CN112892243A - Electric heating ceramic filtering membrane and preparation method thereof - Google Patents
Electric heating ceramic filtering membrane and preparation method thereof Download PDFInfo
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- CN112892243A CN112892243A CN202110129108.0A CN202110129108A CN112892243A CN 112892243 A CN112892243 A CN 112892243A CN 202110129108 A CN202110129108 A CN 202110129108A CN 112892243 A CN112892243 A CN 112892243A
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- filter membrane
- electrothermal
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- support body
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- 239000012528 membrane Substances 0.000 title claims abstract description 267
- 239000000919 ceramic Substances 0.000 title claims abstract description 134
- 238000002360 preparation method Methods 0.000 title claims abstract description 78
- 238000001914 filtration Methods 0.000 title abstract description 52
- 238000005485 electric heating Methods 0.000 title abstract description 12
- 238000000576 coating method Methods 0.000 claims description 60
- 239000011248 coating agent Substances 0.000 claims description 59
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 claims description 50
- 229910001887 tin oxide Inorganic materials 0.000 claims description 48
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 44
- 239000007788 liquid Substances 0.000 claims description 38
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 32
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims description 32
- 239000011787 zinc oxide Substances 0.000 claims description 22
- 238000005507 spraying Methods 0.000 claims description 13
- 238000000889 atomisation Methods 0.000 claims description 12
- 238000006243 chemical reaction Methods 0.000 claims description 12
- 238000000034 method Methods 0.000 claims description 10
- DDFHBQSCUXNBSA-UHFFFAOYSA-N 5-(5-carboxythiophen-2-yl)thiophene-2-carboxylic acid Chemical compound S1C(C(=O)O)=CC=C1C1=CC=C(C(O)=O)S1 DDFHBQSCUXNBSA-UHFFFAOYSA-N 0.000 claims description 9
- 229910021626 Tin(II) chloride Inorganic materials 0.000 claims description 9
- 230000008021 deposition Effects 0.000 claims description 9
- 238000010438 heat treatment Methods 0.000 claims description 9
- 238000000197 pyrolysis Methods 0.000 claims description 9
- 235000011150 stannous chloride Nutrition 0.000 claims description 9
- AXZWODMDQAVCJE-UHFFFAOYSA-L tin(II) chloride (anhydrous) Chemical compound [Cl-].[Cl-].[Sn+2] AXZWODMDQAVCJE-UHFFFAOYSA-L 0.000 claims description 9
- AZWHFTKIBIQKCA-UHFFFAOYSA-N [Sn+2]=O.[O-2].[In+3] Chemical compound [Sn+2]=O.[O-2].[In+3] AZWHFTKIBIQKCA-UHFFFAOYSA-N 0.000 claims description 7
- 229910052758 niobium Inorganic materials 0.000 claims description 7
- 239000010955 niobium Substances 0.000 claims description 7
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 claims description 7
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims description 5
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 5
- 229910052782 aluminium Inorganic materials 0.000 claims description 5
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 5
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- 239000011701 zinc Substances 0.000 claims description 5
- 239000011267 electrode slurry Substances 0.000 claims description 4
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 3
- 229910052738 indium Inorganic materials 0.000 claims description 3
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 claims description 3
- 239000010936 titanium Substances 0.000 claims description 3
- 229910052719 titanium Inorganic materials 0.000 claims description 3
- 230000000694 effects Effects 0.000 abstract description 10
- 239000000463 material Substances 0.000 abstract description 10
- 239000000706 filtrate Substances 0.000 abstract description 6
- 230000007613 environmental effect Effects 0.000 abstract description 4
- 239000000853 adhesive Substances 0.000 abstract description 3
- 230000001070 adhesive effect Effects 0.000 abstract description 3
- 238000004134 energy conservation Methods 0.000 abstract description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 70
- 239000000243 solution Substances 0.000 description 59
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- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 45
- 230000007704 transition Effects 0.000 description 42
- 239000000203 mixture Substances 0.000 description 38
- 238000003756 stirring Methods 0.000 description 36
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 32
- 239000000843 powder Substances 0.000 description 32
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- 238000001816 cooling Methods 0.000 description 30
- 239000004033 plastic Substances 0.000 description 28
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 26
- 239000008367 deionised water Substances 0.000 description 26
- 229910021641 deionized water Inorganic materials 0.000 description 26
- 239000002002 slurry Substances 0.000 description 26
- 229920000609 methyl cellulose Polymers 0.000 description 25
- 239000001923 methylcellulose Substances 0.000 description 25
- 235000010981 methylcellulose Nutrition 0.000 description 25
- 239000005995 Aluminium silicate Substances 0.000 description 24
- 235000012211 aluminium silicate Nutrition 0.000 description 24
- 238000001035 drying Methods 0.000 description 24
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 description 24
- 239000002245 particle Substances 0.000 description 24
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 23
- 238000002156 mixing Methods 0.000 description 20
- 238000005303 weighing Methods 0.000 description 20
- 235000019441 ethanol Nutrition 0.000 description 19
- URLJKFSTXLNXLG-UHFFFAOYSA-N niobium(5+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Nb+5].[Nb+5] URLJKFSTXLNXLG-UHFFFAOYSA-N 0.000 description 18
- 235000006408 oxalic acid Nutrition 0.000 description 15
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 14
- 238000007599 discharging Methods 0.000 description 14
- 238000010304 firing Methods 0.000 description 13
- 238000007789 sealing Methods 0.000 description 13
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 13
- 230000032683 aging Effects 0.000 description 12
- 229910000484 niobium oxide Inorganic materials 0.000 description 12
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- 239000008158 vegetable oil Substances 0.000 description 12
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 11
- 239000010453 quartz Substances 0.000 description 11
- 229910052709 silver Inorganic materials 0.000 description 11
- 239000004332 silver Substances 0.000 description 11
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 10
- 229920002472 Starch Polymers 0.000 description 10
- 239000008107 starch Substances 0.000 description 10
- 235000019698 starch Nutrition 0.000 description 10
- 229910010271 silicon carbide Inorganic materials 0.000 description 9
- 239000002518 antifoaming agent Substances 0.000 description 8
- 238000000498 ball milling Methods 0.000 description 8
- AMGQUBHHOARCQH-UHFFFAOYSA-N indium;oxotin Chemical compound [In].[Sn]=O AMGQUBHHOARCQH-UHFFFAOYSA-N 0.000 description 8
- 238000000926 separation method Methods 0.000 description 8
- 239000007864 aqueous solution Substances 0.000 description 7
- 239000011259 mixed solution Substances 0.000 description 7
- 239000003638 chemical reducing agent Substances 0.000 description 6
- 229910052593 corundum Inorganic materials 0.000 description 6
- 239000010431 corundum Substances 0.000 description 6
- 238000007598 dipping method Methods 0.000 description 6
- 229910003437 indium oxide Inorganic materials 0.000 description 6
- PSCMQHVBLHHWTO-UHFFFAOYSA-K indium(iii) chloride Chemical compound Cl[In](Cl)Cl PSCMQHVBLHHWTO-UHFFFAOYSA-K 0.000 description 6
- ZKATWMILCYLAPD-UHFFFAOYSA-N niobium pentoxide Inorganic materials O=[Nb](=O)O[Nb](=O)=O ZKATWMILCYLAPD-UHFFFAOYSA-N 0.000 description 6
- 239000011148 porous material Substances 0.000 description 6
- 229910000019 calcium carbonate Inorganic materials 0.000 description 5
- 239000002131 composite material Substances 0.000 description 5
- 239000011224 oxide ceramic Substances 0.000 description 5
- 238000012545 processing Methods 0.000 description 5
- 238000005245 sintering Methods 0.000 description 5
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 description 4
- 239000007789 gas Substances 0.000 description 4
- MRELNEQAGSRDBK-UHFFFAOYSA-N lanthanum(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[La+3].[La+3] MRELNEQAGSRDBK-UHFFFAOYSA-N 0.000 description 4
- WPCMRGJTLPITMF-UHFFFAOYSA-I niobium(5+);pentahydroxide Chemical compound [OH-].[OH-].[OH-].[OH-].[OH-].[Nb+5] WPCMRGJTLPITMF-UHFFFAOYSA-I 0.000 description 4
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 description 4
- 238000004321 preservation Methods 0.000 description 4
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- 229910021627 Tin(IV) chloride Inorganic materials 0.000 description 3
- ZOIORXHNWRGPMV-UHFFFAOYSA-N acetic acid;zinc Chemical compound [Zn].CC(O)=O.CC(O)=O ZOIORXHNWRGPMV-UHFFFAOYSA-N 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 description 3
- 230000004907 flux Effects 0.000 description 3
- 239000011521 glass Substances 0.000 description 3
