CN107324780B - Flat catalytic ceramic membrane and forming method and forming equipment thereof - Google Patents
Flat catalytic ceramic membrane and forming method and forming equipment thereof Download PDFInfo
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- CN107324780B CN107324780B CN201710636421.7A CN201710636421A CN107324780B CN 107324780 B CN107324780 B CN 107324780B CN 201710636421 A CN201710636421 A CN 201710636421A CN 107324780 B CN107324780 B CN 107324780B
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- 239000012528 membrane Substances 0.000 title claims abstract description 120
- 239000000919 ceramic Substances 0.000 title claims abstract description 56
- 238000000034 method Methods 0.000 title claims abstract description 51
- 230000003197 catalytic effect Effects 0.000 title claims abstract description 45
- 239000003054 catalyst Substances 0.000 claims abstract description 74
- 239000000463 material Substances 0.000 claims abstract description 74
- 238000000926 separation method Methods 0.000 claims abstract description 48
- 238000005245 sintering Methods 0.000 claims abstract description 21
- 238000011068 loading method Methods 0.000 claims abstract description 15
- 238000013329 compounding Methods 0.000 claims abstract description 3
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 41
- 238000002156 mixing Methods 0.000 claims description 28
- NUJOXMJBOLGQSY-UHFFFAOYSA-N manganese dioxide Chemical compound O=[Mn]=O NUJOXMJBOLGQSY-UHFFFAOYSA-N 0.000 claims description 24
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 20
- 238000002360 preparation method Methods 0.000 claims description 19
- 239000004408 titanium dioxide Substances 0.000 claims description 19
- 239000002245 particle Substances 0.000 claims description 15
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 14
- 239000003795 chemical substances by application Substances 0.000 claims description 12
- 238000003756 stirring Methods 0.000 claims description 11
- 238000000498 ball milling Methods 0.000 claims description 9
- 238000001125 extrusion Methods 0.000 claims description 9
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 8
- 239000011148 porous material Substances 0.000 claims description 8
- 230000032683 aging Effects 0.000 claims description 6
- 239000011230 binding agent Substances 0.000 claims description 6
- 239000002270 dispersing agent Substances 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 6
- 239000004014 plasticizer Substances 0.000 claims description 6
- 238000007789 sealing Methods 0.000 claims description 6
- 239000000725 suspension Substances 0.000 claims description 6
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 4
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims description 4
- 229910001928 zirconium oxide Inorganic materials 0.000 claims description 4
- 230000008569 process Effects 0.000 abstract description 30
- 239000010410 layer Substances 0.000 description 91
- 229910001220 stainless steel Inorganic materials 0.000 description 33
- 239000010935 stainless steel Substances 0.000 description 33
- 239000011229 interlayer Substances 0.000 description 17
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 15
- 239000000126 substance Substances 0.000 description 14
- 239000007787 solid Substances 0.000 description 9
- 238000011160 research Methods 0.000 description 7
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 6
- 230000003647 oxidation Effects 0.000 description 6
- 238000007254 oxidation reaction Methods 0.000 description 6
- 238000004140 cleaning Methods 0.000 description 5
- 238000000465 moulding Methods 0.000 description 5
- 238000011001 backwashing Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 238000010304 firing Methods 0.000 description 4
- 238000005470 impregnation Methods 0.000 description 4
- 230000004907 flux Effects 0.000 description 3
- 230000010354 integration Effects 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- KDLHZDBZIXYQEI-UHFFFAOYSA-N palladium Substances [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 3
- 239000011787 zinc oxide Substances 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 2
- 241000219095 Vitis Species 0.000 description 2
- 235000009754 Vitis X bourquina Nutrition 0.000 description 2
- 235000012333 Vitis X labruscana Nutrition 0.000 description 2
- 235000014787 Vitis vinifera Nutrition 0.000 description 2
- 235000008429 bread Nutrition 0.000 description 2
- 238000001354 calcination Methods 0.000 description 2
- 238000003421 catalytic decomposition reaction Methods 0.000 description 2
- 235000013339 cereals Nutrition 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- 238000003618 dip coating Methods 0.000 description 2
- 238000007598 dipping method Methods 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 239000003344 environmental pollutant Substances 0.000 description 2
- AMWRITDGCCNYAT-UHFFFAOYSA-L hydroxy(oxo)manganese;manganese Chemical compound [Mn].O[Mn]=O.O[Mn]=O AMWRITDGCCNYAT-UHFFFAOYSA-L 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000001000 micrograph Methods 0.000 description 2
- 238000002715 modification method Methods 0.000 description 2
- 229910052763 palladium Inorganic materials 0.000 description 2
- 239000011941 photocatalyst Substances 0.000 description 2
- 231100000719 pollutant Toxicity 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 229910052719 titanium Inorganic materials 0.000 description 2
