 claims description 3
- FPCJKVGGYOAWIZ-UHFFFAOYSA-N butan-1-ol;titanium Chemical compound [Ti].CCCCO.CCCCO.CCCCO.CCCCO FPCJKVGGYOAWIZ-UHFFFAOYSA-N 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 claims description 3
- 239000003795 chemical substances by application Substances 0.000 claims description 2
- 239000004793 Polystyrene Substances 0.000 claims 1
- 229920002223 polystyrene Polymers 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 7
- 229940059939 kayexalate Drugs 0.000 abstract description 6
- 238000006555 catalytic reaction Methods 0.000 abstract description 4
- 239000000243 solution Substances 0.000 description 23
- 239000012065 filter cake Substances 0.000 description 14
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 13
- 238000006243 chemical reaction Methods 0.000 description 11
- 239000000047 product Substances 0.000 description 9
- 238000000034 method Methods 0.000 description 7
- 239000004065 semiconductor Substances 0.000 description 7
- 238000005245 sintering Methods 0.000 description 7
- 238000005507 spraying Methods 0.000 description 7
- 150000001336 alkenes Chemical class 0.000 description 6
- 239000011248 coating agent Substances 0.000 description 6
- 238000000576 coating method Methods 0.000 description 6
- 238000001035 drying Methods 0.000 description 6
- 239000007921 spray Substances 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 5
- 239000011521 glass Substances 0.000 description 5
- 238000004321 preservation Methods 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
- 238000001132 ultrasonic dispersion Methods 0.000 description 5
- 238000005406 washing Methods 0.000 description 5
- 239000000413 hydrolysate Substances 0.000 description 4
- 229920006389 polyphenyl polymer Polymers 0.000 description 4
- -1 carbohydrate organic compounds Chemical class 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 238000001514 detection method Methods 0.000 description 3
- 239000006185 dispersion Substances 0.000 description 3
- 229910002804 graphite Inorganic materials 0.000 description 3
- 239000010439 graphite Substances 0.000 description 3
- 238000005240 physical vapour deposition Methods 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 239000004408 titanium dioxide Substances 0.000 description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 235000010980 cellulose Nutrition 0.000 description 2
- 229920002678 cellulose Polymers 0.000 description 2
- 239000001913 cellulose Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 229910052738 indium Inorganic materials 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 230000005693 optoelectronics Effects 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 238000012827 research and development Methods 0.000 description 2
- 229910052719 titanium Inorganic materials 0.000 description 2
- 239000010936 titanium Substances 0.000 description 2
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 2
- 235000006508 Nelumbo nucifera Nutrition 0.000 description 1
- 240000002853 Nelumbo nucifera Species 0.000 description 1
- 235000006510 Nelumbo pentapetala Nutrition 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 239000000809 air pollutant Substances 0.000 description 1
- 231100001243 air pollutant Toxicity 0.000 description 1
- 239000012736 aqueous medium Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 210000000988 bone and bone Anatomy 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- ALSTYHKOOCGGFT-UHFFFAOYSA-N cis-oleyl alcohol Natural products CCCCCCCCC=CCCCCCCCCO ALSTYHKOOCGGFT-UHFFFAOYSA-N 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 229910021419 crystalline silicon Inorganic materials 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 239000000839 emulsion Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000007210 heterogeneous catalysis Methods 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- 230000001699 photocatalysis Effects 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 1
- 229910052573 porcelain Inorganic materials 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000000717 retained effect Effects 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- BWYYYTVSBPRQCN-UHFFFAOYSA-M sodium;ethenesulfonate Chemical compound [Na+].[O-]S(=O)(=O)C=C BWYYYTVSBPRQCN-UHFFFAOYSA-M 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 230000009967 tasteless effect Effects 0.000 description 1
- 238000009864 tensile test Methods 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 229910000314 transition metal oxide Inorganic materials 0.000 description 1
- 208000016261 weight loss Diseases 0.000 description 1
- 230000004580 weight loss Effects 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
- 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
- B01J21/08—Silica
-
- B01J35/23—
-
- B01J35/39—
-
- B01J35/59—
-
- 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
- B01J37/02—Impregnation, coating or precipitation
- B01J37/0215—Coating
-
- 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
- B01J37/02—Impregnation, coating or precipitation