- 229910010272 inorganic material Inorganic materials 0.000 description 3
- 239000011147 inorganic material Substances 0.000 description 3
- 238000007689 inspection Methods 0.000 description 3
- 238000003801 milling Methods 0.000 description 3
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- 230000004048 modification Effects 0.000 description 3
- 238000007670 refining Methods 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- HPGGPRDJHPYFRM-UHFFFAOYSA-J tin(iv) chloride Chemical compound Cl[Sn](Cl)(Cl)Cl HPGGPRDJHPYFRM-UHFFFAOYSA-J 0.000 description 3
- 239000004246 zinc acetate Substances 0.000 description 3
- 239000002253 acid Substances 0.000 description 2
- 229910021538 borax Inorganic materials 0.000 description 2
- 229910000420 cerium oxide Inorganic materials 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 230000018109 developmental process Effects 0.000 description 2
- 238000001125 extrusion Methods 0.000 description 2
- PJXISJQVUVHSOJ-UHFFFAOYSA-N indium(iii) oxide Chemical compound [O-2].[O-2].[O-2].[In+3].[In+3] PJXISJQVUVHSOJ-UHFFFAOYSA-N 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
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- 239000011368 organic material Substances 0.000 description 2
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 description 2
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 230000008929 regeneration Effects 0.000 description 2
- 238000011069 regeneration method Methods 0.000 description 2
- BSWGGJHLVUUXTL-UHFFFAOYSA-N silver zinc Chemical compound [Zn].[Ag] BSWGGJHLVUUXTL-UHFFFAOYSA-N 0.000 description 2
- 239000004328 sodium tetraborate Substances 0.000 description 2
- 235000010339 sodium tetraborate Nutrition 0.000 description 2
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 description 2
- 229910001928 zirconium oxide Inorganic materials 0.000 description 2
- 229910021532 Calcite Inorganic materials 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
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- 229910000278 bentonite Inorganic materials 0.000 description 1
- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical compound O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 description 1
- 235000013361 beverage Nutrition 0.000 description 1
- YHWCPXVTRSHPNY-UHFFFAOYSA-N butan-1-olate;titanium(4+) Chemical compound [Ti+4].CCCC[O-].CCCC[O-].CCCC[O-].CCCC[O-] YHWCPXVTRSHPNY-UHFFFAOYSA-N 0.000 description 1
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- 238000006555 catalytic reaction Methods 0.000 description 1
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- 238000005372 isotope separation Methods 0.000 description 1
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- 239000007769 metal material Substances 0.000 description 1
- 244000005700 microbiome Species 0.000 description 1
- 229920000620 organic polymer Polymers 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 230000008569 process Effects 0.000 description 1
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- 238000007569 slipcasting Methods 0.000 description 1
- LLZRNZOLAXHGLL-UHFFFAOYSA-J titanic acid Chemical compound O[Ti](O)(O)O LLZRNZOLAXHGLL-UHFFFAOYSA-J 0.000 description 1
- 239000011592 zinc chloride Substances 0.000 description 1
- 235000005074 zinc chloride Nutrition 0.000 description 1
Images
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/02—Inorganic material
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
- B01D67/0039—Inorganic membrane manufacture
- B01D67/0067—Inorganic membrane manufacture by carbonisation or pyrolysis
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
- B01D69/10—Supported membranes; Membrane supports
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Separation Using Semi-Permeable Membranes (AREA)
Abstract
The invention discloses an electrothermal ceramic filtering membrane, which belongs to the technical field of inorganic nonmetallic materials, can directly heat filtrate near the filtering membrane and then filter the filtrate, and has the characteristics of good filtering effect, high heat utilization efficiency, energy conservation and environmental protection; the electric heating filter membrane comprises a support body, wherein an electric heating filter membrane layer is arranged on the surface of the support body, and an electrode is arranged on the surface of the electric heating filter membrane layer. The invention also discloses a preparation method of the electric heating ceramic filtering membrane, and the electric heating ceramic filtering membrane prepared by the preparation method has high adhesive strength and good conductive effect.
Description
Technical Field
The invention relates to the technical field of inorganic non-metallic materials, in particular to an electrothermal ceramic filtering membrane; the invention also relates to a preparation method of the filter membrane.
Background
At present, according to the preparation materials, the filtering membranes are divided into organic material membranes and inorganic material membranes. The inorganic material film is mainly a ceramic material filter film. The ceramic filter membrane is mainly prepared from inorganic materials such as aluminum oxide, silicon carbide, zirconium oxide, titanium oxide, diatomite and the like, and has the advantages of high separation efficiency, acid and alkali resistance, organic solvent resistance, microorganism resistance, high temperature resistance, high mechanical strength, good regeneration performance, simple separation process, simple and convenient operation and maintenance, long service life and the like. The method is widely applied to the fields of environmental protection, sewage treatment, gas separation and purification, food processing, membrane catalysis, biomedicine, membrane bioreactors, resource recycling, fine chemical engineering and the like. Although the ceramic filtration membrane is expensive compared to organic material membranes, it is difficult to replace the ceramic filtration membrane in the treatment of chemically aggressive liquids and gases and in the cleaning and regeneration of strong acids and bases or at high temperatures.
The research and application of ceramic filtration membranes began in the 40's of the 20 th century, initially for isotope separation. In the 80 s, the ceramic filtration membrane separation technology started to turn to the civil field as a precise filtration separation technology, and was used to replace the traditional separation technologies such as evaporation, centrifugation, plate-and-frame filtration and the like. In the meantime, a large number of ceramic filter membrane commodities come out, and organic polymer membranes have been partially replaced in the industrial fields of water treatment, beverages, dairy products and the like. In the 90 s, the development of novel ceramic filtering membrane materials and application projects thereof is accelerated, and the stage enters a research and application stage mainly comprising gas separation and a ceramic filtering membrane separator-reactor combined member. In the 21 st century, the integration of ceramic filtration membranes with various application industries, the combination with other separation, purification and reaction processes, the cross research of membrane materials and membrane application processes, and the like become the main trends of the development of the ceramic filtration membrane field.
The preparation process of the ceramic filter membrane comprises the following steps: membrane support material batching → blank processing → shaping → drying → support body burning → processing inspection → coating filter membrane layer → membrane layer burning → finishing → inspection → assembly membrane module → inspection → finished product warehousing.
The film support is usually formed by plastic extrusion. The preparation of the filtering membrane layer generally adopts the methods of spraying and dipping to coat the filtering membrane slurry on the surface required by the ceramic support body, and then the filtering membrane layer is obtained by heat treatment.
One of the main problems encountered in the use of the ceramic filter membrane is that the filter efficiency is reduced due to the blockage of the membrane pores, and experiments show that if the liquid to be filtered is heated and then filtered, on one hand, the pressure difference required by the filtration can be correspondingly reduced due to the reduction of the viscosity of the liquid, and the blockage of the membrane pores is improved. On the other hand, at the same filtration pressure, the filtration flux will be increased by increasing the temperature of the filtrate, decreasing the viscosity. Therefore, in the prior art, the liquid to be filtered is heated and then filtered, and the processing mode has low working efficiency and large power consumption. Therefore, the invention of a filtering method with good filtering effect, energy saving and environmental protection is urgently needed.
Disclosure of Invention
The invention aims to provide an electrothermal ceramic filtering membrane, which can be used for directly heating and then filtering filtrate near the filtering membrane and has the characteristics of good filtering effect, high heat utilization efficiency, energy conservation and environmental protection.