- 239000010936 titanium Substances 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 229910052684 Cerium Inorganic materials 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 230000001133 acceleration Effects 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000005234 chemical deposition Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000007906 compression Methods 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
- 239000013078 crystal Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 239000003651 drinking water Substances 0.000 description 1
- 235000020188 drinking water Nutrition 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000011010 flushing procedure Methods 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 230000004807 localization Effects 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 description 1
- 238000005374 membrane filtration Methods 0.000 description 1
- 238000009285 membrane fouling Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 244000005700 microbiome Species 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 description 1
- 238000005949 ozonolysis reaction Methods 0.000 description 1
- 230000002093 peripheral effect Effects 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Substances [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 229910052701 rubidium Inorganic materials 0.000 description 1
- IGLNJRXAVVLDKE-UHFFFAOYSA-N rubidium atom Chemical compound [Rb] IGLNJRXAVVLDKE-UHFFFAOYSA-N 0.000 description 1
- 239000012266 salt solution Substances 0.000 description 1
- 238000004528 spin coating Methods 0.000 description 1
- 238000004659 sterilization and disinfection Methods 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- 238000000108 ultra-filtration Methods 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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- 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
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- B01J35/396—Distribution of the active metal ingredient
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B28—WORKING CEMENT, CLAY, OR STONE
- B28B—SHAPING CLAY OR OTHER CERAMIC COMPOSITIONS; SHAPING SLAG; SHAPING MIXTURES CONTAINING CEMENTITIOUS MATERIAL, e.g. PLASTER
- B28B3/00—Producing shaped articles from the material by using presses; Presses specially adapted therefor
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/725—Treatment of water, waste water, or sewage by oxidation by catalytic oxidation
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Abstract
The invention discloses a flat catalytic ceramic membrane for changing the loading state of a catalyst, which comprises a supporting layer and a separating layer, wherein the supporting layer and the separating layer are prepared by adopting a one-step forming method; the separation layer is formed by compounding a catalyst material and a membrane material; the catalyst material is uniformly distributed in the separation layer or is partially embedded into the separation layer and partially exposed. The lower side of the separation layer and the upper side of the support layer are mutually interwoven and integrated after sintering, so that the combination of the support layer and the separation layer is realized. The invention also discloses a forming method and a forming device of the flat catalytic ceramic membrane for changing the loading state of the catalyst. The invention mixes catalyst in the support and film material, and uses relative forming device to form the film and support with assistant catalyzing function, and then uses sintering process to fire them.
Description
Technical Field
The invention relates to a flat catalytic ceramic membrane, a forming method and forming equipment thereof.
Background
The ceramic membrane has more and more researches in water treatment, and has very wide application prospect in water treatment along with the acceleration of the localization process and the reduction of the cost. Compared with the organic membrane widely used at present, the ceramic membrane has very high mechanical strength and chemical stability, so that higher flux can be adopted in the operation process, but the higher flux easily causes serious membrane pollution, particularly the membrane pollution caused by organic matters, and the conventional backwashing process is difficult to completely control the membrane pollution. Therefore, controlling membrane fouling is one of the major obstacles for the popularization and application of ceramic membranes. The current common practice is: based on the excellent chemical stability of the ceramic membrane, the ceramic membrane is directly contacted with oxidants such as ozone to form an ozone ceramic membrane integration process, which can improve the pollutant removal effect, reduce membrane pollution and increase membrane flux (Guojianing, research on treating micro-polluted drinking water by the ceramic membrane and the integration process thereof, Qinghua university, 2013; research on treating micro-polluted raw water by the ozone/ceramic membrane integration process of Van Xiao Jiang, Qinghua university, 2015). The integrated process is characterized in that the ozone oxidation and the membrane filtration are combined, but most of the existing ceramic membranes are made of alpha-alumina materials, the catalytic oxidation effect of ozone is weak, and the catalytic oxidation function of ozone cannot be fully exerted.