- B01J37/03—Precipitation; Co-precipitation
- B01J37/031—Precipitation
- B01J37/033—Using Hydrolysis
-
- 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
- B01J37/084—Decomposition of carbon-containing compounds into carbon
-
- 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
- B01J37/10—Heat treatment in the presence of water, e.g. steam
Abstract
The invention discloses a kind of preparation methods of ceramic base nano titanium dioxide film, belong to catalysis material technical field.Ultrasonic disperse after the present invention first mixes graphene oxide, microcrystalline cellulose and water adds kayexalate, and after continuing ultrasonic disperse, filtering washs and dry, obtains modified graphene oxide；Titanate esters and alcohol diluent are stirred again, obtain A liquid, then by oleic acid and modified graphene oxide ultrasonic disperse, obtain B liquid；Then under constant temperature stirring, A liquid is slowly added dropwise into B liquid, after A liquid is added dropwise, then sulfuric acid solution is added dropwise, after sulfuric acid solution is added dropwise, hydro-thermal is stirred to react 4~6h, and cooling, discharging obtains into film liquid；Ceramic base plate surface will be sprayed at film liquid again, then under inert gas shielding state, heating charing is further warming up to 1480~1500 DEG C, after pyroreaction, and cooling, discharging is to get ceramic base nano titanium dioxide film.
Description
Technical field
The invention discloses a kind of preparation methods of ceramic base nano titanium dioxide film, belong to catalysis material technology neck
Domain.
Background technique
Titanium dioxide generates strong oxidizing property and the reduction of having respectively due to its specific band structure under the action of incident light
Property hole and electronics pair, the carbohydrate organic compounds in the air that can degrade, aqueous medium.In recent years it is net as photocatalysis environment
The research for changing material is in the ascendant.The nanosizing of titania structure size, can produce quantum optical field, greatly improve catalysis
Activity.Nano-titanium dioxide carries out photocatalytic degradation to organic pollutant using some semiconductor materials, it is finally made to generate nothing
Malicious, tasteless CO2、H2O and some simple inorganic matters are becoming an industrialization technology of environment protection field.Titanium dioxide is
N-type semiconductor, it is to use a kind of more material in heterogeneous catalysis research.Since semi-conductor nano particles have significant quantum
Dimensional effect, therefore its optical physics and photochemical properties rapidly become one of most active research field.In terms of photoelectric conversion,
It attracts attention since the porous Large ratio surface photochemical cell that Nano semiconductor is constituted has excellent photoelectric conversion performance,
It holds out broad prospects on environmental protection and Solar use.Due to nano titanium dioxide powder dispersion suspension system recycling and separation
The problems such as difficulty is big, bad dispersibility, and the toxic and harmful gas for being generated in processing air pollutants, especially room without
It can be power.Therefore research and development nanometer titania film preparing technology is more tended in recent years.Current existing nano-silica
Changing titanium film preparation method has a collosol and gel, physical vapour deposition (PVD) (PVD) method, some new to prepare nanometer titania
Film thought and technology are also in continuous research and development.Nano titanium dioxide film has characteristic of semiconductor, it can be achieved that photoelectric conversion,
Make optoelectronic pole in photocell.In the titanium dioxide membrane electrode of semiconductor doping, doping active matter is mainly transition metal oxide
Or its ion, p-type or N-type photoresponse are generated in illumination condition lower semiconductor optoelectronic pole and improve photoelectric conversion efficiency.
And traditional ceramics based nano-titanium dioxide film is in product preparation process, between titanium oxide film layer and ceramic substrate
Binding force it is weaker, cause product to be easy to happen removing in use, to influence lacking for properties of product and service life
It falls into, to obtain the promotion of more high combination property, is that it is promoted and is applied to broader field, meets industrial production demand urgently
It solves the problems, such as.
Summary of the invention
The present invention solves the technical problem of: for traditional ceramics based nano-titanium dioxide film in product preparation process
In, the binding force between titanium oxide film layer and ceramic substrate is weaker, and cause product to be easy to happen removing in use, from
And the defect of properties of product and service life is influenced, provide a kind of preparation method of ceramic base nano titanium dioxide film.