The invention also aims to provide a preparation method of the electrothermal ceramic filter membrane, and the electrothermal ceramic filter membrane prepared by the preparation method has high adhesive strength and good conductive effect.
The former technical scheme adopted by the invention is as follows:
an electrothermal ceramic filter membrane comprises a support body, wherein an electrothermal filter membrane layer is arranged on the surface of the support body, and an electrode is arranged on the surface of the electrothermal filter membrane layer.
Furthermore, a middle filter membrane layer is arranged between the electric heating filter membrane layer and the support body, and the number of the middle filter membrane layer is one or more.
Further, the electrothermal ceramic filter membrane is any one of a porous flat plate, a single-hole tube, a porous tube, a hollow round plate and a hollow round sheet.
The latter technical scheme adopted by the invention is as follows:
a preparation method of an electrothermal ceramic filter membrane comprises the following preparation steps:
(1) placing the support body in a space, heating, introducing atomized coating liquid to carry out pyrolysis reaction deposition, and generating an electrothermal filtering film layer on the surface of the support body;
(2) coating electrode slurry on the electrothermal filtering membrane layer and then baking or burning the electrode to obtain the electrothermal ceramic filtering membrane, or thermally spraying the electrode on the electrothermal filtering membrane layer to obtain the electrothermal ceramic filtering membrane.
Further, the coating liquid is doped tin oxide sol, wherein the concentration of tin dichloride is 0.01-1.5 mol/L, the concentration of ammonium fluoride is 0.001-0.01 mol/L, and the molar ratio of tin to niobium in the doped tin oxide sol is as follows: 9.5: 0.5-9.99: 0.01.
Further, the coating solution is doped zinc oxide sol, wherein the molar ratio of zinc to aluminum in the doped zinc oxide sol is 8: 2-9.9: 0.1.
Further, the coating liquid is doped tin oxide-indium oxide sol, wherein the molar ratio of tin to indium in the doped tin oxide-indium oxide sol is 9.5: 0.5-0.5: 9.5.
Further, the coating liquid is doped titanium oxide sol, wherein the molar ratio of niobium to titanium in the niobium-doped titanium oxide sol is 0.01: 1-0.1: 1.
Further, in the step (1), the temperature is 500-750 ℃ when the pyrolysis reaction deposition is carried out.
Further, the atomization method of the coating liquid is any one of pressure atomization, compressed air atomization and ultrasonic atomization.
Compared with the prior art, the invention has the beneficial effects that:
1. the invention relates to an electrothermal ceramic filter membrane, which comprises a support body, wherein an electrothermal filter membrane layer is arranged on the surface of the support body, and an electrode is arranged on the surface of the electrothermal filter membrane layer. The electrothermal filter membrane layer is arranged on the surface of the support body, so that the electrothermal filter membrane layer can be subjected to the functions of conductive heating, surface modification and filtering, the filtered liquid near the filter membrane can be filtered after being heated, the viscosity of the filtered liquid is reduced, the blockage of membrane pores is reduced, the filtering flux is improved, and the filtering effect is better; when the device is used, only the filtrate near the filtering membrane is heated, so that the heat utilization efficiency is higher, and the device is energy-saving and environment-friendly.
2. The invention relates to a preparation method of an electrothermal ceramic filter membrane, which comprises the steps of placing a support body in a space, heating, introducing atomized coating liquid for pyrolytic reaction and deposition, and generating an electrothermal filter membrane layer on the surface of the support body; coating electrode slurry on the electrothermal filtering membrane layer and then baking or burning the electrode to obtain the electrode, or thermally spraying the electrode on the electrothermal filtering membrane layer to obtain the electrode. The electric heating ceramic filtering membrane prepared by the preparation method has high adhesive strength and good electric conduction effect.
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 application, illustrate embodiment(s) of the invention and together with the description serve to explain the invention without limiting the invention. In the drawings:
fig. 1 is a schematic structural view of the present invention.
Description of reference numerals: 1. a support body; 2. an electrothermal filter membrane layer; 3. an electrode; 4. an intermediate filter membrane layer.
Detailed Description
The technical solution of the present invention will be described in further detail with reference to the following embodiments, but the present invention is not limited thereto.
Referring to fig. 1, the electrothermal ceramic filter membrane of the present invention comprises a support 1, wherein an electrothermal filter membrane layer 2 is disposed on a surface of the support 1, an electrode 3 is disposed on a surface of the electrothermal filter membrane layer 2, and the electrode 3 can perform electrical distribution and electrical connection. The electrothermal filter membrane layer 2 is arranged on the surface of the support body 1, so that the electrothermal filter membrane layer 2 can be subjected to the functions of conductive heating, surface modification and filtering, the filtered liquid near the filter membrane can be filtered after being heated, the viscosity of the filtered liquid is reduced, the membrane hole blockage is reduced, the filtering flux is improved, and the filtering effect is better; when the device is used, only the filtrate near the filtering membrane is heated, so that the heat utilization efficiency is higher, and the device is energy-saving and environment-friendly.
An intermediate filtering film layer 4 is also arranged between the electric heating filtering film layer 2 and the support body 1, and the number of the intermediate filtering film layer 4 is one or more. When the pore size of the support body 1 is too large to support the electro-thermal filter membrane layer 2, the intermediate filter membrane layer 4 is added as a transition in order to bridge the support body 1 and the electro-thermal filter membrane layer 2. The support body 1 and the middle filter membrane layer 4 are made of materials such as alumina, silicon oxide, zirconia, silicon carbide, titanium oxide, diatomite and the like or a composite of the materials, the pore diameter of the support body 1 is 0.1-10 micrometers, and the pore diameter of a layer membrane of the middle filter membrane layer 4 is 0.05-0.5 micrometer. The electrothermal filter membrane layer 2 is made of conductive tin oxide, zinc oxide, indium oxide, titanium oxide, titanic acid , carbon (graphite, graphene) or the like or a composite of the materials, and the electrode material can be metal silver, copper, aluminum, zinc and the like.
The electric heating ceramic filtering membrane is any one of a porous flat plate, a single-hole tubular, a porous tubular, a hollow round plate and a hollow round sheet.
The invention relates to a preparation method of an electrothermal ceramic filter membrane, which comprises the following preparation steps:
(1) after the support body 1 is placed in an independent space and heated, the atomized coating liquid is introduced to carry out pyrolysis reaction deposition under a certain temperature condition, and a layer of compound is generated on the surface of the support body 1 through chemical reaction generated among components of a gas medium, so that the electrothermal filter film layer 2 is generated on the surface of the support body 1. Wherein, the temperature during the deposition of the pyrolysis reaction is 500-750 ℃, the preferable temperature is 560-590 ℃, and the deposition of the pyrolysis reaction is carried out when the temperature is controlled in the range, so that the deposition effect of the pyrolysis reaction can be optimal. The atomization method of the coating liquid is any one of pressure atomization, compressed air atomization and ultrasonic atomization, and the particle fineness of atomized liquid drops of the coating liquid is not limited.
(2) Coating electrode slurry on the electrothermal filter membrane layer 2 and then baking or burning the electrode 3 to obtain the electrothermal ceramic filter membrane, or thermally spraying the electrode 3 on the electrothermal filter membrane layer 2 to obtain the electrothermal ceramic filter membrane.
The electrothermal ceramic filter membrane prepared by the preparation method of the electrothermal ceramic filter membrane is thin and has a thickness of 100 micrometers (mum) or less, but the membrane deposited on the surface of the support body through pyrolysis reaction has high adhesion strength and good electric conduction effect.
The process for preparing the support body 1 comprises the following steps: the forming method of the support body 1 comprises any one of extrusion forming, dry pressing forming, slip casting forming, hot pressing injection forming and injection molding.
The process for preparing the intermediate filter membrane layer 4 comprises the following steps: batching, slurry processing, slurry performance adjustment, coating, drying and sintering, wherein the coating method of the intermediate filter membrane layer 4 is any one of a dip coating method, a spraying method, a pouring method and a throwing and pouring method.