In order to exert the catalytic oxidation function of ozone, improve the removal efficiency of organic matters and control membrane pollution in a membrane process, the ceramic membrane is modified to have a catalytic function. The hydroxyl radicals generated by the ozonolysis oxidize the organic matter. Not only can reduce the precursor of disinfection by-products in raw water, but also can reduce the biodegradability of organic matters in membrane effluent, inhibit the propagation of microorganisms and the like. At present, the catalytic function of the ceramic membrane is modified mainly by loading materials with the catalytic function, such as iron oxide, manganese oxide, titanium oxide and the like, on the ceramic membrane. The modification process is to load active components of Ti, Pd, Pt and Ni onto the surface of the membrane or to immerse the active components into the pores of the membrane by surface impregnation, ion exchange, chemical deposition and other methods, and the membrane and the catalytically active components constitute the catalyst and the membrane plays the role of separation and catalyst carrier. Compared with the conventional catalyst, the modified catalytic ceramic membrane has the following characteristics: the catalyst is immobilized to realize heterogeneous catalytic oxidation; the catalyst becomes a part of the membrane, and the ozone is forced to contact with the catalyst and pollutants through a micropore effect while the separation effect is achieved, so that the reaction rate is increased; the immobilization of the catalyst reduces the operation and maintenance cost of the process, the process is more compact, and the space cost is saved.
Aiming at the problem that the catalytic function of the existing ceramic membrane material is weak, modification research for loading metals such as manganese, titanium, palladium, iron, rubidium, zinc, cerium and the like on the surface of an alumina ceramic membrane is carried out, and a plurality of patents in the aspect are also provided. Through research and arrangement, relevant patents about preparation and forming of the catalytic ceramic membrane are found as follows:
1) a device and method for preparing catalytic membrane (application publication No. CN102274757A), belonging to the field of membrane equipment, the core of the device is that the salt solution of catalyst is soaked by negative pressure suction, so that the catalyst is loaded in the membrane pores and on the membrane surface, and a uniform catalytic membrane is obtained after reduction, the problem is that the catalyst is not sintered, and the mechanical stability of the catalyst is likely to have problems;
2) MnO2-TiO2 graphene-porous inorganic ceramic membrane low-temperature denitration catalyst and a preparation method thereof (application publication number CN102728348A) belong to the field of gas denitration, and the core is that after an inorganic ceramic membrane body is prepared, MnO2-TiO2 graphene is loaded on the surface of the membrane by adopting a dipping method, and then sintering is carried out. The prepared ceramic membrane is not suitable for the field of water treatment in the aspects of chemical stability and mechanical stability;
3) a modification method for water treatment inorganic catalytic membrane (application publication No. CN103495345A), belonging to the field of water treatment, the core of which is that a catalyst is loaded on the surface of the membrane by adopting an immersion method or a laser deposition method without sintering process;
4) a ceramic membrane with ozone catalytic function, a preparation method thereof and a circulating coating device (application publication number CN104841292A) belong to the technical field of membrane material preparation, and the core is that a catalytic coating is prepared on a membrane surface by a layer-by-layer dip coating method, and then a catalyst is loaded on the membrane surface by a sintering process. The catalyst and the membrane formed by the method are still divided into two parts, and the catalyst may have instability in the backwashing and chemical cleaning processes of water treatment, and needs two sintering processes, so that the energy consumption is high;
5) a carrier type titanium dioxide ultrafiltration membrane, a preparation method and application thereof (CN102489172A) belong to the field of environmental pollution treatment, and the core is to load titanium dioxide on the surface of a ceramic membrane support body by a dip-coating method and fix the titanium dioxide by a sintering process. The catalyst and the support body are still divided into two parts, the mechanical property cannot be ensured, and the catalyst is prepared by a twice sintering process, so that the cost is high;
6) a multifunctional flat ceramic membrane and a preparation process thereof (application publication No. CN105000871A) belong to the technical field of ceramic membrane preparation, and the core is that a catalyst is loaded on a membrane surface on a prepared support body by a vacuum impregnation method, and then the catalyst is fixed by a sintering process. However, the matching between the catalyst and the support body in the aspects of chemical stability and mechanical stability has problems, and the requirements of back flushing and chemical cleaning processes in water treatment cannot be met;
7) a preparation method of a ceramic membrane loaded zinc oxide photocatalyst (application publication No. CN105396570A) belongs to the technical field of catalysis, and the core of the preparation method is that a dipping, pulling and calcining method is adopted, a layer of zinc oxide nanometer seed crystal is loaded on the surface of a ceramic membrane, and then a hydrothermal method and a calcining process are used for preparing the ceramic membrane loaded zinc oxide photocatalyst. The catalytic membrane is only loaded on the surface of the membrane, the mechanical and chemical stability is not high, and the catalyst and the membrane are prepared and calcined by times, so that the preparation cost is higher.
