CN106588092A - Photocatalytic zinc titanate porous ceramic and its preparation method and use - Google Patents
Photocatalytic zinc titanate porous ceramic and its preparation method and use Download PDFInfo
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- CN106588092A CN106588092A CN201611107946.3A CN201611107946A CN106588092A CN 106588092 A CN106588092 A CN 106588092A CN 201611107946 A CN201611107946 A CN 201611107946A CN 106588092 A CN106588092 A CN 106588092A
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- zinc titanate
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- coal dust
- zinc
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- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 title claims abstract description 46
- 229910052725 zinc Inorganic materials 0.000 title claims abstract description 45
- 239000011701 zinc Substances 0.000 title claims abstract description 45
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 title claims abstract description 43
- 230000001699 photocatalysis Effects 0.000 title claims abstract description 40
- 238000002360 preparation method Methods 0.000 title claims abstract description 26
- 239000000919 ceramic Substances 0.000 title claims abstract description 25
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims abstract description 56
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 54
- 239000011787 zinc oxide Substances 0.000 claims abstract description 29
- 238000005245 sintering Methods 0.000 claims abstract description 28
- 239000004408 titanium dioxide Substances 0.000 claims abstract description 25
- 230000004907 flux Effects 0.000 claims abstract description 17
- 238000010438 heat treatment Methods 0.000 claims abstract description 14
- 239000002994 raw material Substances 0.000 claims abstract description 9
- 238000007792 addition Methods 0.000 claims abstract description 8
- 238000002156 mixing Methods 0.000 claims abstract description 7
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 4
- 238000000465 moulding Methods 0.000 claims abstract description 4
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims description 50
- 239000000463 material Substances 0.000 claims description 39
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 38
- 239000011230 binding agent Substances 0.000 claims description 32
- 238000007146 photocatalysis Methods 0.000 claims description 31
- 235000019270 ammonium chloride Nutrition 0.000 claims description 25
- 239000002817 coal dust Substances 0.000 claims description 25
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 21
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 21
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 20
- 239000011780 sodium chloride Substances 0.000 claims description 19
- 238000001816 cooling Methods 0.000 claims description 14
- GNTDGMZSJNCJKK-UHFFFAOYSA-N divanadium pentaoxide Chemical compound O=[V](=O)O[V](=O)=O GNTDGMZSJNCJKK-UHFFFAOYSA-N 0.000 claims description 14
- 238000001035 drying Methods 0.000 claims description 11
- 230000014759 maintenance of location Effects 0.000 claims description 11
- 238000009835 boiling Methods 0.000 claims description 10
- 239000011343 solid material Substances 0.000 claims description 10
- 239000008187 granular material Substances 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 7
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 6
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 4
- 239000012467 final product Substances 0.000 claims description 4
- 230000003647 oxidation Effects 0.000 claims description 4
- 238000007254 oxidation reaction Methods 0.000 claims description 4
- 239000011941 photocatalyst Substances 0.000 claims description 4
- 238000003756 stirring Methods 0.000 claims description 4
- -1 flux Substances 0.000 claims description 3
- 229920002472 Starch Polymers 0.000 claims description 2
- 229910000410 antimony oxide Inorganic materials 0.000 claims description 2
- 229910000416 bismuth oxide Inorganic materials 0.000 claims description 2
- 239000004327 boric acid Substances 0.000 claims description 2
- 125000005619 boric acid group Chemical group 0.000 claims description 2
- TYIXMATWDRGMPF-UHFFFAOYSA-N dibismuth;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Bi+3].[Bi+3] TYIXMATWDRGMPF-UHFFFAOYSA-N 0.000 claims description 2
- 238000004898 kneading Methods 0.000 claims description 2
- VTRUBDSFZJNXHI-UHFFFAOYSA-N oxoantimony Chemical compound [Sb]=O VTRUBDSFZJNXHI-UHFFFAOYSA-N 0.000 claims description 2
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 2
- 239000008107 starch Substances 0.000 claims description 2
- 235000019698 starch Nutrition 0.000 claims description 2
- 238000001238 wet grinding Methods 0.000 claims description 2
- 230000007797 corrosion Effects 0.000 abstract description 18
- 238000005260 corrosion Methods 0.000 abstract description 18
- 239000003054 catalyst Substances 0.000 abstract description 9
- 238000000034 method Methods 0.000 abstract description 8
- 239000000126 substance Substances 0.000 abstract description 8
- 230000008569 process Effects 0.000 abstract description 5
- 238000011068 loading method Methods 0.000 abstract description 2
- 238000005469 granulation Methods 0.000 abstract 1
- 230000003179 granulation Effects 0.000 abstract 1
- 238000009413 insulation Methods 0.000 abstract 1
- 238000003825 pressing Methods 0.000 abstract 1
- 235000014692 zinc oxide Nutrition 0.000 description 22
- 229960001296 zinc oxide Drugs 0.000 description 19
- 238000000227 grinding Methods 0.000 description 12
- 239000011148 porous material Substances 0.000 description 12
- 210000001161 mammalian embryo Anatomy 0.000 description 11
- 239000002253 acid Substances 0.000 description 8
- 239000007788 liquid Substances 0.000 description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 6
- 239000000853 adhesive Substances 0.000 description 6
- 230000001070 adhesive effect Effects 0.000 description 6