Further, the coating solution is doped tin oxide sol and is prepared by the following steps:
(1) dissolving a certain amount of tin dichloride and ammonium fluoride in deionized water, sealing and stirring uniformly, adding a proper amount of ethanol and hydrochloric acid, standing to obtain a tin oxide solution for later use, wherein the stirring time is about 30 minutes.
(2) And dissolving niobium pentoxide in hydrofluoric acid, and adding a proper amount of absolute ethyl alcohol after the hydrofluoric acid is volatilized sufficiently to prepare a niobium oxide solution.
(3) And (3) mixing the tin oxide solution obtained in the step (1) and the niobium oxide solution obtained in the step (2) according to a certain concentration ratio to obtain the doped tin oxide sol. Wherein, the concentration of the tin dichloride is 0.01-1.5 mol/L, the concentration of the ammonium fluoride is 0.001-0.01 mol/L, and the mol ratio of tin to niobium in the doped tin oxide sol is as follows: 9.5: 0.5-9.99: 0.01.
Further, the coating solution is doped zinc oxide sol, and the preparation process comprises the following steps: dissolving a certain amount of zinc acetate and aluminum trichloride in deionized water, sealing and stirring uniformly for about 30 minutes, adding a proper amount of ethanol and hydrochloric acid, and standing to obtain doped zinc oxide sol, wherein the concentration of zinc element is 0.01-1.5 mol/L, and the molar ratio of zinc to aluminum in the doped zinc oxide sol is 8: 2-9.9: 0.1.
Further, the coating liquid is doped tin oxide-indium oxide sol, and the preparation process comprises the following steps: dissolving a certain amount of stannic chloride and indium trichloride in deionized water, stirring uniformly in a sealed state for about 30 minutes, then adding a proper amount of ethanol and hydrofluoric acid, and standing to obtain doped stannic oxide-indium oxide sol, wherein the total concentration of stannic oxide and indium oxide is 0.01-1.5 mol/L, and the molar ratio of stannic to indium in the doped stannic oxide-indium oxide sol is 9.5: 0.5-0.5: 9.5.
Further, the coating solution is doped titanium oxide sol and is prepared by the following steps:
(1) dissolving a certain amount of titanium tetrachloride in a mixed solution of oxalic acid, absolute ethyl alcohol and deionized water, and stirring the solution in a sealed manner uniformly to obtain a solution A for later use, wherein the molar ratio of the titanium tetrachloride to the oxalic acid in the solution A is 1: 2-1: 6, the concentration of the oxalic acid in an ethanol aqueous solution is 1.0-2.0 mol/L, the volume ratio of water to ethanol in the ethanol aqueous solution is 1:1, and the stirring time is about 30 minutes.
(2) And dissolving niobium hydroxide into an oxalic acid aqueous solution to obtain a solution B for later use, wherein the concentration of the oxalic acid aqueous solution is 1.0-2.0 mol/L, and the molar ratio of niobium to oxalic acid in the solution B is 1: 2-1: 5.
(3) And (3) mixing the solution A obtained in the step (1) and the solution B obtained in the step (2) according to a certain proportion to obtain doped titanium oxide sol, wherein the molar ratio of niobium to titanium in the niobium-doped titanium oxide sol is 0.01: 1-0.1: 1.
Example 1:
preparation of support 1: weighing 50 kg of alumina powder with the average particle size of 3 microns, 4.6 kg of kaolin, 0.83 kg of calcium carbonate, 2.0 kg of starch and 2.6 kg of methyl cellulose, putting the mixture into a mixer to be uniformly mixed, adding 15 kg of water and 2.7 kg of vegetable oil to be uniformly stirred, putting the mixture into a vacuum pug mill to be milled into compact plastic mud segments, ageing the compact plastic mud segments for 48 hours, putting the compact plastic mud segments into a vacuum extruder to be extruded and formed into porous flat ceramic membrane support body blanks, drying the porous flat ceramic membrane support body blanks, putting the porous flat ceramic membrane support body blanks into a kiln to be baked at 1350 ℃ for 2 hours, and taking the porous flat ceramic membrane support body out of the kiln.
Preparing a doped tin oxide coating liquid:
(1) dissolving 0.5mol of tin dichloride and 0.006mol of ammonium fluoride in 1.0L of deionized water, sealing and stirring uniformly, adding 60mL of ethanol and 5mL of hydrochloric acid, standing to obtain a tin oxide solution for later use, wherein the stirring time is about 30 minutes.
(2) 0.0263mol of niobium pentoxide is fully dissolved in 30mL of hydrofluoric acid, and after the hydrofluoric acid is fully volatilized, 50mL of absolute ethyl alcohol is added to prepare a niobium oxide solution.
(3) And (3) mixing the tin oxide solution obtained in the step (1) with the niobium oxide solution obtained in the step (2) to obtain the doped tin oxide coating solution.
Preparation of the electrothermal filter membrane layer 2: the alumina ceramic flat membrane with the specification of 100mm multiplied by 500mm multiplied by 3mm is vertically placed in a muffle furnace, the temperature is heated to 500 ℃, 20 g of doped tin oxide sol prepared by the preparation process is sprayed into the furnace from a furnace door, after the composition of the sol is decomposed, a conductive tin oxide membrane layer is generated on the surface of an intermediate transition membrane layer on one side, the other side is changed, 20 g of doped tin oxide sol prepared by the preparation process is sprayed, a conductive tin oxide membrane layer is generated on the surface of an intermediate transition membrane layer on the other side, and after cooling, low-temperature silver electrodes are coated on two ends of the ceramic membrane, so that the electrothermal ceramic filter membrane with the resistance value of 50 ohms is obtained.
Example 2:
preparation of support 1: weighing 50 kg of quartz powder with the average particle size of 5 microns, 3.3 kg of kaolin, 2.6 kg of glass powder, 5.5 kg of starch and 2.6 kg of methyl cellulose, putting the mixture into a mixer to be uniformly mixed, adding 13 kg of water and 2.8 kg of vegetable oil to be uniformly stirred, putting the mixture into a vacuum pug mill to be refined into compact plastic mud sections, ageing the compact plastic mud sections for 24 hours, putting the compact plastic mud sections into a vacuum extruder to be extruded and formed into porous flat ceramic membrane support body blanks, drying the porous flat ceramic membrane support body blanks, putting the porous flat ceramic membrane support body blanks into a kiln to be subjected to heat preservation at 1100 ℃ for 2 hours, and taking the porous flat ceramic membrane support bodies.
Preparing a doped tin oxide coating liquid:
(1) dissolving 1.5mol of tin dichloride and 0.01mol of ammonium fluoride in 0.785L of deionized water, sealing and stirring uniformly, adding 100mL of ethanol and 15mL of hydrochloric acid, standing to obtain a tin oxide solution for later use, wherein the stirring time is about 30 minutes.
(2) 0.079mol of niobium pentoxide is fully dissolved in 80mL of hydrofluoric acid, and 100mL of absolute ethyl alcohol is added after the hydrofluoric acid is fully volatilized to prepare a niobium oxide solution.
(3) And (3) mixing the tin oxide solution obtained in the step (1) with the niobium oxide solution obtained in the step (2) to obtain the doped tin oxide coating solution.
Preparation of the electrothermal ceramic filter membrane 2: vertically placing a quartz ceramic flat membrane with the specification of 100mm multiplied by 500mm multiplied by 3mm in a muffle furnace, heating to 590 ℃, spraying 20 g of doped tin oxide sol prepared by the preparation process into the furnace from a furnace door, generating a conductive tin oxide membrane layer on the surface of the intermediate transition membrane layer on one side after the composition of the sol is decomposed, changing the surface, spraying 20 g of doped tin oxide sol prepared by the preparation process, generating a conductive tin oxide membrane layer on the surface of the intermediate transition membrane layer on the other side, coating high-temperature silver-zinc electrodes on two ends of the ceramic membrane after cooling, and obtaining the electrothermal ceramic filtering membrane with the resistance value of 35 ohms after burning the electrodes at 600 ℃.