Meanwhile, in the invention patents in the aspect of the preparation of the ceramic membrane support, such as the patents with the grant numbers CN102688700B, CN103381338A, CN104828929A, CN105000871A and CN105818260A, the catalyst loading method and the forming device adopted in the invention are not mentioned.
In summary, most of the existing ceramic membrane modification methods utilize vacuum impregnation, spin coating, multiple impregnation and pulling, and then the catalyst is loaded on the surface of the membrane pores and the surface of the membrane through a firing process. However, most researches and patents do not consider the matching problem between the mechanical and chemical stability of the catalyst and the overlong service life of the ceramic membrane, the catalyst only covers the surface of the membrane support, a sintering neck may exist during sintering, and in the field of water treatment, a high-recoil strength and harsh chemical cleaning process is often used, so that the catalyst is likely to fall off from the membrane body, and the catalytic capability of the membrane is lost. In addition, the current preparation of the catalytic membrane adopts the steps of preparing the membrane firstly and modifying secondly, and the front and the back of the catalytic membrane need to be fired for at least 2 times, so that the energy consumption is increased, and the preparation cost of the catalytic membrane is increased.
Therefore, how to mold the catalyst and the ceramic membrane at one time, realize integrated preparation, strengthen the chemical and mechanical stability of the catalyst, improve the coupling degree of the catalyst and the membrane, match the catalyst with the service life of the ceramic membrane in water treatment for more than ten years, reduce the preparation cost, and become the problem which needs to be solved at present.
Disclosure of Invention
The technical problem to be solved by the invention is to overcome the defects of the prior art, and provide the flat catalytic ceramic membrane with the changed catalyst loading state, the forming method and the forming equipment thereof, so that the problem that the chemical stability and the mechanical stability of the catalyst in the catalytic ceramic membrane are not matched with the membrane body can be solved, the preparation cost of the catalytic membrane is reduced, and the industrial mass production of the catalytic ceramic membrane is promoted.
In order to solve the technical problems, the invention provides the following technical scheme:
the invention provides a flat catalytic ceramic membrane for changing the loading state of a catalyst, which comprises a supporting layer and a separating layer, wherein the supporting layer and the separating layer are prepared by adopting a one-step forming method; the separation layer is formed by compounding a catalyst material and a membrane material; the catalyst material is uniformly distributed in the separation layer or is partially embedded into the separation layer and partially exposed.
Furthermore, the lower side of the separation layer and the upper side of the support layer are mutually interwoven and integrated after sintering, so that the combination of the support layer and the separation layer is realized.
Furthermore, the aperture of the separation layer is 1-5 μm, and the thickness is 100-200 μm.
Furthermore, the porosity of the supporting layer is 40-50%, the pore diameter is 5-8 μm, and the material is high-purity alumina; the catalyst material is uniformly dispersed in the supporting layer or is partially embedded into the supporting layer and partially exposed.
The second aspect of the present invention provides a method for forming a flat catalytic ceramic membrane with a catalyst loading state changed, which comprises the following specific steps:
and 3, respectively putting the materials of the separation layer and the support layer into a feed inlet of extrusion forming equipment, and combining the material of the separation layer and the material of the support layer into a whole by using the extrusion forming equipment under the extrusion pressure of 1-10 MPa.
Further, step 1 specifically comprises:
1) taking a certain amount of alumina or zirconia with the particle size of 100-500nm, adding a pore-forming agent, a binder, a sintering agent, water and a plasticizer, and putting the mixture into a ball-milling mixer for mixing;
2) taking titanium dioxide or manganese dioxide with the particle size of 20-50nm according to the proportion of 30-70%, placing the titanium dioxide or manganese dioxide in a dispersing agent, and intensively stirring for 10 hours for later use;
3) under the stirring state, adding titanium dioxide or manganese dioxide in the suspension state into aluminum oxide or zirconium oxide in a ball-milling mixer, and mixing for 2-10 h;
4) and (3) putting the mixed separation layer material into a vacuum mixing roll for mixing mud, sealing and aging for 12-24h after mixing mud.