- 238000013019 agitation Methods 0.000 description 6
- 239000003518 caustics Substances 0.000 description 6
- 238000000748 compression moulding Methods 0.000 description 6
- 230000000875 corresponding effect Effects 0.000 description 6
- 229960000935 dehydrated alcohol Drugs 0.000 description 6
- 238000006253 efflorescence Methods 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 6
- 235000013312 flour Nutrition 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 6
- 229940012189 methyl orange Drugs 0.000 description 6
- 239000004570 mortar (masonry) Substances 0.000 description 6
- 239000011236 particulate material Substances 0.000 description 6
- 238000001782 photodegradation Methods 0.000 description 6
- 239000000843 powder Substances 0.000 description 6
- 206010037844 rash Diseases 0.000 description 6
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 5
- 238000006555 catalytic reaction Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 238000010521 absorption reaction Methods 0.000 description 3
- 229910010293 ceramic material Inorganic materials 0.000 description 3
- 239000002131 composite material Substances 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 239000006260 foam Substances 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 238000007493 shaping process Methods 0.000 description 2
- 239000010936 titanium Substances 0.000 description 2
- 229910052719 titanium Inorganic materials 0.000 description 2
- 241000894006 Bacteria Species 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 241000790917 Dioxys <bee> Species 0.000 description 1
- XSTXAVWGXDQKEL-UHFFFAOYSA-N Trichloroethylene Chemical group ClC=C(Cl)Cl XSTXAVWGXDQKEL-UHFFFAOYSA-N 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 239000012615 aggregate Substances 0.000 description 1
- 230000000844 anti-bacterial effect Effects 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 239000012018 catalyst precursor Substances 0.000 description 1
- 230000001413 cellular effect Effects 0.000 description 1
- 238000005660 chlorination reaction Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 230000002596 correlated effect Effects 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 238000013016 damping Methods 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000009837 dry grinding Methods 0.000 description 1
- 239000000975 dye Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- DNJIEGIFACGWOD-UHFFFAOYSA-N ethanethiol Chemical compound CCS DNJIEGIFACGWOD-UHFFFAOYSA-N 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 238000005470 impregnation Methods 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 239000011810 insulating material Substances 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 239000002366 mineral element Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 239000012860 organic pigment Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229910052573 porcelain Inorganic materials 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- 238000011946 reduction process Methods 0.000 description 1
- 230000000284 resting effect Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 229960005196 titanium dioxide Drugs 0.000 description 1
- 235000010215 titanium dioxide Nutrition 0.000 description 1
- 229960002415 trichloroethylene Drugs 0.000 description 1
- UBOXGVDOUJQMTN-UHFFFAOYSA-N trichloroethylene Natural products ClCC(Cl)Cl UBOXGVDOUJQMTN-UHFFFAOYSA-N 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
- GPPXJZIENCGNKB-UHFFFAOYSA-N vanadium Chemical compound [V]#[V] GPPXJZIENCGNKB-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
- C04B38/06—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof by burning-out added substances by burning natural expanding materials or by sublimating or melting out added substances
- C04B38/063—Preparing or treating the raw materials individually or as batches
- C04B38/0635—Compounding ingredients
- C04B38/0645—Burnable, meltable, sublimable materials
- C04B38/068—Carbonaceous materials, e.g. coal, carbon, graphite, hydrocarbons
-
- 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
- B01J23/06—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of zinc, cadmium or mercury
-
- 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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/46—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on titanium oxides or titanates
- C04B35/462—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on titanium oxides or titanates based on titanates
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3284—Zinc oxides, zincates, cadmium oxides, cadmiates, mercury oxides, mercurates or oxide forming salts thereof
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
- C04B2235/9669—Resistance against chemicals, e.g. against molten glass or molten salts
- C04B2235/9692—Acid, alkali or halogen resistance
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Structural Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Manufacturing & Machinery (AREA)
- Catalysts (AREA)
Abstract
The invention belongs to the field of chemical industry, relates to a photocatalytic zinc titanate porous ceramic and its preparation method and use and especially relates to a zinc titanate porous ceramic having direct photocatalytic performances without additional catalyst loading. The preparation method of the photocatalytic zinc titanate porous ceramic utilizes the traditional oxide mixing and sintering process and comprises the following steps: (1) raw material preparation, (B) granulation and pressing molding, and (c) sintering. By controlling the addition amounts of raw materials such as titanium dioxide, zinc oxide, a flux and a pore-forming agent, a sintering temperature, thermal insulation time and a heating rate are adjusted so that the sintered porous ceramic has good porosity, corrosion resistance and photocatalytic performances.
