CN116835996A - Preparation method of low-temperature sintered anti-pollution ceramic membrane - Google Patents
Preparation method of low-temperature sintered anti-pollution ceramic membrane Download PDFInfo
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- CN116835996A CN116835996A CN202310803741.2A CN202310803741A CN116835996A CN 116835996 A CN116835996 A CN 116835996A CN 202310803741 A CN202310803741 A CN 202310803741A CN 116835996 A CN116835996 A CN 116835996A
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- 239000012528 membrane Substances 0.000 title claims abstract description 111
- 239000000919 ceramic Substances 0.000 title claims abstract description 91
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 239000000843 powder Substances 0.000 claims abstract description 75
- 239000002002 slurry Substances 0.000 claims abstract description 32
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 29
- 238000009766 low-temperature sintering Methods 0.000 claims abstract description 24
- 238000000498 ball milling Methods 0.000 claims abstract description 23
- 229920000592 inorganic polymer Polymers 0.000 claims abstract description 23
- 238000002156 mixing Methods 0.000 claims abstract description 22
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 21
- 239000002131 composite material Substances 0.000 claims abstract description 20
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 16
- 239000002585 base Substances 0.000 claims abstract description 15
- 239000012752 auxiliary agent Substances 0.000 claims abstract description 13
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims abstract description 12
- 239000011230 binding agent Substances 0.000 claims abstract description 12
- 239000003513 alkali Substances 0.000 claims abstract description 10
- 239000002270 dispersing agent Substances 0.000 claims abstract description 9
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 claims abstract description 8
- 230000005284 excitation Effects 0.000 claims abstract description 8
- 238000010304 firing Methods 0.000 claims abstract description 8
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000004088 foaming agent Substances 0.000 claims abstract description 6
- 238000010438 heat treatment Methods 0.000 claims abstract description 6
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 claims abstract description 6
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000011780 sodium chloride Substances 0.000 claims abstract description 6
- 238000005507 spraying Methods 0.000 claims abstract description 5
- 239000002518 antifoaming agent Substances 0.000 claims abstract description 4
- 239000000203 mixture Substances 0.000 claims description 19
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 15
- 238000001035 drying Methods 0.000 claims description 11
- 238000000034 method Methods 0.000 claims description 11
- 238000000227 grinding Methods 0.000 claims description 8
- -1 polytetrafluoroethylene Polymers 0.000 claims description 8
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 8
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 8
- 238000001354 calcination Methods 0.000 claims description 7
- 239000000314 lubricant Substances 0.000 claims description 7
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 5
- 230000032683 aging Effects 0.000 claims description 5
- 239000000835 fiber Substances 0.000 claims description 5
- 238000007873 sieving Methods 0.000 claims description 5
- 229920001353 Dextrin Polymers 0.000 claims description 4
- 239000004375 Dextrin Substances 0.000 claims description 4
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 4
- 238000004140 cleaning Methods 0.000 claims description 4
- 239000011248 coating agent Substances 0.000 claims description 4
- 238000000576 coating method Methods 0.000 claims description 4
- 235000019425 dextrin Nutrition 0.000 claims description 4
- 239000001866 hydroxypropyl methyl cellulose Substances 0.000 claims description 4
- 229920003088 hydroxypropyl methyl cellulose Polymers 0.000 claims description 4
- 235000010979 hydroxypropyl methyl cellulose Nutrition 0.000 claims description 4
- 238000004898 kneading Methods 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 claims description 4
- 238000010907 mechanical stirring Methods 0.000 claims description 4
- 239000011734 sodium Substances 0.000 claims description 4
- 229910052708 sodium Inorganic materials 0.000 claims description 4
- 239000007921 spray Substances 0.000 claims description 4
- 238000003756 stirring Methods 0.000 claims description 4
- 239000004952 Polyamide Substances 0.000 claims description 3
- 230000003373 anti-fouling effect Effects 0.000 claims description 3
- 239000005457 ice water Substances 0.000 claims description 3
- 229920002647 polyamide Polymers 0.000 claims description 3
- 229920005646 polycarboxylate Polymers 0.000 claims description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 2
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 2
- 229920002472 Starch Polymers 0.000 claims description 2
- 229960003943 hypromellose Drugs 0.000 claims description 2
- 229920000609 methyl cellulose Polymers 0.000 claims description 2
- 239000001923 methylcellulose Substances 0.000 claims description 2
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 2
- 239000008107 starch Substances 0.000 claims description 2
- 235000019698 starch Nutrition 0.000 claims description 2
- 238000001914 filtration Methods 0.000 abstract description 7
- 230000000694 effects Effects 0.000 abstract description 6
- 238000005245 sintering Methods 0.000 abstract description 2
- 239000000243 solution Substances 0.000 description 12
- 238000000926 separation method Methods 0.000 description 9
- 230000004907 flux Effects 0.000 description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 239000002351 wastewater Substances 0.000 description 4
- QJZYHAIUNVAGQP-UHFFFAOYSA-N 3-nitrobicyclo[2.2.1]hept-5-ene-2,3-dicarboxylic acid Chemical compound C1C2C=CC1C(C(=O)O)C2(C(O)=O)[N+]([O-])=O QJZYHAIUNVAGQP-UHFFFAOYSA-N 0.000 description 3
- 239000000654 additive Substances 0.000 description 3
- 230000000996 additive effect Effects 0.000 description 3