Further, step 2 specifically comprises:
1) taking a certain amount of alumina with the particle size of 5-10 mu m, adding a pore-forming agent, a binder, a sintering agent, water and a plasticizer, and putting the mixture into a ball-milling mixer for mixing;
2) according to the proportion of less than 30 percent, taking a proper amount of titanium dioxide or manganese dioxide with the particle size of 200-500nm, placing the titanium dioxide or manganese dioxide in a dispersing agent, and intensively stirring for 5-10h for later use;
3) under the stirring state, adding titanium dioxide or manganese dioxide in the suspension state into aluminum oxide or zirconium oxide in a ball-milling mixer, and mixing for 2-10 h;
4) and (3) putting the mixed separation layer material into a vacuum mixing roll for mixing mud, sealing and aging for 12-24h after mixing mud.
The third aspect of the invention provides a forming device for a flat catalytic ceramic membrane for changing the loading state of a catalyst, which comprises a solid stainless steel square column, wherein middle stainless steel interlayers are surrounded on the upper side and the lower side of the solid stainless steel square column, and a supporting layer forming area is formed between the solid stainless steel square column and the middle stainless steel interlayer; stainless steel shells are enclosed on the upper side and the lower side of the middle stainless steel interlayer, and a separation layer forming area is formed between each stainless steel shell and the middle stainless steel interlayer; a separating layer material inlet is formed in one side of the separating layer forming area, and a supporting layer material inlet is formed in one side of the supporting layer forming area; and a flat membrane blank outlet is formed in the other side of the support layer forming area.
Preferably, the width of the middle stainless steel interlayer is smaller than the width of the solid stainless steel square column and the width of the stainless steel shell, and the forming equipment is divided into a material conveying area and a material combining area.
Preferably, the end of the stainless steel interlayer is provided with a wedge-shaped section.
The catalysts with different particle sizes are dispersed in the separation layer and the supporting layer and are of a 'grape bread' embedded structure, and part of the catalysts are embedded on the surface of the membrane or the inner surface of the membrane hole and can contact with ozone to complete the catalytic oxidation of the ozone and the decomposition process of organic matters. Meanwhile, the embedded structure of the catalyst enables the catalyst to have a larger contact area with the surrounding membrane materials, ensures the mechanical stability of the catalyst and solves the matching problem of the mechanical stability of the catalyst and the ceramic membrane body. Even if part of the catalyst is lost due to backwashing, chemical cleaning and the like in the using process, the membrane material is lost at the same time, new catalyst is exposed again, the catalytic decomposition function of ozone can still be realized, and the structure provides a realization way for matching the catalyst with the membrane body.
When the material is used, the separating layer material and the supporting layer material respectively enter different feed inlets by adopting equal extrusion pressure, and the water content of the separating layer material is 5-10% higher than that of the supporting layer material, so that the different conveying resistances of the separating layer material and the supporting layer material are balanced, and the two materials are convenient to combine. The separating layer and the supporting layer are formed gradually in the conveying and forming process, the separating layer and the supporting layer are combined with each other in the combining area under the guidance of the middle stainless steel interlayer wedge-shaped section, and due to the fact that the water content of the separating layer is high and the grain size of the separating layer is small, part of the separating layer enters the supporting layer, and the combination of the two layers of materials is stable.
The core of the invention is that the special forming device and method are utilized to change the loading form of the catalyst in the ceramic membrane, improve the matching degree of the catalyst and the membrane body in the aspects of mechanical and chemical stability, and enable the industrial production and application of the ozone catalytic ceramic membrane to be possible. The pore size control of the support, the pore size control of the separation layer, the temperature rise procedure of the firing, etc. are not the core content of the present invention, and are similar to the procedures mentioned in most of the inventions.
The invention has the following beneficial effects:
the invention mixes catalyst in the support and film material, and uses relative forming device to form the film and support with assistant catalyzing function, and then uses sintering process to fire them.