Description
Technical field
The invention belongs to chemical field, is related to a kind of photocatalysis zinc titanate porous ceramicss and its production and use.Especially
Which is related to a kind of zinc titanate porous ceramicss for just possessing direct photocatalysis performance without other supported catalyst.
Background technology
Porous ceramic film material is the important ceramic material of a class, and its distinctive three-dimensional porous structure makes it have high hole
The features such as rate, good chemical stability, small volumetric density and low heat conductivity, so as to be widely used in various fields.It is many
Hole ceramics are also called micropore ceramics, are a kind of new ceramic materials, are through high temperature by components such as aggregate, binding agent and pore creating materials
Fire, the ceramic body with 3 D stereo network skeleton structure.
Porous ceramicss inner homogeneous are dispersed with the micropore or hole being mutually communicated, therefore which has porosity height, volume close
The big and unique physical surface property of little, specific surface area is spent, in addition the distinctive high temperature resistant of ceramic material, corrosion-resistant, high chemistry
The stability of stability and size, allows this green material of porous ceramicss in gas and liquid filtration, purification separation, chemical industry
Catalytic carrier, sound absorption damping, high-quality thermal insulating material, bio-medical plant people's material, extraordinary materials for wall and sensor material etc. are more
Aspect is used widely.Preparation technology has addition pore creating material technique, particle packing moulding process, foam process, organic foam
The new preparation process such as the conventional preparation techniques such as impregnation technology, sol-gel technology and gradient pores preparation method, ion exchange
Deng.
Due to even resting on porous ceramicss as photocatalysis about the porous ceramicss research related to photocatalysis at present
The carrier of agent, and directly there are no photocatalysiss, it is single with catalysis activity system component, and sintering temperature is high, energy consumption compared with
Big the shortcomings of.Also the pertinent literature report that zinc titanate is prepared into porous ceramicss is had no at present, and porous ceramicss are directly provided with
The case of photocatalytic activity is also more rare, is as support applications mostly using porous ceramicss.The present inventor sets
If thinking to make material system that all there is photocatalytic activity by changing correlated condition, and allow cellular ceramic substrate itself that there is catalysis
Property do not need extra load catalyst, and reduce ceramic sintering temperature, then production technology will greatly simplify, realize preparation cost
Reduction and preparation process simplification.
The content of the invention
Technical problem solved by the invention is to provide a kind of porous ceramicss prepared as major ingredient using zinc titanate, the porous
Ceramics have direct photocatalysis performance.
The preparation method of photocatalysis zinc titanate porous ceramicss of the present invention, is by controlling titanium dioxide, Zinc Oxide, fluxing
The addition of the raw materials such as agent, pore creating material, adjusts sintering temperature, temperature retention time and heating rate etc., makes sintered porous ceramics
Possess preferable percent opening, corrosion resistance and photocatalysis performance.
The preparation method of photocatalysis zinc titanate porous ceramicss of the present invention, is to prepare titanium using conventional oxide mixed-sintering method
Sour zinc system porous ceramicss, comprise the steps：
A, raw material prepare：
(1) titanium dioxide, Zinc Oxide and flux are weighed, is mixed；Coal dust, ammonium chloride and Sodium Chloride are subsequently adding, are mixed,
Obtain solid material；
(2) preparation of binding agent：Binding agent adds water to be completely dissolved and makes clear viscous solution, that is, obtain binder solution,
Seal after cooling stand-by；
It is B, pelletize, compressing：
Binder solution obtained by step A (2), mix homogeneously is added to make 0.2- solid material obtained by step A (1)
The granule of 0.5mm, is then pressed into shape, is drying to obtain ceramic idiosome；
C. sinter：
Compacting gained ceramic idiosome is sintered, is cooled down, is obtained final product zinc titanate porous ceramicss.
In above-mentioned technical proposal, step A (1) titanium dioxide, Zinc Oxide and flux are weighed by weight ratio：Dioxy
Change titanium 10-30 parts, Zinc Oxide 1-7 part, flux 0.2-6 parts.