Example 3:
preparation of support 1: weighing 50 kg of zirconia powder with the average particle size of 1 micron, 1.5 kg of yttrium oxide, 1.0 kg of kaolin, 60 g of lanthanum oxide, 72 g of cerium oxide, 6.0 kg of starch and 2.8 kg of methyl cellulose, putting the materials into a mixer, uniformly mixing, adding 19 kg of water and 2.8 kg of vegetable oil, uniformly stirring, putting the mixture into a vacuum pug mill, refining into a compact plastic pug segment, ageing for 72 hours, putting the compact plastic pug segment into a vacuum extruder, extruding and forming into a single-hole tubular ceramic membrane support body blank with the diameter of 20mm, drying, putting the blank into a kiln, keeping the temperature at 1350 ℃ for 2 hours, firing, cooling, and taking the blank out of the kiln to obtain the zirconia ceramic support body.
Preparing a doped tin oxide coating liquid:
(1) dissolving 0.01mol of tin dichloride and 0.001mol of ammonium fluoride in 0.949L of deionized water, sealing and stirring uniformly, adding 30mL of ethanol and 1mL of hydrochloric acid, standing to obtain a tin oxide solution for later use, wherein the stirring time is about 30 minutes.
(2) And fully dissolving 0.0001mol of niobium pentoxide in 10mL of hydrofluoric acid, and adding 20mL of absolute ethyl alcohol after the hydrofluoric acid is fully volatilized to prepare a niobium oxide solution.
(3) And (3) mixing the tin oxide solution obtained in the step (1) with the niobium oxide solution obtained in the step (2) to obtain the doped tin oxide coating solution.
Preparation of the electrothermal ceramic filter membrane 2: transversely placing a zirconium oxide ceramic tubular membrane with the specification of (phi 20 mm-phi 16mm) multiplied by 300mm in a muffle furnace, enabling the tube to rotate ceaselessly, heating to 650 ℃, spraying 100 g of doped tin oxide sol prepared through the preparation process into the furnace from the top of the furnace for multiple times, generating a conductive tin oxide membrane layer on the outer surface of the membrane tube after the composition of the sol is decomposed, coating high-temperature silver electrodes at two ends of the ceramic membrane after cooling, and sintering the electrodes at 700 ℃ to obtain the tubular electrothermal ceramic filter membrane with the resistance value of 330 ohms.
Example 4:
preparation of support 1: weighing 50 kg of alumina powder with the average particle size of 30 microns, 4.6 kg of kaolin, 0.33 kg of calcium carbonate, 2.0 kg of starch and 2.6 kg of methyl cellulose, putting the mixture into a mixer to be uniformly mixed, adding 15 kg of water and 2.5 kg of vegetable oil to be uniformly stirred, putting the mixture into a vacuum pug mill to be milled into compact plastic mud segments, ageing the compact plastic mud segments for 48 hours, putting the compact plastic mud segments into a vacuum extruder to be extruded and formed into porous flat ceramic membrane support body blanks, drying the porous flat ceramic membrane support body blanks, putting the porous flat ceramic membrane support body blanks into a kiln, keeping the temperature of 1400 ℃ for 2 hours, firing the porous flat ceramic membrane support body blanks, cooling.
Preparation of the intermediate transition film layer 4: weighing 10 kg of alumina powder with the average particle size of 3 microns, 1.8 kg of kaolin, 35 g of methylcellulose and 6.6 kg of water, putting the alumina powder, 1.8 kg of kaolin, 35 g of methylcellulose and 6.6 kg of water into a ball mill, ball-milling for 2 hours, discharging slurry, adding a defoaming agent to remove bubbles, coating the slurry on the surface required by an alumina support body in a dipping way, drying, putting the alumina support body into a kiln for 1350 ℃, preserving heat for 1 hour, firing, cooling and discharging the alumina support body out of the kiln to obtain the alumina ceramic flat membrane with the intermediate.
Preparing a doped tin oxide coating liquid:
(1) dissolving 0.5mol of tin dichloride and 0.006mol of ammonium fluoride in 0.885L of deionized water, sealing and stirring uniformly, adding 60mL of ethanol and 5mL of hydrochloric acid, standing to obtain a tin oxide solution for later use, wherein the stirring time is about 30 minutes.
(2) 0.018mol of niobium pentoxide is fully dissolved in 30mL of hydrofluoric acid, and after the hydrofluoric acid is fully volatilized, 50mL of absolute ethyl alcohol is added to prepare a niobium oxide solution.
(3) And (3) mixing the tin oxide solution obtained in the step (1) with the niobium oxide solution obtained in the step (2) to obtain the doped tin oxide coating solution.
Preparation of the electrothermal filter membrane layer 2: the alumina ceramic flat membrane with the specification of 100mm multiplied by 500mm multiplied by 3mm and the middle transition membrane layer is vertically placed in a muffle furnace, the temperature is heated to 620 ℃, 15 g of doped tin oxide sol prepared by the preparation process is sprayed into the furnace from a furnace door, after the composition of the sol is decomposed, a conductive tin oxide membrane layer is generated on the surface of the middle transition membrane layer on one side, the other side is changed, 15 g of doped tin oxide sol prepared by the preparation process is sprayed, a conductive tin oxide membrane layer is generated on the surface of the middle transition membrane layer on the other side, and low-temperature silver electrodes are coated on two ends of the ceramic membrane after cooling, so that the electrothermal ceramic filter membrane with the resistance value of 65 ohms is obtained.
Example 5:
preparation of support 1: weighing 40 kg of alumina powder with the average particle size of 30 microns, 10 kg of zirconia powder with the average particle size of 10 microns, 330 g of yttrium oxide, 3.9 kg of kaolin and 2.6 kg of methylcellulose, putting the mixture into a mixer, uniformly mixing, adding 13 kg of water and 2.6 kg of vegetable oil, uniformly stirring, putting the mixture into a vacuum pug mill, milling into compact plastic mud segments, ageing for 48 hours, putting the compact plastic mud segments into a vacuum extruder, extruding and forming into porous flat ceramic membrane support body blanks, drying, putting the porous flat ceramic membrane support body blanks into a kiln, keeping the temperature of 1400 ℃ for 2 hours, sintering, cooling and taking the ceramic support body out of the kiln to obtain the alumina-zirconia composite ceramic support body.
Preparation of the intermediate transition film layer 4: weighing 10 kg of alumina powder with the average particle size of 3 microns, 1.8 kg of kaolin, 35 g of methylcellulose and 7.9 kg of water, putting the alumina powder, 1.8 kg of kaolin, 35 g of methylcellulose and 7.9 kg of water into a ball mill, ball-milling for 2 hours, discharging the slurry, adding a defoaming agent to remove bubbles, spraying the slurry on the surface required by an alumina support body by pressure, drying, putting the slurry into a kiln at 1350 ℃, preserving heat for 1 hour, firing, cooling and discharging the slurry out of the kiln to obtain the alumina-zirconia composite ceramic flat membrane with the intermediate transition membrane layer.
Preparing a doped tin oxide coating liquid:
(1) dissolving 0.5mol of tin dichloride and 0.002mol of ammonium fluoride in 0.915L of deionized water, sealing and stirring uniformly, adding 60mL of ethanol and 5mL of hydrochloric acid, standing to obtain a tin oxide solution for later use, wherein the stirring time is about 30 minutes.
(2) 0.0005mol of niobium pentoxide is fully dissolved in 10mL of hydrofluoric acid, and 20mL of absolute ethyl alcohol is added after the hydrofluoric acid is fully volatilized to prepare a niobium oxide solution.
(3) And (3) mixing the tin oxide solution obtained in the step (1) with the niobium oxide solution obtained in the step (2) to obtain the doped tin oxide coating solution.
Preparation of the electrothermal ceramic filter membrane 2: the alumina-zirconia composite ceramic flat membrane with the specification of 100mm multiplied by 500mm multiplied by 3mm and the middle transition membrane layer is vertically placed in a muffle furnace, the temperature is heated to 620 ℃, 10 g of doped tin oxide sol prepared by the preparation process is sprayed into the furnace from a furnace door, after the composition of the sol is decomposed, a conductive tin oxide membrane layer is generated on the surface of the middle transition membrane layer on one side, the other side is changed, 10 g of doped tin oxide sol prepared by the preparation process is sprayed, a conductive tin oxide membrane layer is generated on the surface of the middle transition membrane layer on the other side, and low-temperature silver electrodes are coated on two ends of the ceramic membrane after cooling, so that the electrothermal ceramic filter membrane with the resistance value of 170 ohms is obtained.