In order to solve the above-mentioned technical problem, the technical scheme adopted by the invention is that:
A kind of preparation method of ceramic base nano titanium dioxide film, specific preparation step are as follows:
(1) according to parts by weight, 30~40 parts of graphene oxides are successively taken, 4~6 parts of kayexalates, 2-4 parts micro-
Crystalline cellulose, 100~120 parts of water, ultrasonic disperse after first mixing graphene oxide, microcrystalline cellulose and water add polyphenyl
Vinyl sulfonic acid sodium, after continuing ultrasonic disperse, filtering washs and dry, obtains modified graphene oxide；
(2) according to parts by weight, 80~100 parts of titanate esters, 60~80 parts of alcohol diluents, 40~50 parts of oil are successively taken
Acid, 10~20 parts of modified graphene oxides, the sulfuric acid solution that 4~5 parts of mass fractions are 95~98%, first by titanate esters and alcohols
Diluent is stirred, and obtains A liquid, then by oleic acid and modified graphene oxide ultrasonic disperse, obtain B liquid；
(3) under constant temperature stirring, A liquid is slowly added dropwise into B liquid, after A liquid is added dropwise, then that sulfuric acid is added dropwise is molten
Liquid, after sulfuric acid solution is added dropwise, hydro-thermal is stirred to react 4~6h, cooling, and discharging obtains into film liquid；
(4) ceramic base plate surface will be sprayed at film liquid, then under inert gas shielding state, heating charing, then into
One step is warming up to 1480~1500 DEG C, after pyroreaction, and cooling, discharging is to get ceramic base nano titanium dioxide film.
Step (1) described microcrystalline cellulose is the microcrystalline cellulose that levelling off degree of polymerization is 100~120.
Step (2) titanate esters are tetraethyl titanate, metatitanic acid orthocarbonate, any one in butyl titanate.
Step (2) alcohol diluent is ethyl alcohol, normal propyl alcohol, any one in isopropanol.
Step (3) is described to be slowly added dropwise are as follows: is added dropwise with 3~5mL/min rate.
Step (4) inert gas is helium, argon gas, any one in nitrogen.
Step (4) described ceramic substrate is the ceramic substrate that dioxide-containing silica is 8~10%.
The beneficial effects of the present invention are:
(1) technical solution of the present invention changes first with dispersion performance of the kayexalate to graphene oxide
It is kind, it is conjugated between plot structure using the phenyl ring in kayexalate molecular structure and graphene oxide because π-π interacts
Power combines, while sulfonyloxy portion can make more negative electricity on graphene oxide layer structure band in kayexalate
Lotus reduces the stacking between graphene oxide layer structure because of like charges repulsive interaction；
(2) technical solution of the present invention utilizes in a heated condition, the dehydrating condensation occurred between oleic acid and alcohol diluent
The water that reaction generates makes titanate esters that slowly hydrolysis occur uniformly, and the dispersibility and partial size of hydrolysate are adjusted with this, makes its ruler
It is very little to be positively retained at nanoscale, and there is good dispersion performance, the nucleus of hydrolysate once being formed, can be by the oxygen of monolithic layer
The absorption of graphite alkene structure is fixed, and the further reunion of hydrolysate is effectively prevented, and since oleic acid and water are incompatible, in oxygen
Under the auxiliary of graphite alkene, but system forms emulsion system in whipping process, and hydrolysate is adsorbed at oil-water interfaces,
In spraying process, water phase and ceramic matrix are directly contacted, and oily phase is then covered on film surface, in inert gas shielding state
Under heating charing, oily phase organic matter and microcrystalline cellulose etc. carbonize in system, form carbonaceous skeleton and by nano-silica
Change titanium to be fixed in skeleton-pore structure, nano-titanium dioxide is avoided to reunite during the sintering process, furthermore, with temperature
It further increases, carbonaceous skeleton can form C-Si chemical bonding between the silica in ceramic matrix, thus in carbonaceous bone
Under frame auxiliary, so that nano-titanium dioxide is firmly secured to ceramic base plate surface, improve binding force between the two, effectively prevent
The loss and removing of product in use, extend product service life.