In above-mentioned technical proposal, step A (1) titanium dioxide, Zinc Oxide and the flux of mixing is to adopt wet grinding
Mix, mixed with coal dust, ammonium chloride and Sodium Chloride after being dried again.Wherein, the drying preferably adopts freeze-day with constant temperature.Specifically,
The condition of freeze-day with constant temperature：Temperature is 80-130 DEG C, and drying time is 30-100min.
In above-mentioned technical proposal, step A (1) coal dust, ammonium chloride and Sodium Chloride are its additions as pore creating material application
Amount presses the calculating of oxide gross mass addition：Quality proportioning be coal dust 0.1-9 parts, ammonium chloride 0.1-9 parts, Sodium Chloride 0.1-9 part.
In above-mentioned technical proposal, step A (1) adds coal dust, ammonium chloride and Sodium Chloride, mixing to refer to using dry grinding
Mode is mixed.
In above-mentioned technical proposal, step A (1) titanium dioxide, Zinc Oxide, flux, coal dust, ammonium chloride and Sodium Chloride
Weight proportion be：Titanium dioxide 10-30 parts, Zinc Oxide 1-7 part, flux 0.2-6 parts, coal dust 0.1-9 parts, ammonium chloride 0.1-
9 parts, Sodium Chloride 0.1-9 part.
In above-mentioned technical proposal, step A (1) flux is boric acid, bismuth oxide, antimony oxide, five oxidations
Any one in two vanadium, sodium carbonate, sodium hydroxide or its mixing.
In above-mentioned technical proposal, step A (2) binder solution of preparing is that binding agent adds water, in the bar being stirred continuously
Close boiling is progressively heated under part, continues stirring under conditions of micro-boiling, until whole binding agents is completely dissolved to form viscous
Thick clear solution, obtains final product.
In above-mentioned technical proposal, step A (2) binding agent is soluble starch or polyvinyl alcohol (PVA).Using upper
The concentration for stating final binder solution obtained by binder making is 3%-8% (mass fraction).
In above-mentioned technical proposal, solid material obtained by blend step A (1) described in step B and binding agent obtained by step A (2)
Solution is to adopt：To solid material obtained by step A (1) slowly attach step A (2) obtained by binder solution, be fully ground solid
Body material, makes solid material mix homogeneously with binder solution, and reach being capable of the pockets of moistening degree of kneading.
In above-mentioned technical proposal, compressing described in step B, shape can adopt arbitrary shape.Can adopt and be molded into
Shape or rubbing shaping.Wherein, the molding pressure ensure that shaping without the need for too big.
In above-mentioned technical proposal, it is dried described in step B to be dried under room temperature naturally.
In above-mentioned technical proposal, sintering condition described in step C is sintering heating rate, temperature retention time, and sintering final temperature.
Specifically, it is 0.5-5 DEG C/min to sinter heating rate, and temperature retention time is 40-170min, and sintering final temperature is 900-1150 DEG C.
In above-mentioned technical proposal, the agglomerating plant that adopts is sintered described in step C for any controllable temperature heating furnace, such as Muffle
Stove.
One of the raw material that the present invention is adopted nano titanium oxide has very strong photocatalytic activity, the energy under ultraviolet light
The hole of the electronegative electronics and positively charged for moving freely enough is decomposited, hole-electron pair is formed, then with absorption on surface
H2O、O2Have an effect, generate O2, the high chemical active radical such as OH, can rapid oxidation Organic substance, so as to decomposing organic matter,
Antibacterial is killed, stench is eliminated.But nano titanium oxide is only capable of absorbing ultraviolet light in solar spectrum, does not ring in visible-range
Should；Light excites the hole of generation and electronics to be easy to be combined, and the recombination rate of photo-generated carrier is high, and photocatalysis efficiency is low, limits
The extensive application of nano titanium oxide.
One of the raw material that the present invention is adopted ZnO is a kind of new broad stopband II-VI races chemical combination with many excellent performances
Thing semi-conducting material, energy gap are about 3.3eV.It is the Novel environment-friendlymaterial material being widely studied at present, because which can pass through light
The various organic pollutions of auxiliary catalysis action breaks down；The Organic substance of difficult degradation can be ultimately oxidized as CO2And H2The inorganic matters such as O；Energy
Almost all of organic pollution in oxidation removal water, including other water technologies be difficult remove chloroform, four chlorinations
The small organic molecule such as carbon and trichloro ethylene：Electronics on conduction band has moderate reducing power. can by the heavy metal in water from
Son reduction, without removing mineral element beneficial to human body in eliminating water；Meanwhile, photocatalysis are also killed with more higher than ultraviolet
Bacterium ability, to solving the serious organic dyestuff pollution of benefit there is provided effective processing method.