According to the invention, catalysts with different proportions and different particle sizes are respectively doped in the support body and the membrane layer material, the catalysts are dispersed in the membrane layer and the support layer and are in a 'grape bread' type embedded structure, the embedded structure of the catalysts enables the catalysts to have larger contact area with the peripheral membrane material, the mechanical stability of the catalysts is ensured, the problem of matching of the mechanical stability of the catalysts and the ceramic membrane body is solved, even if part of the catalysts are lost due to backwashing or chemical cleaning and the like in the use process, the membrane material is lost, the new catalysts are exposed again, and the catalytic decomposition function of ozone can be still realized. Meanwhile, catalyst materials with different particle sizes and contents are adopted in the separation layer and the supporting layer, so that the preparation cost is reduced. Moreover, the preparation cost of the catalytic membrane is further reduced due to the adoption of one-step forming and one-step sintering processes.
The invention does not consider from the scientific research angle completely, but focuses on the actual production and application aspect of the catalytic ceramic membrane, and adopts raw materials which can be purchased or processed in a large scale.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the principles of the invention and not to limit the invention. In the drawings:
FIG. 1 is a schematic plan view of a molding apparatus.
FIG. 2 is a schematic cross-sectional view of the molding apparatus A-A.
FIG. 3 is a schematic cross-sectional view of a molding apparatus B-B.
Fig. 4 is an interfacial electron microscope image of the separation layer and the support layer after firing.
In the figure: 1. solid stainless steel square column, 2, stainless steel shell, 3, separation layer forming area, 4, middle stainless steel interlayer, 5, support layer forming area, 6, flat membrane blank outlet, 7, stainless steel interlayer end wedge, 8, separation layer material, 9, support layer material, 10, separation layer material inlet, 11, support layer material inlet.
Detailed Description
The preferred embodiments of the present invention will be described in conjunction with the accompanying drawings, and it will be understood that they are described herein for the purpose of illustration and explanation and not limitation.
A flat catalytic ceramic membrane for changing the loading state of a catalyst and a forming method thereof are disclosed, the flat catalytic ceramic membrane for changing the loading state of the catalyst mainly comprises: the catalyst is dispersed in the support layer and the separation layer or embedded on the pore channel surfaces of the support layer and the separation layer.
As shown in fig. 1 to 3, a forming apparatus for a flat catalytic ceramic membrane for changing a catalyst loading state includes a solid stainless steel square column 1, wherein middle stainless steel interlayers 4 are enclosed on upper and lower sides of the solid stainless steel square column 1, and a supporting layer forming region 5 is formed between the solid stainless steel square column 1 and the middle stainless steel interlayer 4; stainless steel shells 2 are enclosed on the upper side and the lower side of the middle stainless steel interlayer 4, and a separation layer forming area 3 is formed between each stainless steel shell 2 and the middle stainless steel interlayer 4; a separating layer material inlet 10 is formed in one side of the separating layer forming area 3, and a supporting layer material inlet 11 is formed in one side of the supporting layer forming area 5; and a flat membrane blank outlet 6 is arranged on the other side of the support layer forming area 5. The width of the middle stainless steel interlayer 4 is smaller than the widths of the solid stainless steel square column 1 and the stainless steel shell 2, and the forming equipment is divided into a material conveying area a and a material combining area b. The tail end of the middle stainless steel interlayer 4 is provided with a wedge-shaped section 7.
The specific forming method comprises the following steps:
1) taking a certain amount of alumina with the particle size of 500nm, adding a pore-forming agent, a binder, a sintering agent, water, a plasticizer and the like according to a proper proportion, and putting the mixture into a ball-milling mixer for mixing. According to the proportion of 70 percent of the mass of the alumina, the nano titanium dioxide with the grain diameter of 50nm is taken and placed in the dispersant to be intensively stirred for 10 hours. Under the stirring state, the titanium dioxide in the suspension state is added into the alumina or the zirconia of the ball mill mixer and mixed for 10 hours. And (3) putting the mixed separation layer material 8 into a vacuum mixing roll for mixing mud, sealing and aging for 24 hours after 5 hours of mixing mud.
2) Taking a certain amount of alumina with the particle size of 5 mu m, adding a pore-forming agent, a binder, a sintering agent, water, a plasticizer and the like according to a proper proportion, and putting the mixture into a ball mill mixer for mixing. Taking titanium dioxide with the particle size of 200nm according to 20 percent of the mass of the alumina, placing the titanium dioxide in a dispersing agent, and intensively stirring for 10 hours.
3) Under the stirring state, the titanium dioxide in the suspension state is added into the alumina or the zirconia of the ball mill mixer and mixed for 10 hours. And (3) putting the mixed separation layer material 8 into a vacuum mixing roll for mixing mud, sealing and aging for 24 hours after 5 hours of mixing mud.