Specific embodiment
According to parts by weight, 30~40 parts of graphene oxides, 4~6 parts of kayexalates, 2~4 parts of crystallites are successively taken
Graphene oxide, microcrystalline cellulose and water are first mixed and are poured into No. 1 beaker, stirred with glass bar by cellulose, 100~120 parts of water
5~10min of mixing is mixed, is 45~55 DEG C then at temperature, under the conditions of supersonic frequency is 45~55kHz, thermostatic ultrasonic dispersion 45~
After 60min, kayexalate is added into No. 1 beaker, after continuing 30~45min of thermostatic ultrasonic dispersion, filtering must be filtered
Cake, and being washed with deionized filter cake 3~5 times, then the filter cake after washing is transferred in vacuum oven, in temperature be 95~
100 DEG C, under the conditions of pressure is 90~100Pa, it is dried under vacuum to constant weight, discharges, obtains modified graphene oxide；In parts by weight
Meter, successively takes 80~100 parts of titanate esters, 60~80 parts of alcohol diluents, 40~50 parts of oleic acid, 10~20 parts of modified graphite oxides
Alkene, the sulfuric acid solution that 4~5 parts of mass fractions are 95~98%, first pours into titanate esters and alcohol diluent in No. 2 beakers, uses
Blender is stirred 10~20min with 200~300r/min revolving speed, obtains A liquid, then oleic acid and modified graphene oxide are poured into
In No. 3 beakers, and 45~60min of ultrasonic disperse under the conditions of supersonic frequency is 55~60kHz, obtain B liquid；B liquid is transferred to water again
In hot kettle, in temperature be 65~75 DEG C, revolving speed be 400~600r/min under the conditions of, while constant temperature stirring while pass through dropping funel to
A liquid is slowly added dropwise with 3~5mL/min rate in water heating kettle, after A liquid is added dropwise, then with 8~10mL/min rate to hydro-thermal
Sulfuric acid solution is added dropwise in kettle, it is after sulfuric acid solution is added dropwise, water heating kettle is closed, it is 150~160 DEG C in temperature, revolving speed is
Under the conditions of 400~500r/min, hydro-thermal is stirred to react 4~6h, to after reaction, opens water heating kettle, cooled to room temperature,
Discharging, obtains into film liquid；Gained is passed through into spray gun spraying in ceramic base plate surface at film liquid again, control coating thickness is 2~3mm,
After 3~5h of natural drying, ceramic substrate is transferred in sintering furnace, and indifferent gas is passed through into furnace with 600~800mL/min rate
Body is warming up to 500~550 DEG C, after heat preservation carbonizes 2~3h under inert gas shielding state with 4~6 DEG C/min rate program,
Continue with the further temperature programming of 8~15 DEG C/min rate to 1480~1500 DEG C, after 1~2h of pyroreaction, cools to the furnace
Room temperature discharges to get ceramic base nano titanium dioxide film.The microcrystalline cellulose is the crystallite that levelling off degree of polymerization is 100~120
Cellulose.The titanate esters are tetraethyl titanate, metatitanic acid orthocarbonate, any one in butyl titanate.The alcohols dilution
Agent is ethyl alcohol, normal propyl alcohol, any one in isopropanol.The inert gas is helium, argon gas, any one in nitrogen.