Two kinds of raw materials are used alone the photocatalysis performance for being not equipped with industrial applications, but inventor using ZnO's
Energy gap is 3.2eV, has Absorption to long wave ultraviolet (UVA) and ultraviolet B radiation (UVB).Although nano-ZnO hinders
It is not so good as nano-TiO every the effect of UVB2, but it is better than nano-TiO to intercepting UVA (355～388nm) effect2.By ZnO and TiO2Enter
Row is compound, using the coupling between nanoparticle, can improve catalysis material quantum efficiency and the utilization to sunlight
Rate.
Coal dust, ammonium chloride and Sodium Chloride in the present invention is as pore creating material application.Wherein, easily divide under ammonium chloride low temperature
Solution, is low temperature occupy-place pore creating material, can form the basic structure of porous ceramicss；Coal dust is occupy-place pore creating material under higher temperature, in high temperature
Lower volatilization pore-creating, forms high temperature pore structure；Sodium Chloride is non-volatile, soluble, occupy-place pore-creating, by dissolution mechanism pore-creating, shape
Into delocalization pore structure.
The photocatalysis zinc titanate porous ceramicss obtained by above-mentioned preparation method, its material system include titanium dioxide, oxygen
Change the metatitanic acid zinc composite oxide formed between zinc and titanium dioxide and Zinc Oxide.Titanium dioxide has good with Zinc Oxide itself
Good photocatalysis performance, but sintering temperature is very high；And metatitanic acid zinc composite oxide itself also has preferable photocatalysis performance；
Therefore flux need to be added to make the material system be easy to sinter porous zinc titanate pottery in the range of compared with low temperature (900-1200 DEG C) into
Porcelain.The zinc titanate porous ceramicss obtained to the present invention carry out photocatalysis detection, and photocatalytic activity is more than 75%, even as high as
90%, it is seen that the photocatalysis performance of zinc titanate porous ceramicss of the present invention is superior, a kind of brand-new photocatalyst is provided for the public
Material, while being also equipped with preferable percent opening, corrosion resistance.
Specific embodiment
The specific embodiment of form, remakes further specifically to the above of the present invention by the following examples
It is bright, illustrate but do not limit the present invention.
The photocatalysis performance detection method of zinc titanate porous ceramicss obtained by following examples is as follows：
Zinc titanate porous ceramicss are immersed in organic pigment solution to be degraded, are stirred under light illumination or recycle stream
It is dynamic (to note：Catalyst and stirring power local collision should be avoided during stirring).Pigment solution is taken after a period of time carries out concentration survey
Examination, assesses the photocatalytic degradation effect of catalyst with this.
Embodiment 1
Polyvinyl alcohol is weighed by binder solution concentration 5% (mass percentage concentration), water is added, starts mechanical agitation, will
System is heated to slight boiling condition.After all dissolving forms clear viscous liquid to polyvinyl alcohol, as polyvinyl alcohol water solution is cold
But seal stand-by.Weigh titanium dioxide 15g, vanadic anhydride 2.79g, Zinc Oxide 4.3g, coal dust 7.6g, ammonium chloride 0.1g make
Added material is ground with ceramic mortar.Dehydrated alcohol is initially charged during grinding to material is just flooded, is carefully ground to
Dry flour bulk.130 DEG C of freeze-day with constant temperature 30min.Grind after cooling thin.Corresponding adhesive solution 10g is weighed (due to viscosity
Greatly, the mode for claiming quality is taken to be quantitatively adding) levigate powder is added, continue grinding uniform and can be kneaded into after dough gently
It is light to crumple, until whole material shapes uniformly fine particulate.(make granule pressurized according to the aqueous situation suitably drying of particulate material
After will not efflorescence immediately).After compression molding (diameter 1cm, thickness 5～6mm disc-shapeds), embryo piece is dried under field conditions (factors).By embryo
Body is sintered in being put into sintering furnace, and sintering temperature is 980 DEG C, temperature retention time 150min, and heating rate is 3 DEG C/min.With stove
Zinc titanate porous ceramicss are obtained after cooling.
The percent opening of the zinc titanate porous ceramicss under the conditions of this is 78.65%, and caustic corrosion rate is 2.51%, acid corrosion rate
5.56%, it is 77.75% to the photodegradation rate of methyl orange under ultraviolet light.