Example 6:
preparation of support 1: weighing 50 kg of alumina powder with the average particle size of 3 microns, 4.6 kg of kaolin, 0.83 kg of calcium carbonate, 2.0 kg of starch and 2.6 kg of methyl cellulose, putting the mixture into a mixer to be uniformly mixed, adding 15 kg of water and 2.7 kg of vegetable oil to be uniformly stirred, putting the mixture into a vacuum pug mill to be milled into compact plastic mud segments, ageing the compact plastic mud segments for 48 hours, putting the compact plastic mud segments into a vacuum extruder to be extruded and formed into porous flat ceramic membrane support body blanks, drying the porous flat ceramic membrane support body blanks, putting the porous flat ceramic membrane support body blanks into a kiln to be baked at 1350 ℃ for 2 hours, and taking the porous flat ceramic membrane support body out of the kiln.
Preparing a coating liquid of doped titanium oxide:
(1) mixing 300mL of ethanol with 700mL of deionized water, adding 0.01mol of hydrochloric acid into the ethanol water, and stirring for 30 minutes to obtain a mixed solution of hydrochloric acid, absolute ethyl alcohol and deionized water; dissolving 1.2mol of titanium tetrachloride in a mixed solution of hydrochloric acid, absolute ethyl alcohol and deionized water, and sealing and uniformly stirring to obtain a solution A for later use.
(2) Adding 1.0mol of oxalic acid into 1.0L of deionized water, stirring uniformly, adding 0.3mol of niobium hydroxide, and dissolving in oxalic acid aqueous solution to obtain solution B for later use.
(3) And (3) adding 200mL of the solution B obtained in the step (2) into 1.0L of the solution A obtained in the step (1), and mixing to obtain the doped titanium oxide coating solution.
Preparation of the electrothermal ceramic filter membrane 2: the silicon carbide ceramic flat membrane with the specification of 100mm multiplied by 500mm multiplied by 3mm and the middle transition membrane layer is vertically placed in a muffle furnace, the furnace is heated to 550 ℃, 75 g of doped titanium oxide sol prepared by the preparation process is sprayed into the furnace from a furnace door, after the composition of the sol is decomposed, a conductive titanium oxide membrane layer is generated on the surface of the middle transition membrane layer on one side, the other side is changed, 75 g of doped titanium oxide sol prepared by the preparation process is sprayed, a conductive titanium oxide membrane layer is generated on the surface of the middle transition membrane layer on the other side, and low-temperature silver electrodes are coated on two ends of the ceramic membrane after cooling, so that the electrothermal ceramic filter membrane with the resistance value of 120 ohms is obtained.
Example 7:
preparation of support 1: weighing 50 kg of silicon carbide powder with the average particle size of 25 microns, 3.3 kg of kaolin and 2.1 kg of methylcellulose, putting the silicon carbide powder, the kaolin and the methylcellulose into a mixer, uniformly mixing, adding 12 kg of water and 2.0 kg of vegetable oil, uniformly stirring, putting the mixture into a vacuum pug mill, milling into compact plastic pug segments, aging for 48 hours, putting the mixture into a vacuum extruder, extruding and forming into a porous flat ceramic membrane support body blank, drying, putting the blank into a kiln, keeping the temperature for 2 hours at 1350 ℃, firing, cooling and taking the blank out of the kiln to obtain the silicon carbide ceramic support body.
Preparation of the intermediate transition film layer 4: weighing 10 kg of silicon carbide powder with the average particle size of 3 microns, 1.2 kg of kaolin, 40 g of methylcellulose, 6.9 kg of water and a proper amount of water reducing agent, putting the silicon carbide powder, the kaolin, the methylcellulose, the water and the water reducing agent into a ball mill, performing ball milling for 2 hours, discharging slurry, adding a defoaming agent to remove bubbles, coating the slurry on the surface required by a silicon carbide support body in a dipping manner, drying, putting the silicon carbide support body into a kiln 1300 ℃, performing heat preservation for 1 hour, firing, cooling and discharging the silicon carbide support body out of the kiln to obtain the silicon carbide.
Preparing a coating liquid of doped titanium oxide:
(1) mixing 500mL of ethanol with 500mL of deionized water, adding 0.01mol of hydrochloric acid into the ethanol water, and stirring for 30 minutes to obtain a mixed solution of hydrochloric acid, absolute ethyl alcohol and deionized water; dissolving 1.5mol of titanium tetrachloride in a mixed solution of hydrochloric acid, absolute ethyl alcohol and deionized water, and sealing and uniformly stirring to obtain a solution A for later use.
(2) Adding 1.0mol of oxalic acid into 1.0L of deionized water, stirring uniformly, adding 0.15mol of niobium hydroxide, and dissolving in oxalic acid aqueous solution to obtain solution B for later use.
(3) And (3) adding 100mL of the solution B obtained in the step (2) into 1.0L of the solution A obtained in the step (1), and mixing to obtain the doped titanium oxide coating solution.
Preparation of the electrothermal ceramic filter membrane 2: the silicon carbide ceramic flat membrane with the specification of 100mm multiplied by 500mm multiplied by 3mm and the middle transition membrane layer is vertically placed in a muffle furnace, the furnace is heated to 550 ℃, 75 g of doped titanium oxide sol prepared by the preparation process is sprayed into the furnace from a furnace door, after the composition of the sol is decomposed, a conductive titanium oxide membrane layer is generated on the surface of the middle transition membrane layer on one side, the other side is changed, 75 g of doped titanium oxide sol prepared by the preparation process is sprayed, a conductive titanium oxide membrane layer is generated on the surface of the middle transition membrane layer on the other side, and low-temperature silver electrodes are coated on two ends of the ceramic membrane after cooling, so that the electrothermal ceramic filter membrane with the resistance value of 120 ohms is obtained.
Example 8:
preparation of support 1: weighing 50 kg of titanium oxide powder with the average particle size of 30 microns, 0.2 kg of corundum powder with the average particle size of 10 microns, 1.0 kg of kaolin, 0.3 kg of calcium carbonate powder, 4.3 kg of starch and 2.7 kg of methyl cellulose, putting the mixture into a mixer, uniformly mixing, adding 19 kg of water and 2.6 kg of vegetable oil, uniformly stirring, putting the mixture into a vacuum pug mill, refining into compact plastic pug segments, aging for 24 hours, putting the compact plastic pug mill into a vacuum extruder, extruding and forming into a porous flat ceramic membrane support body blank, drying, putting the blank into a kiln, keeping the temperature at 1250 ℃ for 2 hours, firing, cooling, and taking the blank out of the kiln to obtain the titanium oxide ceramic support body.
Preparation of the intermediate transition film layer 4: weighing 10 kg of titanium oxide powder with the average particle size of 0.5 micron, 95 g of calcium carbonate powder, 250 g of bentonite, 60 g of methyl cellulose, 26.8 kg of water and a proper amount of water reducing agent, putting the mixture into a ball mill for ball milling for 1 hour, discharging the slurry, adding a defoaming agent to remove bubbles, spraying the slurry on the surface required by the titanium oxide ceramic support body by ultrasonic waves, drying, putting the slurry into a kiln for 1150 ℃ and keeping the temperature for 1 hour for firing, cooling and taking the slurry out of the kiln to obtain the titanium oxide ceramic flat membrane with the intermediate transition membrane layer.
Preparing a coating liquid of doped titanium oxide:
(1) mixing 500mL of ethanol with 500mL of deionized water, adding 1.0mol of oxalic acid in the ethanol water, and stirring for 30 minutes to obtain a mixed solution of oxalic acid, absolute ethanol and deionized water; and dissolving 0.5mol of tetrabutyl titanate in the mixed solution of oxalic acid, absolute ethyl alcohol and deionized water, and sealing and uniformly stirring to obtain a solution A for later use.
(2) Adding 1.0mol of oxalic acid into 1.0L of deionized water, stirring uniformly, adding 0.5mol of niobium hydroxide, and dissolving in oxalic acid aqueous solution to obtain solution B for later use.