Example 1
According to parts by weight, 40 parts of graphene oxides are successively taken, 6 parts of kayexalates, 4 parts of microcrystalline celluloses, 120
Part water, graphene oxide, microcrystalline cellulose and water are first mixed and are poured into No. 1 beaker, be stirred 10min with glass bar, then
It is 55 DEG C in temperature, under the conditions of supersonic frequency is 55kHz, after thermostatic ultrasonic disperses 60min, polyphenyl second is added into No. 1 beaker
Alkene sodium sulfonate, after continuing thermostatic ultrasonic dispersion 45min, filtering obtains filter cake, and be washed with deionized filter cake 5 times, then will washing
Filter cake afterwards is transferred in vacuum oven, is 100 DEG C in temperature, under the conditions of pressure is 100Pa, is dried under vacuum to constant weight, discharges,
Obtain modified graphene oxide；According to parts by weight, 100 parts of titanate esters are successively taken, 80 parts of alcohol diluents, 50 parts of oleic acid, 20 parts
Titanate esters and alcohol diluent are first poured into No. 2 beakers by modified graphene oxide, the sulfuric acid solution that 5 parts of mass fractions are 98%
In, 20min is stirred with 300r/min revolving speed with blender, obtains A liquid, then oleic acid and modified graphene oxide are poured into No. 3
In beaker, and the ultrasonic disperse 60min under the conditions of supersonic frequency is 60kHz, obtain B liquid；B liquid is transferred in water heating kettle again, Yu Wen
Degree is 75 DEG C, under the conditions of revolving speed is 600r/min, passes through dropping funel into water heating kettle with 5mL/min rate in constant temperature stirring
A liquid is slowly added dropwise, sulfuric acid solution is added dropwise into water heating kettle after A liquid is added dropwise, then with 10mL/min rate, to sulfuric acid solution
It is after being added dropwise, water heating kettle is closed, it is 160 DEG C in temperature, under the conditions of revolving speed is 500r/min, hydro-thermal is stirred to react 6h, to
After reaction, water heating kettle, cooled to room temperature are opened, discharging obtains into film liquid；Gained is passed through into spray gun spraying at film liquid again
In ceramic base plate surface, control coating thickness is 3mm, and after natural drying 5h, ceramic substrate is transferred in sintering furnace, and with
800mL/min rate is passed through inert gas into furnace, under inert gas shielding state, is warming up to 6 DEG C/min rate program
550 DEG C, after heat preservation charing 3h, continue with the further temperature programming of 15 DEG C/min rate to 1500 DEG C, after pyroreaction 2h, with furnace
It is cooled to room temperature, discharges to get ceramic base nano titanium dioxide film.The microcrystalline cellulose be levelling off degree of polymerization be 120 it is micro-
Crystalline cellulose.The titanate esters are tetraethyl titanate.The alcohol diluent is ethyl alcohol.The inert gas is helium.
Example 2
According to parts by weight, 40 parts of graphene oxides are successively taken, 6 parts of kayexalates, 120 parts of water first will oxidation
Graphene and water mixing are poured into No. 1 beaker, are stirred 10min with glass bar, are 55 DEG C then at temperature, supersonic frequency is
Under the conditions of 55kHz, after thermostatic ultrasonic disperses 60min, kayexalate is added into No. 1 beaker, continues thermostatic ultrasonic point
After dissipating 45min, filtering obtains filter cake, and be washed with deionized filter cake 5 times, then the filter cake after washing is transferred to vacuum oven
In, it is 100 DEG C in temperature, under the conditions of pressure is 100Pa, is dried under vacuum to constant weight, discharges, obtain modified graphene oxide；By weight
Number meter is measured, 100 parts of titanate esters, 80 parts of alcohol diluents, 50 parts of oleic acid, 20 parts of modified graphene oxides, 5 parts of quality are successively taken
The sulfuric acid solution that score is 98%, first pours into titanate esters and alcohol diluent in No. 2 beakers, is turned with blender with 300r/min
Speed is stirred 20min, obtains A liquid, then oleic acid and modified graphene oxide are poured into No. 3 beakers, and be in supersonic frequency
Ultrasonic disperse 60min under the conditions of 60kHz obtains B liquid；B liquid is transferred in water heating kettle again, in temperature be 75 DEG C, revolving speed 600r/
Under the conditions of min, passes through dropping funel in constant temperature stirring and A liquid is slowly added dropwise with 5mL/min rate into water heating kettle, to A drop
After adding, then sulfuric acid solution is added dropwise into water heating kettle with 10mL/min rate, after sulfuric acid solution is added dropwise, by water heating kettle
It is closed, it is 160 DEG C in temperature, under the conditions of revolving speed is 500r/min, hydro-thermal is stirred to react 6h, to after reaction, open hydro-thermal
Kettle, cooled to room temperature, discharging obtain into film liquid；Gained is passed through into spray gun spraying in ceramic base plate surface, control at film liquid again
Coating thickness is 3mm, and after natural drying 5h, ceramic substrate is transferred in sintering furnace, and is passed through with 800mL/min rate into furnace
Inert gas is warming up to 550 DEG C, after heat preservation carbonizes 3h with 6 DEG C/min rate program, continues under inert gas shielding state
With the further temperature programming of 15 DEG C/min rate to 1500 DEG C, after pyroreaction 2h, cools to room temperature with the furnace, discharge to get pottery
Porcelain based nano-titanium dioxide film.The titanate esters are tetraethyl titanate.The alcohol diluent is ethyl alcohol.The inert gas is
Helium.