Embodiment 2
Polyvinyl alcohol is weighed by binder solution concentration 3% (mass percentage concentration), water is added, starts mechanical agitation, will
System is heated to slight boiling condition.After all dissolving forms clear viscous liquid to polyvinyl alcohol, as polyvinyl alcohol water solution is cold
But seal stand-by.Weigh titanium dioxide 26g, vanadic anhydride 0.35g, Zinc Oxide 6.73g, coal dust 1.32g, ammonium chloride 6.12g,
Added material is ground using ceramic mortar.Dehydrated alcohol is initially charged during grinding to material is just flooded, is carefully ground
To dry flour bulk.120 DEG C of freeze-day with constant temperature 40min.Grind after cooling thin.Corresponding adhesive solution 10g is weighed (due to viscosity
Greatly, the mode for claiming quality is taken to be quantitatively adding) levigate powder is added, continue grinding uniform and can be kneaded into after dough gently
It is light to crumple, until whole material shapes uniformly fine particulate.(make granule pressurized according to the aqueous situation suitably drying of particulate material
After will not efflorescence immediately).After compression molding (diameter 1cm, thickness 5～6mm disc-shapeds), embryo piece is dried under field conditions (factors).By embryo
Body is sintered in being put into sintering furnace, and sintering temperature is 1080 DEG C, temperature retention time 170min, and heating rate is 5 DEG C/min.With stove
Zinc titanate porous ceramicss are obtained after cooling.
The percent opening of the zinc titanate porous ceramicss under the conditions of this is 80.08%, and caustic corrosion rate is 4.62%, acid corrosion rate
9.91%, it is 83.79% to the photodegradation rate of methyl orange under ultraviolet light.
Embodiment 3
Polyvinyl alcohol is weighed by binder solution concentration 4% (mass percentage concentration), water is added, starts mechanical agitation, will
System is heated to slight boiling condition.After all dissolving forms clear viscous liquid to polyvinyl alcohol, as polyvinyl alcohol water solution is cold
But seal stand-by.Weigh titanium dioxide 10g, vanadic anhydride 1.68g, Zinc Oxide 5.66g, coal dust 0.61g, ammonium chloride 8.4g,
Added material is ground using ceramic mortar.Dehydrated alcohol is initially charged during grinding to material is just flooded, is carefully ground
To dry flour bulk.110 DEG C of freeze-day with constant temperature 50min.Grind after cooling thin.Corresponding adhesive solution 10g is weighed (due to viscosity
Greatly, the mode for claiming quality is taken to be quantitatively adding) levigate powder is added, continue grinding uniform and can be kneaded into after dough gently
It is light to crumple, until whole material shapes uniformly fine particulate.(make granule pressurized according to the aqueous situation suitably drying of particulate material
After will not efflorescence immediately).After compression molding (diameter 1cm, thickness 5～6mm disc-shapeds), embryo piece is dried under field conditions (factors).By embryo
Body is sintered in being put into sintering furnace, and sintering temperature is 1000 DEG C, temperature retention time 130min, and heating rate is 4 DEG C/min.With stove
Zinc titanate porous ceramicss are obtained after cooling.
The percent opening of the zinc titanate porous ceramicss under the conditions of this is 76.28%, and caustic corrosion rate is 5.17%, acid corrosion rate
7.53%, it is 89.83% to the photodegradation rate of methyl orange under ultraviolet light.
Embodiment 4
Polyvinyl alcohol is weighed by binder solution concentration 6% (mass percentage concentration), water is added, starts mechanical agitation, will
System is heated to slight boiling condition.After all dissolving forms clear viscous liquid to polyvinyl alcohol, as polyvinyl alcohol water solution is cold
But seal stand-by.Weigh titanium dioxide 23g, vanadic anhydride 5.71g, Zinc Oxide 2.06g, coal dust 6.6g, ammonium chloride 1.2g make
Added material is ground with ceramic mortar.Dehydrated alcohol is initially charged during grinding to material is just flooded, is carefully ground to
Dry flour bulk.100 DEG C of freeze-day with constant temperature 65min.Grind after cooling thin.Corresponding adhesive solution 10g is weighed (due to viscosity
Greatly, the mode for claiming quality is taken to be quantitatively adding) levigate powder is added, continue grinding uniform and can be kneaded into after dough gently
It is light to crumple, until whole material shapes uniformly fine particulate.(make granule pressurized according to the aqueous situation suitably drying of particulate material
After will not efflorescence immediately).After compression molding (diameter 1cm, thickness 5～6mm disc-shapeds), embryo piece is dried under field conditions (factors).By embryo
Body is sintered in being put into sintering furnace, and sintering temperature is 960 DEG C, temperature retention time 100min, and heating rate is 2 DEG C/min.With stove
Zinc titanate porous ceramicss are obtained after cooling.
The percent opening of the zinc titanate porous ceramicss under the conditions of this is 77.79%, and caustic corrosion rate is 5.37%, acid corrosion rate
10.89%, it is 90.25% to the photodegradation rate of methyl orange under ultraviolet light.