(3) And (3) adding 100mL of the solution B obtained in the step (2) into 1.0L of the solution A obtained in the step (1), and mixing to obtain the doped titanium oxide coating solution.
Preparation of the electrothermal ceramic filter membrane 2: the titanium oxide ceramic flat membrane with the specification of 100mm multiplied by 500mm multiplied by 3mm and the intermediate transition membrane layer is horizontally placed in a muffle furnace, the muffle furnace is heated to 550 ℃, the total amount of doped titanium oxide sol prepared by the preparation process is sprayed into the furnace from the top of the furnace for a plurality of times, the composition of the sol is decomposed, a conductive titanium oxide membrane layer is generated on the surface of the membrane, and after one surface is sprayed, the other surface is sprayed. And (3) thermally spraying metal aluminum electrodes at two ends of the ceramic membrane after cooling, and obtaining a flat electrothermal ceramic filter membrane with the resistance value of 120 ohms after cooling.
Example 9:
preparation of support 1: weighing 50 kg of quartz powder with the average particle size of 20 microns, 3.3 kg of kaolin, 2.6 kg of glass powder, 2.8 kg of starch and 2.0 kg of methyl cellulose, putting the mixture into a mixer to be uniformly mixed, adding 11 kg of water and 2.2 kg of vegetable oil to be uniformly stirred, putting the mixture into a vacuum pug mill to be refined into compact plastic mud sections, ageing the compact plastic mud sections for 24 hours, putting the compact plastic mud sections into a vacuum extruder to be extruded and formed into porous flat ceramic membrane support body blanks, drying the porous flat ceramic membrane support body blanks, putting the porous flat ceramic membrane support body blanks into a kiln to be subjected to heat preservation at 1100 ℃ for 2 hours, and taking the porous flat ceramic membrane support bodies.
Preparation of the intermediate transition film layer 4: weighing 10 kg of quartz powder with the average particle size of 0.5 micron, 630 g of 0.3 micron glass powder, 0.9 kg of kaolin, 20 g of methyl cellulose, 36.8 kg of water and a proper amount of water reducing agent, putting the mixture into a ball mill, performing ball milling for 3 hours, discharging slurry, adding a defoaming agent to remove bubbles, spraying the slurry on the surface required by a quartz support body by ultrasonic atomization, drying, putting the quartz support body into a kiln, performing heat preservation at 1050 ℃ for 1 hour, firing, cooling, and taking the quartz support body out of the kiln to obtain the quartz ceramic flat membrane with the intermediate transition membrane layer.
Preparing a doped zinc oxide coating liquid: dissolving 0.01mol of zinc acetate and 0.0025mol of aluminum trichloride in 1.0L of deionized water, sealing and stirring uniformly for about 30 minutes, adding 30mL of ethanol and 5mL of hydrochloric acid, and standing to obtain the doped zinc oxide coating liquid.
Preparation of the electrothermal ceramic filter membrane 2: the quartz ceramic flat membrane with the specification of 100mm multiplied by 500mm multiplied by 3mm and the middle transition membrane layer is vertically placed in a muffle furnace, the temperature is heated to 750 ℃, 80 g of doped zinc oxide sol prepared by the preparation process is sprayed into the furnace from a furnace door, the composition of the sol is decomposed, a conductive zinc oxide membrane layer is generated on the surface of the middle transition membrane layer on one side, the other side is changed, 80 g of doped zinc oxide sol prepared by the preparation process is sprayed, a conductive zinc oxide membrane layer is generated on the surface of the middle transition membrane layer on the other side, high-temperature silver-zinc electrodes are coated on two ends of the ceramic membrane after cooling, and the electric heating ceramic filter membrane with the resistance value of 650 ohms is obtained after the electrodes are baked at 600 ℃.
Example 10:
preparation of support 1: weighing 50 kg of zirconia powder with the average particle size of 10 microns, 1.5 kg of yttrium oxide, 1.0 kg of kaolin, 60 g of lanthanum oxide, 72 g of cerium oxide, 4.6 kg of starch and 2.0 kg of methyl cellulose, putting the materials into a mixer, uniformly mixing, adding 19 kg of water and 2.3 kg of vegetable oil, uniformly stirring, putting the mixture into a vacuum pug mill, refining into a compact plastic pug segment, ageing for 72 hours, putting the compact plastic pug segment into a vacuum extruder, extruding and forming into a single-hole tubular ceramic membrane support body blank with the diameter of 20mm, drying, putting the blank into a kiln, keeping the temperature at 1350 ℃ for 2 hours, firing, cooling, and taking the blank out of the kiln to obtain the zirconia ceramic support body.
Preparation of the intermediate transition film layer 4: weighing 10 kg of zirconia powder with the average particle size of 0.3 micron, 400 g of yttrium oxide, 0.2 kg of kaolin, 60 g of methyl cellulose, 16.8 kg of water and a proper amount of water reducing agent, putting the mixture into a ball mill for ball milling for 2 hours, discharging the slurry, adding a defoaming agent to remove bubbles, coating the slurry on the surface required by a zirconia support body in a dipping way, drying, putting the slurry into a kiln at 1250 ℃, preserving the heat for 1 hour, firing the slurry, cooling and discharging the slurry out of the kiln to obtain the zirconia ceramic tubular membrane with the intermediate transition membrane layer.
Preparing a doped zinc oxide coating liquid: dissolving 1.5mol of zinc acetate and 0.375mol of aluminum trichloride in 1.0L of deionized water, sealing and stirring uniformly for about 30 minutes, adding 130mL of ethanol and 35mL of hydrochloric acid, and standing to obtain the doped zinc oxide coating liquid.
Preparation of the electrothermal ceramic filter membrane 2: the zirconia ceramic tubular membrane with (phi 20 mm-phi 16mm) multiplied by 300mm and an intermediate transition membrane layer is transversely placed in a muffle furnace, the tube is continuously rotated, the tube is heated to 700 ℃, 20 grams of doped zinc oxide sol prepared by the preparation process is sprayed into the furnace from the top of the furnace for multiple times, conductive zinc oxide membrane layers are generated on the outer surfaces of the membrane tubes after the composition of the sol is decomposed, high-temperature silver electrodes are coated on the two ends of the ceramic membrane after cooling, and the tubular electrothermal ceramic filter membrane with the resistance value of 30 ohms is obtained after the electrodes are baked at 700 ℃.
Example 11:
preparation of support 1: weighing 40 kg of quartz powder with the average particle size of 30 microns, 10 kg of corundum powder with the average particle size of 10 microns, 2.0 kg of kaolin, 0.5 kg of borax powder, 4.6 kg of starch and 2.0 kg of methylcellulose, adding 19 kg of water and 2.0 kg of vegetable oil after uniformly mixing in a mixer, putting in a vacuum pug mill to be refined into a compact plastic pug segment, ageing for 48 hours, putting in a vacuum extruder to be extruded and formed into a porous tubular ceramic membrane support body blank with (phi 40 mm-phi 8mm multiplied by 9 holes), drying, putting in a kiln, keeping the temperature for 2 hours at 1200 ℃, sintering, cooling and taking out of the kiln to obtain the quartz-corundum ceramic support body.
Preparation of the intermediate transition film layer 4: weighing 10 kg of quartz powder with the average particle size of 0.5 micron, 120 g of borax powder, 250 g of kaolin, 60 g of methyl cellulose, 16.8 kg of water and a proper amount of water reducing agent, putting the mixture into a ball mill for ball milling for 1 hour, discharging slurry, adding a defoaming agent to remove bubbles, coating the slurry on the surface required by the quartz-corundum ceramic support body in a dipping way, drying, putting the mixture into a kiln for 1100 ℃, preserving the heat for 1 hour, firing, cooling and discharging the product out of the kiln to obtain the quartz-corundum ceramic tubular membrane with the intermediate transition membrane layer.
Preparing a doped zinc oxide coating liquid: dissolving 1.0mol of zinc chloride and 0.111mol of aluminum trichloride in 1.0L of deionized water, sealing and stirring uniformly for about 30 minutes, adding 100mL of ethanol and 10mL of hydrochloric acid, and standing to obtain the doped zinc oxide coating liquid.