- 238000011001 backwashing Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000003344 environmental pollutant Substances 0.000 description 3
- 239000004021 humic acid Substances 0.000 description 3
- 231100000719 pollutant Toxicity 0.000 description 3
- 239000011148 porous material Substances 0.000 description 3
- 238000005406 washing Methods 0.000 description 3
- 229910021536 Zeolite Inorganic materials 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 239000003929 acidic solution Substances 0.000 description 2
- 239000012670 alkaline solution Substances 0.000 description 2
- 230000002238 attenuated effect Effects 0.000 description 2
- 238000005530 etching Methods 0.000 description 2
- UFVKGYZPFZQRLF-UHFFFAOYSA-N hydroxypropyl methyl cellulose Chemical compound OC1C(O)C(OC)OC(CO)C1OC1C(O)C(O)C(OC2C(C(O)C(OC3C(C(O)C(O)C(CO)O3)O)C(CO)O2)O)C(CO)O1 UFVKGYZPFZQRLF-UHFFFAOYSA-N 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 238000013001 point bending Methods 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000004065 wastewater treatment Methods 0.000 description 2
- 239000010457 zeolite Substances 0.000 description 2
- 241000195493 Cryptophyta Species 0.000 description 1
- 229910018068 Li 2 O Inorganic materials 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 239000013530 defoamer Substances 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 239000010840 domestic wastewater Substances 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 238000005187 foaming Methods 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000010287 polarization Effects 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000000518 rheometry Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000010918 textile wastewater Substances 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
Classifications
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- 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
-
- 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
- B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
- B01D67/0039—Inorganic membrane manufacture
- B01D67/0076—Pretreatment of inorganic membrane material prior to membrane formation, e.g. coating of metal powder
-
- 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
- B01D69/02—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor characterised by their properties
-
- 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
- B01D69/12—Composite membranes; Ultra-thin membranes
-
- 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
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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
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/10—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on aluminium oxide
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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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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/63—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B using additives specially adapted for forming the products, e.g.. binder binders
- C04B35/632—Organic additives
- C04B35/634—Polymers
- C04B35/63404—Polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds
- C04B35/63416—Polyvinylalcohols [PVA]; Polyvinylacetates
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- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/63—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B using additives specially adapted for forming the products, e.g.. binder binders
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- C04B38/06—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof by burning-out added substances by burning natural expanding materials or by sublimating or melting out added substances
- C04B38/063—Preparing or treating the raw materials individually or as batches
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- C04B38/06—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof by burning-out added substances by burning natural expanding materials or by sublimating or melting out added substances
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- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/009—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone characterised by the material treated
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- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
- C04B41/52—Multiple coating or impregnating multiple coating or impregnating with the same composition or with compositions only differing in the concentration of the constituents, is classified as single coating or impregnation
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- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
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- Separation Using Semi-Permeable Membranes (AREA)
Abstract
The invention discloses a preparation method of a low-temperature sintered anti-pollution ceramic membrane, which aims to solve the problem that the existing ceramic membrane is high in sintering temperature and the anti-pollution capability is required to be improved. The preparation method comprises the following steps: 1. preparing a composite low-temperature sintering auxiliary agent; 2. preparing a ceramic membrane base membrane; 3. adding zeolite particles, alumina powder and silicon dioxide powder into a ball mill, adding NaCl solution, and performing ball milling treatment to obtain anti-pollution powder; 4. uniformly mixing water, anti-pollution powder, a composite low-temperature sintering auxiliary agent, a dispersing agent, a slurry rheological agent and a defoaming agent to prepare middle-layer slurry, and spraying the middle-layer slurry onto a ceramic membrane base membrane; 5. mixing metakaolin, anti-pollution powder, a foaming agent, silica sol and alkali excitation solution to prepare inorganic polymer slurry; 6. the inorganic polymer slurry is coated on the anti-pollution ceramic film for heat treatment. The invention optimizes the low-temperature binder, reduces the firing temperature, combines the inorganic polymer layer on the base film, and improves the filtering effect of the separating layer.