Embodiment 5
Polyvinyl alcohol is weighed by binder solution concentration 7% (mass percentage concentration), water is added, starts mechanical agitation, will
System is heated to slight boiling condition.After all dissolving forms clear viscous liquid to polyvinyl alcohol, as polyvinyl alcohol water solution is cold
But seal stand-by.Weigh titanium dioxide 18g, vanadic anhydride 4.53g, Zinc Oxide 3.11g, coal dust 4.8g, ammonium chloride 5.4g make
Added material is ground with ceramic mortar.Dehydrated alcohol is initially charged during grinding to material is just flooded, is carefully ground to
Dry flour bulk.90 DEG C of freeze-day with constant temperature 80min.Grind after cooling thin.Weigh corresponding adhesive solution 10g (due to viscosity greatly,
The mode for claiming quality is taken to be quantitatively adding) levigate powder is added, continue grinding uniform and can be kneaded into after dough gently
Rubbing, until whole material shapes uniformly fine particulate.Suitably it is dried (after making granule pressurized according to the aqueous situation of particulate material
Will not efflorescence immediately).After compression molding (diameter 1cm, thickness 5～6mm disc-shapeds), embryo piece is dried under field conditions (factors).By idiosome
It is sintered in being put into sintering furnace, sintering temperature is 920 DEG C, temperature retention time 75min, heating rate is 1 DEG C/min.Furnace cooling
Zinc titanate porous ceramicss are obtained afterwards.
The percent opening of the zinc titanate porous ceramicss under the conditions of this is 71.96%, and caustic corrosion rate is 4.62%, acid corrosion rate
11.42%, it is 85.69% to the photodegradation rate of methyl orange under ultraviolet light.
Embodiment 6
Polyvinyl alcohol is weighed by binder solution concentration 8% (mass percentage concentration), water is added, starts mechanical agitation, will
System is heated to slight boiling condition.After all dissolving forms clear viscous liquid to polyvinyl alcohol, as polyvinyl alcohol water solution is cold
But seal stand-by.Weigh titanium dioxide 30g, vanadic anhydride 3.36g, Zinc Oxide 1.34g, coal dust 5.3g, ammonium chloride 3.6g make
Added material is ground with ceramic mortar.Dehydrated alcohol is initially charged during grinding to material is just flooded, is carefully ground to
Dry flour bulk.80 DEG C of freeze-day with constant temperature 100min.Grind after cooling thin.Corresponding adhesive solution 10g is weighed (due to viscosity
Greatly, the mode for claiming quality is taken to be quantitatively adding) levigate powder is added, continue grinding uniform and can be kneaded into after dough gently
It is light to crumple, until whole material shapes uniformly fine particulate.(make granule pressurized according to the aqueous situation suitably drying of particulate material
After will not efflorescence immediately).After compression molding (diameter 1cm, thickness 5～6mm disc-shapeds), embryo piece is dried under field conditions (factors).By embryo
Body is sintered in being put into sintering furnace, and sintering temperature is 900 DEG C, temperature retention time 40min, and heating rate is 0.5 DEG C/min.With stove
Zinc titanate porous ceramicss are obtained after cooling.
The percent opening of the zinc titanate porous ceramicss under the conditions of this is 80.53%, and caustic corrosion rate is 4.85%, acid corrosion rate
10.11%, it is 89.72% to the photodegradation rate of methyl orange under ultraviolet light.
To sum up, addition of the preparation method of the present invention by raw materials such as control titanium dioxide, Zinc Oxide, flux, pore creating materials
Amount, adjusts sintering temperature, temperature retention time and heating rate etc., makes sintered porous ceramics possess preferable percent opening, corrosion resistant
Corrosion and photocatalysis performance.The innovative point of the present invention is to be combined the titanium dioxide with photocatalysis performance and Zinc Oxide
Porous ceramicss are made together.Without extra load again, other catalyst have photocatalysis performance to the porous ceramicss.Because nothing
By being individually titanium dioxide or Zinc Oxide in the porous ceramicss, or their composite oxides zinc titanate, all with light
Catalytic performance.And general traditional photocatalyst is to need a carrier, and this carrier be typically also porous material (can be with
It is ceramics, or plastics etc.).Therefore, the preparation of traditional photocatalyst is made up of three processes, including the system of carrier
The preparation of standby and catalyst precursor, load of the catalyst on carrier.And before the present invention specially need not go to prepare catalyst
Drive body, it is not required that single catalyst loading process.Once synthesis porous ceramicss of the present invention, i.e., with photocatalysis performance.