Preparation of the electrothermal ceramic filter membrane 2: the quartz-corundum ceramic tubular membrane with (phi 40 mm-phi 8 mm-phi 9 mm) x 300mm and an intermediate transition membrane layer is transversely placed in a muffle furnace, the tube is continuously rotated, the tube is heated to 500 ℃, 20 g of doped zinc oxide sol prepared by the preparation process is sprayed into the furnace from the top of the furnace for multiple times, after the composition of the sol is decomposed, a conductive zinc oxide membrane layer is generated on the outer surface of the membrane tube, high-temperature silver electrodes are coated on the two ends of the ceramic membrane after cooling, and after the electrodes are baked at 700 ℃, the tubular electrothermal ceramic filter membrane with the resistance value of 380 ohm is obtained.
Example 12:
preparation of support 1: weighing 50 kg of alumina powder with the average particle size of 30 microns, 4.6 kg of kaolin, 0.43 kg of calcite powder, 2.0 kg of starch and 2.6 kg of methylcellulose, putting the mixture into a mixer, uniformly mixing, adding 15 kg of water and 2.5 kg of vegetable oil, uniformly stirring, putting the mixture into a vacuum pug mill, milling into compact plastic mud segments, ageing for 48 hours, putting the compact plastic mud segments into a vacuum extruder, extruding and forming into porous flat ceramic membrane support body blanks, drying, putting the porous flat ceramic membrane support body blanks into a kiln, keeping the temperature of 1400 ℃ for 2 hours, sintering, cooling, and taking the porous flat ceramic membrane support bodies out of the kiln to obtain the alumina ceramic support body.
Preparation of the intermediate transition film layer 4: weighing 10 kg of alumina powder with the average particle size of 3 microns, 1.8 kg of kaolin, 35 g of methylcellulose and 6.6 kg of water, putting the alumina powder, 1.8 kg of kaolin, 35 g of methylcellulose and 6.6 kg of water into a ball mill, ball-milling for 2 hours, discharging slurry, adding a defoaming agent to remove bubbles, coating the slurry on the surface required by an alumina support body in a dipping way, drying, putting the alumina support body into a kiln for 1350 ℃, preserving heat for 1 hour, firing, cooling and discharging the alumina support body out of the kiln to obtain the alumina ceramic flat membrane with the intermediate.
Preparing a doped tin oxide-indium oxide coating liquid: dissolving 1.425mol of stannic chloride and 0.075mol of indium trichloride in 1.0L of deionized water, hermetically stirring the solution uniformly for about 30 minutes, then adding 100mL of ethanol and 18mL of hydrofluoric acid, and standing the solution to obtain the doped stannic oxide-indium oxide coating solution.
Preparation of the electrothermal ceramic filter membrane 2: the alumina ceramic flat membrane with the specification of 100mm multiplied by 500mm multiplied by 3mm and the middle transition membrane layer is flatly placed in a muffle furnace, the temperature is heated to 520 ℃, 20 g of doped indium tin oxide sol prepared by the preparation process is sprayed from the furnace top to the surface close to the membrane in the furnace, after the composition of the sol is decomposed, a conductive indium tin oxide membrane layer is generated on the surface of the middle transition membrane layer on one side, the other side is changed, 20 g of doped indium tin oxide sol prepared by the preparation process is sprayed, a conductive indium tin oxide membrane layer is generated on the surface of the middle transition membrane layer on the other side, low-temperature silver electrodes are coated on the two ends of the ceramic membrane after cooling, and after drying at 200 ℃, the electrothermal ceramic filter membrane with the resistance value of 35.
Example 13:
preparing a doped tin oxide-indium oxide coating liquid: dissolving 0.75mol of stannic chloride and 0.25mol of indium trichloride in 1.0L of deionized water, hermetically stirring uniformly for about 30 minutes, then adding 50mL of ethanol and 6mL of hydrofluoric acid, and standing to obtain the doped stannic oxide-indium oxide coating liquid.
Preparation of the electrothermal ceramic filter membrane 2: the alumina ceramic flat membrane with the specification of 100mm multiplied by 500mm multiplied by 3mm and the middle transition membrane layer is flatly placed in a muffle furnace, the furnace is heated to 500 ℃, 50 g of doped indium tin oxide sol prepared by the preparation process is sprayed from the furnace top to the surface close to the membrane in the furnace, after the composition of the sol is decomposed, a conductive indium tin oxide membrane layer is generated on the surface of the middle transition membrane layer on one side, the other side is changed, 50 g of doped indium tin oxide sol prepared by the preparation process is sprayed, a conductive indium tin oxide membrane layer is generated on the surface of the middle transition membrane layer on the other side, low-temperature silver electrodes are coated on the two ends of the ceramic membrane after cooling, and after drying at 200 ℃, the electrothermal ceramic filter membrane with the resistance value of 75.
The above description is only exemplary of the invention, and any modification, equivalent replacement, and improvement made within the spirit and scope of the present invention should be considered within the scope of the present invention.
Claims (10)
1. The electrothermal ceramic filter membrane comprises a support body (1) and is characterized in that an electrothermal filter membrane layer (2) is arranged on the surface of the support body (1), and an electrode (3) is arranged on the surface of the electrothermal filter membrane layer (2).
2. An electrothermal ceramic filter membrane according to claim 1, wherein an intermediate filter membrane layer (4) is further provided between the electrothermal filter membrane layer (2) and the support body (1), and the number of the intermediate filter membrane layers (4) is one or more.
3. An electrothermal ceramic filter membrane according to claim 1, which is any one of a porous flat plate-like, a single-hole tubular, a porous tubular, a hollow circular plate-like and a hollow circular sheet-like.
4. A method for preparing an electrothermal ceramic filter membrane according to claim 1, comprising the steps of:
(1) placing the support body (1) in a space, heating, introducing atomized coating liquid to carry out pyrolysis reaction deposition, and generating an electrothermal filter film layer (2) on the surface of the support body (1);
(2) coating electrode slurry on the electrothermal filter membrane layer (2) and baking or burning the electrode (3) to obtain the electrothermal ceramic filter membrane, or thermally spraying the electrode (3) on the electrothermal filter membrane layer (2) to obtain the electrothermal ceramic filter membrane.
5. The preparation method of the electrothermal ceramic filter membrane according to claim 4, wherein the coating solution is a doped tin oxide sol, wherein the concentration of tin dichloride is 0.01-1.5 mol/L, the concentration of ammonium fluoride is 0.001-0.01 mol/L, and the molar ratio of tin to niobium in the doped tin oxide sol is as follows: 9.5: 0.5-9.99: 0.01.
6. The preparation method of the electrothermal ceramic filter membrane according to claim 4, wherein the coating solution is doped zinc oxide sol, wherein the molar ratio of zinc to aluminum in the doped zinc oxide sol is 8:2 to 9.9: 0.1.
7. The preparation method of the electrothermal ceramic filter membrane according to claim 4, wherein the coating solution is doped tin oxide-indium oxide sol, and the molar ratio of tin to indium in the doped tin oxide-indium oxide sol is 9.5: 0.5-0.5: 9.5.
8. The preparation method of the electrothermal ceramic filter membrane according to claim 4, wherein the coating solution is a doped titanium oxide sol, wherein the molar ratio of niobium to titanium in the niobium-doped titanium oxide sol is 0.01: 1-0.1: 1.
9. The method for preparing an electrothermal ceramic filter membrane according to claim 4, wherein in the step (1), the temperature for deposition by pyrolysis reaction is 500 to 750 ℃.
10. The method for preparing an electrothermal ceramic filter membrane according to claim 4, wherein the coating liquid is atomized by any one of pressure atomization, compressed air atomization and ultrasonic atomization.
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Denomination of invention: A type of electric heating ceramic filtration membrane and its preparation method Granted publication date: 20210928 Pledgee: China CITIC Bank Nanning Branch Pledgor: GUANGXI BIQINGYUAN ENVIRONMENTAL PROTECTION INVESTMENT Co.,Ltd. Registration number: Y2024450000018 |