Description
Technical Field
The invention relates to a preparation method of a ceramic membrane for wastewater treatment.
Background
Under the condition that the membrane separation technology has the advantages of the traditional water treatment technology, the separation, concentration and purification of different components can be realized, and the membrane separation technology has the characteristics of good separation effect, flexible and changeable separation process, simple operation, compact equipment and the like. Ceramic membranes possess a number of excellent characteristics such as good chemical properties, reusability, good biological resistance, long service life, high mechanical strength, etc., so that ceramic membranes are often active in the fields of treatment of oily wastewater, treatment of textile wastewater, extraction of chemical wastewater, purification of domestic wastewater, etc. However, in the practical production process, ceramic membranes are limited to large-scale and wide application due to the problem of manufacturing cost, and all membrane products have reduced service life due to membrane pollution, so that the expected targets are not achieved. In specific applications, the separation efficiency is reduced due to concentration polarization and other phenomena, and membrane pollution and other conditions cannot be ignored. The ceramic membrane is modified by a special method to have different functions or be coupled with other treatment means, so that the treatment cost of the whole process is reduced. As algae, organic matters, colloid and other substances in the water body have negative electricity, the electrostatic effect can be used as a means for relieving membrane pollution.
Disclosure of Invention
The invention provides a preparation method of a low-temperature sintering anti-pollution ceramic membrane, which aims to solve the problem that the mechanical strength and the anti-pollution capability of the existing ceramic membrane are required to be improved.
The preparation method of the low-temperature sintered anti-pollution ceramic membrane is realized according to the following steps:
1. the mass ratio is 1:1:4 Li is 2 O、B 2 O 3 And SiO 2 Placing the powder into a polytetrafluoroethylene ball milling tank, and grinding for 3.5-4.5 h to obtain powder A; the mass ratio is 1:0.8 CuO and H 3 BO 3 Grinding in a polytetrafluoroethylene ball milling tank for 3.5-4.5 h to obtain powder B; the mass ratio of the powder A to the powder B is (1.8-3): 1, ball milling for 1-2 hours after mixing to obtain a composite low-temperature sintering aid;
2. placing alumina powder, a composite low-temperature sintering auxiliary agent, a pore-forming agent and a binder into a planetary ball mill, ball-milling and mixing at a speed of 400-500 r/min, sieving to obtain a fine powder mixture, placing the fine powder mixture into a mixer, adding water and a lubricant, mixing, kneading to form a green body, repeatedly pugging the green body by a vacuum pugging machine, standing and ageing to obtain a mixed pug, and calcining to obtain a ceramic membrane base membrane;
3. according to the mass ratio of (3-5): (1-2): (1-2) adding zeolite particles, alumina powder and silicon dioxide powder into a ball mill, adding NaCl solution with the concentration of 2-3 mol/L, performing wet ball milling treatment at the speed of 600-800 r/min, and cleaning and drying to obtain anti-pollution powder;
4. uniformly mixing water, (part of) anti-pollution powder, a composite low-temperature sintering auxiliary agent, a dispersing agent, a slurry rheological agent and a defoaming agent, mechanically stirring for 2-2.5 hours to obtain middle-layer slurry, spraying the middle-layer slurry onto a ceramic membrane base membrane by using a spray gun, drying, and firing at 850-950 ℃ to obtain an anti-pollution ceramic membrane;
5. in ice waterUnder the bath condition, metakaolin, (another part of) anti-pollution powder and H 2 O 2 Mixing a foaming agent, silica sol and alkali excitation solution, and carrying out ultrasonic and mechanical stirring uniformly to obtain inorganic polymer slurry;
6. immersing the anti-pollution ceramic membrane in water for 6-8 h, coating inorganic polymer slurry on the immersed anti-pollution ceramic membrane, and performing heat treatment at 100-180 ℃ for 1-2 h to obtain a low-temperature sintered anti-pollution ceramic membrane;
wherein in the second step, the alumina powder is 90-95 parts by weight (additive amount), the composite low-temperature sintering auxiliary agent is 5-10 parts by weight, the pore-forming agent is 10-20 parts by weight, the binder is 5-20 parts by weight, and the water is 5-10 parts by weight.