Claims (9)
1. the preparation method of photocatalysis zinc titanate porous ceramicss, it is characterised in that：Comprise the steps：
A, raw material prepare：
(1) titanium dioxide, Zinc Oxide and flux are weighed, is mixed；Coal dust, ammonium chloride and Sodium Chloride are subsequently adding, are mixed, must be consolidated
Body material；
(2) preparation of binding agent：Binding agent adds water and is configured to binding agent and is completely dissolved to form clear viscous solution, that is, bondd
Agent solution, seals after cooling stand-by；
It is B, pelletize, compressing：
Binder solution obtained by step A (2), mix homogeneously is added to make 0.2-0.5mm's solid material obtained by step A (1)
Granule, is then pressed into shape, is drying to obtain ceramic idiosome；
C. sinter：
Compacting gained ceramic idiosome is sintered, is cooled down, is obtained final product zinc titanate porous ceramicss.
2. the preparation method of photocatalysis zinc titanate porous ceramicss according to claim 1, it is characterised in that：At least meet with
Lower any one：
Step A (1) titanium dioxide, Zinc Oxide and flux are weighed by weight ratio：Titanium dioxide 10-30 parts, Zinc Oxide
1-7 parts, flux 0.2-6 parts；
Step A (1) coal dust, ammonium chloride and Sodium Chloride addition are calculated according to oxide gross mass addition is pressed：Quality is matched somebody with somebody
Than for coal dust 0.1-9 parts, ammonium chloride 0.1-9 parts, the coal dust of Sodium Chloride 0.1-9 part, ammonium chloride and Sodium Chloride；
Preferably, the weight proportion of step A (1) coal dust, ammonium chloride and Sodium Chloride is：Coal dust 0.1-9 parts, ammonium chloride 0.1-
9 parts, Sodium Chloride 0.1-9 part；
Step A (1) flux is boric acid, bismuth oxide, antimony oxide, vanadic anhydride, sodium carbonate, sodium hydroxide
In any one or its mixing.
3. the preparation method of photocatalysis zinc titanate porous ceramicss according to claim 2, it is characterised in that：Step A (1) institute
The weight proportion for stating titanium dioxide, Zinc Oxide, flux, coal dust, ammonium chloride and Sodium Chloride is：Titanium dioxide 10-30 parts, oxidation
Zinc 1-7 parts, flux 0.2-6 parts, coal dust 0.1-9 parts, ammonium chloride 0.1-9 parts, Sodium Chloride 0.1-9 part.
4. the preparation method of photocatalysis zinc titanate porous ceramicss according to claim 1, it is characterised in that：At least meet with
Lower any one：
Step A (1) titanium dioxide, Zinc Oxide and flux of mixing is mixed using wet grinding, after being dried again with coal dust,
Ammonium chloride and Sodium Chloride are mixed；
Preferably, the drying adopts freeze-day with constant temperature；
Further preferably, the condition of the freeze-day with constant temperature：Temperature is 80-130 DEG C, and drying time is 30-100min；
Step A (1) adds coal dust, ammonium chloride and Sodium Chloride, mixing to refer to.
5. the preparation method of photocatalysis zinc titanate porous ceramicss according to claim 1, it is characterised in that：At least meet with
Lower any one：
Step A (2) binder solution of preparing is that binding agent adds water, and close boiling is progressively heated under conditions of being stirred continuously
Rise, continue stirring under conditions of micro-boiling, until whole binding agents is completely dissolved to form clear viscous solution, obtain final product；
Step A (2) binding agent is soluble starch or polyvinyl alcohol；
Preferably, the concentration of the binder solution is 3%-8%.
6. the preparation method of photocatalysis zinc titanate porous ceramicss according to claim 1, it is characterised in that：At least meet with
Lower any one：
Solid material obtained by blend step A (1) described in step B and binder solution obtained by step A (2) are to adopt：To step A
(1) solid material obtained by slowly attach step A (2) obtained by binder solution, be fully ground solid material, make solid material with
Binder solution mix homogeneously, and reach being capable of the pockets of moistening degree of kneading；
It is to make disc-shaped using molding that disc-shaped is pressed into described in step B；
It is dried described in step B to be dried under room temperature naturally.
7. the preparation method of photocatalysis zinc titanate porous ceramicss according to claim 1, it is characterised in that：At least meet with
Lower any one：
Described in step C, sintering condition is：Sintering heating rate is 0.5-5 DEG C/min, and temperature retention time is 40-170min, and sintering is eventually
Temperature is 900-1150 DEG C；
The agglomerating plant that adopts is sintered described in step C for controllable temperature heating furnace；
Preferably, the agglomerating plant for adopting is sintered described in step C for Muffle furnace.
8. the photocatalysis zinc titanate porous ceramicss that preparation method described in any one of claim 1-7 is obtained.
9. the zinc titanate porous ceramicss described in claim 8 are used as photocatalyst applications.
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