Example 3
According to parts by weight, 100 parts of titanate esters, 80 parts of alcohol diluents, 50 parts of oleic acid, 20 parts of graphite oxides are successively taken
Alkene, the sulfuric acid solution that 5 parts of mass fractions are 98%, first pours into titanate esters and alcohol diluent in No. 2 beakers, with blender with
300r/min revolving speed is stirred 20min, obtains A liquid, then oleic acid and modified graphene oxide are poured into No. 3 beakers, and in super
Acoustic frequency is ultrasonic disperse 60min under the conditions of 60kHz, obtains B liquid；B liquid is transferred in water heating kettle again, in temperature be 75 DEG C, revolving speed
Under the conditions of 600r/min, passes through dropping funel in constant temperature stirring and A liquid is slowly added dropwise with 5mL/min rate into water heating kettle,
Sulfuric acid solution is added dropwise into water heating kettle after A liquid is added dropwise, then with 10mL/min rate, after sulfuric acid solution is added dropwise,
Water heating kettle is closed, it is 160 DEG C in temperature, under the conditions of revolving speed is 500r/min, hydro-thermal is stirred to react 6h, to after reaction,
Water heating kettle, cooled to room temperature are opened, discharging obtains into film liquid；Gained is passed through into spray gun spraying in ceramic substrate at film liquid again
Surface, control coating thickness is 3mm, after natural drying 5h, ceramic substrate is transferred in sintering furnace, and with 800mL/min rate
It is passed through inert gas into furnace, under inert gas shielding state, is warming up to 550 DEG C with 6 DEG C/min rate program, heat preservation charing
After 3h, continues with the further temperature programming of 15 DEG C/min rate to 1500 DEG C, after pyroreaction 2h, cool to room temperature with the furnace, out
Material is to get ceramic base nano titanium dioxide film.The microcrystalline cellulose is the microcrystalline cellulose that levelling off degree of polymerization is 120.It is described
Titanate esters are tetraethyl titanate.The alcohol diluent is ethyl alcohol.The inert gas is helium.
Example 4
According to parts by weight, 40 parts of graphene oxides are successively taken, 6 parts of kayexalates, 4 parts of microcrystalline celluloses, 120
Part water, graphene oxide, microcrystalline cellulose and water are first mixed and are poured into No. 1 beaker, be stirred 10min with glass bar, then
It is 55 DEG C in temperature, under the conditions of supersonic frequency is 55kHz, after thermostatic ultrasonic disperses 60min, polyphenyl second is added into No. 1 beaker
Alkene sodium sulfonate, after continuing thermostatic ultrasonic dispersion 45min, filtering obtains filter cake, and be washed with deionized filter cake 5 times, then will washing
Filter cake afterwards is transferred in vacuum oven, is 100 DEG C in temperature, under the conditions of pressure is 100Pa, is dried under vacuum to constant weight, discharges,
Obtain modified graphene oxide；According to parts by weight, 100 parts of titanate esters, 80 parts of alcohol diluents, 20 parts of modified oxidized stones are successively taken
Black alkene, the sulfuric acid solution that 5 parts of mass fractions are 98%, titanate esters and alcohol diluent are first poured into No. 2 beakers, use blender
It is stirred 20min with 300r/min revolving speed, obtains A liquid, then modified graphene oxide is poured into No. 3 beakers, and in supersonic frequency
Rate is ultrasonic disperse 60min under the conditions of 60kHz, obtains B liquid；B liquid is transferred in water heating kettle again, is 75 DEG C in temperature, revolving speed is
Under the conditions of 600r/min, passes through dropping funel in constant temperature stirring and A liquid is slowly added dropwise with 5mL/min rate into water heating kettle, to A