4) The separation layer material 8 and the supporting layer material 9 are respectively placed into a feed inlet 10 and a feed inlet 11 of an extrusion molding machine, under the extrusion pressure of 8.0MPa, the separation layer material and the supporting layer material respectively enter a separation layer molding area 3 and a supporting layer molding area 5 under the action of pressure, and the membrane materials are separated by an intermediate stainless steel interlayer 4 and are not in contact with each other.
4) When the membrane material enters the end of the section of the forming device 1, the membrane material enters the section of the forming device 2 under the guidance of the wedge 7 at the end of the middle stainless steel interlayer, and the supporting layer and the separation layer material start to contact and combine. Because the water content of the material of the separation layer is higher than that of the material of the support layer by 5 percent and the particle size is smaller, part of the material of the separation layer enters the support layer, so that the combination of the two layers of materials is more stable. After the bonding process is completed in the forming device 2 area, the catalytic ceramic membrane blank is output from the blank outlet 6.
5) The output green body is dried and then fired to obtain the flat catalytic ceramic membrane. The porosity of the prepared flat catalytic ceramic membrane is 47%, the integral compression resistance of the prepared flat catalytic ceramic membrane is 96% of that of a catalyst-free ceramic membrane, and the ozone decomposition rate is improved by 20%.
Fig. 4 is an interfacial electron microscope image of the separation layer and the support layer after firing.
Finally, it should be noted that: although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that changes may be made in the embodiments and/or equivalents thereof without departing from the spirit and scope of the invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (1)
1. A flat catalytic ceramic membrane for changing the loading state of a catalyst comprises a supporting layer and a separating layer, wherein the supporting layer and the separating layer are prepared by a one-step forming method; the separation layer is formed by compounding a catalyst material and a membrane material; the catalyst material is uniformly distributed in the separation layer or is partially embedded into the separation layer and partially exposed; the lower side of the separation layer and the upper side of the supporting layer are mutually interwoven and integrated after sintering, so that the combination of the supporting layer and the separation layer is realized; the aperture of the separating layer is 1-5 μm, and the thickness is 100-200 μm; the porosity of the supporting layer is 40-50%, the pore diameter is 5-8 mu m, and the material is high-purity alumina; the catalyst material is uniformly dispersed in the supporting layer or is partially embedded into the supporting layer and partially exposed; it is characterized in that the preparation method is characterized in that,
the forming method of the flat catalytic ceramic membrane for changing the catalyst loading state comprises the following specific steps:
step 1, preparing a separation layer material;
step 2, preparing a supporting layer material;
step 3, respectively putting the materials of the separation layer and the support layer into a feed inlet of extrusion forming equipment, and combining the material of the separation layer and the material of the support layer into a whole by using the extrusion forming equipment under the extrusion pressure of 1-10 MPa;
wherein, the step 1 specifically comprises the following steps:
1) taking a certain amount of alumina or zirconia with the particle size of 100-500nm, adding a pore-forming agent, a binder, a sintering agent, water and a plasticizer, and putting the mixture into a ball-milling mixer for mixing;
2) taking titanium dioxide or manganese dioxide with the particle size of 20-50nm according to the proportion of 30-70%, placing the titanium dioxide or manganese dioxide in a dispersing agent, and intensively stirring for 10 hours for later use;
3) under the stirring state, adding titanium dioxide or manganese dioxide in the suspension state into aluminum oxide or zirconium oxide in a ball-milling mixer, and mixing for 2-10 h;
4) putting the mixed separation layer material into a vacuum mixing roll for mixing mud, sealing and aging for 12-24h after mixing mud;
the step 2 specifically comprises the following steps:
1) taking a certain amount of alumina with the particle size of 5-10 mu m, adding a pore-forming agent, a binder, a sintering agent, water and a plasticizer, and putting the mixture into a ball-milling mixer for mixing;
2) according to the proportion of less than 30 percent, taking a proper amount of titanium dioxide or manganese dioxide with the particle size of 200-500nm, placing the titanium dioxide or manganese dioxide in a dispersing agent, and intensively stirring for 5-10h for later use;
3) under the stirring state, adding titanium dioxide or manganese dioxide in the suspension state into aluminum oxide or zirconium oxide in a ball-milling mixer, and mixing for 2-10 h;
4) and (3) putting the mixed separation layer material into a vacuum mixing roll for mixing mud, sealing and aging for 12-24h after mixing mud.
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