After liquid is added dropwise, then sulfuric acid solution is added dropwise into water heating kettle with 10mL/min rate, after sulfuric acid solution is added dropwise, by water
Hot kettle is closed, is 160 DEG C in temperature, and under the conditions of revolving speed is 500r/min, hydro-thermal is stirred to react 6h, to after reaction, open
Water heating kettle, cooled to room temperature, discharging obtain into film liquid；Again by gained at film liquid by spray gun spraying in ceramic base plate surface,
Control coating thickness is 3mm, after natural drying 5h, ceramic substrate is transferred in sintering furnace, and with 800mL/min rate into furnace
It is passed through inert gas, under inert gas shielding state, is warming up to 550 DEG C, after heat preservation carbonizes 3h with 6 DEG C/min rate program,
Continue with the further temperature programming of 15 DEG C/min rate to 1500 DEG C, after pyroreaction 2h, cool to room temperature with the furnace, discharges, i.e.,
Obtain ceramic base nano titanium dioxide film.The microcrystalline cellulose is the microcrystalline cellulose that levelling off degree of polymerization is 120.The titanate esters
For tetraethyl titanate.The alcohol diluent is ethyl alcohol.The inert gas is helium.
Example 5
According to parts by weight, 40 parts of graphene oxides are successively taken, 6 parts of kayexalates, 4 parts of microcrystalline celluloses, 120
Part water, graphene oxide, microcrystalline cellulose and water are first mixed and are poured into No. 1 beaker, be stirred 10min with glass bar, then
It is 55 DEG C in temperature, under the conditions of supersonic frequency is 55kHz, after thermostatic ultrasonic disperses 60min, polyphenyl second is added into No. 1 beaker
Alkene sodium sulfonate, after continuing thermostatic ultrasonic dispersion 45min, filtering obtains filter cake, and be washed with deionized filter cake 5 times, then will washing
Filter cake afterwards is transferred in vacuum oven, is 100 DEG C in temperature, under the conditions of pressure is 100Pa, is dried under vacuum to constant weight, discharges,
Obtain modified graphene oxide；According to parts by weight, 100 parts of titanate esters are successively taken, 80 parts of alcohol diluents, 50 parts of oleic acid, 20 parts
Titanate esters and alcohol diluent are first poured into No. 2 beakers by modified graphene oxide, the sulfuric acid solution that 5 parts of mass fractions are 98%
In, 20min is stirred with 300r/min revolving speed with blender, obtains A liquid, then oleic acid and modified graphene oxide are poured into No. 3
In beaker, and the ultrasonic disperse 60min under the conditions of supersonic frequency is 60kHz, obtain B liquid；B liquid is transferred in water heating kettle again, Yu Wen
Degree is 75 DEG C, under the conditions of revolving speed is 600r/min, passes through dropping funel into water heating kettle with 5mL/min rate in constant temperature stirring
A liquid is slowly added dropwise, sulfuric acid solution is added dropwise into water heating kettle after A liquid is added dropwise, then with 10mL/min rate, to sulfuric acid solution
It is after being added dropwise, water heating kettle is closed, it is 160 DEG C in temperature, under the conditions of revolving speed is 500r/min, hydro-thermal is stirred to react 6h, to
After reaction, water heating kettle, cooled to room temperature are opened, discharging obtains into film liquid；Gained is passed through into spray gun spraying at film liquid again
In ceramic base plate surface, control coating thickness is 3mm, after natural drying 5h, ceramic substrate is transferred in sintering furnace, at 500 DEG C
Under the conditions of calcine 3h, cool to room temperature with the furnace, discharge to get ceramic base nano titanium dioxide film.The microcrystalline cellulose is pole
Limit the microcrystalline cellulose that the degree of polymerization is 120.The titanate esters are tetraethyl titanate.The alcohol diluent is ethyl alcohol.
Comparative example: the ceramic base nano titanium dioxide film of Wuxi new material Co., Ltd production.
Example 1 to the resulting ceramic base nano titanium dioxide film of example 5 and comparative example product are subjected to performance detection, specifically
Detection method is as follows:
Overburden amount: using pressor unit determination of tensile test method, between 25mm × 300mm sample is placed in upper/lower die, on
Lower mold imposes the certain pressing force of sample (3000N), sample within the regular hour (1min) with certain speed (100mm/
Min) by mold, sample is then removed, overburden amount is evaluated using weight-loss method.
Using testing test specimen overburden amount again after 60 days.
Specific testing result is as shown in table 1:
The 1 specific testing result of ceramic base nano titanium dioxide film of table
| Detection project | Example 1 | Example 2 | Example 3 | Example 4 | Example 5 | Comparative example |
| Overburden amount/g | 0.005 | 0.012 | 0.019 | 0.021 | 0.024 | 0.032 |
| Overburden amount/g after 60 days | 0.007 | 0.018 | 0.027 | 0.036 | 0.041 | 0.057 |
By 1 testing result of table it is found that the ceramic base nano titanium dioxide film of technical solution of the present invention preparation is with excellent
The characteristics of peeling resistance and long service life, has broad prospects in the development of catalysis material technology industry.
Claims (7)
1. a kind of preparation method of ceramic base nano titanium dioxide film, it is characterised in that specific preparation step are as follows:
(1) according to parts by weight, 30~40 parts of graphene oxides, 4~6 parts of kayexalates, 2-4 parts of crystallites fibres are successively taken
Dimension element, 100~120 parts of water, ultrasonic disperse after first mixing graphene oxide, microcrystalline cellulose and water add polystyrene
Sodium sulfonate, after continuing ultrasonic disperse, filtering washs and dry, obtains modified graphene oxide；
(2) according to parts by weight, 80~100 parts of titanate esters are successively taken, 60~80 parts of alcohol diluents, 40~50 parts of oleic acid, 10
~20 parts of modified graphene oxides, the sulfuric acid solution that 4~5 parts of mass fractions are 95~98% first dilute titanate esters and alcohols
Agent is stirred, and obtains A liquid, then by oleic acid and modified graphene oxide ultrasonic disperse, obtain B liquid；
(3) under constant temperature stirring, A liquid is slowly added dropwise into B liquid, after A liquid is added dropwise, then sulfuric acid solution is added dropwise, to
After sulfuric acid solution is added dropwise, hydro-thermal is stirred to react 4~6h, cooling, and discharging obtains into film liquid；
(4) ceramic base plate surface will be sprayed at film liquid, then under inert gas shielding state, heating charing, further
1480~1500 DEG C, after pyroreaction are warming up to, cooling, discharging is to get ceramic base nano titanium dioxide film.
2. a kind of preparation method of ceramic base nano titanium dioxide film according to claim 1, it is characterised in that step (1)
The microcrystalline cellulose is the microcrystalline cellulose that levelling off degree of polymerization is 100~120.
3. a kind of preparation method of ceramic base nano titanium dioxide film according to claim 1, it is characterised in that step (2)
The titanate esters are tetraethyl titanate, metatitanic acid orthocarbonate, any one in butyl titanate.
4. a kind of preparation method of ceramic base nano titanium dioxide film according to claim 1, it is characterised in that step (2)
The alcohol diluent is ethyl alcohol, normal propyl alcohol, any one in isopropanol.
5. a kind of preparation method of ceramic base nano titanium dioxide film according to claim 1, it is characterised in that step (3)
It is described to be slowly added dropwise are as follows: to be added dropwise with 3~5mL/min rate.
6. a kind of preparation method of ceramic base nano titanium dioxide film according to claim 1, it is characterised in that step (4)
The inert gas is helium, argon gas, any one in nitrogen.
7. a kind of preparation method of ceramic base nano titanium dioxide film according to claim 1, it is characterised in that step (4)
The ceramic substrate is the ceramic substrate that dioxide-containing silica is 8~10%.
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