The invention is made of Li 2 O、B 2 O 3 And SiO 2 Composition A powder, cuO and H 3 BO 3 And (3) forming powder B, controlling the proportion of the powder A and the powder B to form a combined sintering aid, and reducing the firing temperature of the ceramic membrane by using the composite low-temperature sintering aid. The zeolite particles in the anti-pollution powder are subjected to wet ball milling treatment by using NaCl solution, so that the zeolite surface has more negative charges, and the membrane pollution is slowed down by using the effect of electrostatic repulsion. The middle layer slurry is sprayed on the ceramic membrane base membrane, the middle layer is used as a transition layer between the ceramic membrane base membrane and the inorganic polymer layer, then the inorganic polymer slurry is coated on the immersed anti-pollution ceramic membrane, the inorganic polymer layer is formed on the ceramic membrane after heat treatment, the inorganic polymer forms a three-dimensional porous structure after foaming, the anti-pollution powder is doped on the pore channel (wall) to be used as a supporting body, the alumina powder and the silica powder can also be used as an aluminum source and a silicon source respectively, and the inorganic polymer layer has better pressure-bearing property and mechanical property, better water-flow impact resistance and improved flexural strength.
The preparation method of the low-temperature sintered anti-pollution ceramic membrane provided by the invention has the following beneficial effects:
1. the invention develops a low-temperature binder, which can reduce the firing temperature of a ceramic film to 850-950 ℃, and the firing temperature of the ceramic film commonly used at present is about 1400 ℃, thereby achieving the aim of reducing energy consumption and production cost.
2. The pollution-resistant ceramic membrane prepared by the invention has Zeta potential of-70 mV to-80 mV and pure water flux of 3500-5000L/(m) 2 h bar), the flexural strength reaches more than 40MPa, and the film performance is better.
3. According to the invention, the inorganic polymer layer is compounded on the ceramic membrane base membrane to serve as a separation layer, the inorganic polymer layer has high porosity, the porosity is more than 45%, the ceramic membrane base membrane is resistant to water flow, and is better in temperature resistance and acid and alkali corrosion resistance, and a three-dimensional multi-pore structure is formed by combining the pore structure of zeolite, so that the retention rate of pollutants is improved.
4. The pollution resistance of the pollution-resistant ceramic membrane prepared by the method is evaluated, the pollution-resistant ceramic membrane runs continuously under the condition of humic acid pollution, the flux decays to 40% and reaches a plateau period, and the pollution-resistant ceramic membrane can be recovered to about 90% after backwashing; the common ceramic membrane runs under the same condition, the flux is attenuated to below 20% to reach the plateau period, and the flux cannot be effectively recovered after backwashing.
Drawings
FIG. 1 is a photograph of a low temperature sintered anti-fouling ceramic membrane obtained in example one.
Detailed Description
The first embodiment is as follows: the preparation method of the low-temperature sintered anti-pollution ceramic membrane in the embodiment is realized according to the following steps:
1. the mass ratio is 1:1:4 Li is 2 O、B 2 O 3 And SiO 2 Placing the powder into a polytetrafluoroethylene ball milling tank, and grinding for 3.5-4.5 h to obtain powder A; the mass ratio is 1:0.8 CuO and H 3 BO 3 Grinding in a polytetrafluoroethylene ball milling tank for 3.5-4.5 h to obtain powder B; the mass ratio of the powder A to the powder B is (1.8-3): 1, ball milling for 1-2 hours after mixing to obtain a composite low-temperature sintering aid;
2. placing alumina powder, a composite low-temperature sintering auxiliary agent, a pore-forming agent and a binder into a planetary ball mill, ball-milling and mixing at a speed of 400-500 r/min, sieving to obtain a fine powder mixture, placing the fine powder mixture into a mixer, adding water and a lubricant, mixing, kneading to form a green body, repeatedly pugging the green body by a vacuum pugging machine, standing and ageing to obtain a mixed pug, and calcining to obtain a ceramic membrane base membrane;
3. according to the mass ratio of (3-5): (1-2): (1-2) adding zeolite particles, alumina powder and silicon dioxide powder into a ball mill, adding NaCl solution with the concentration of 2-3 mol/L, performing wet ball milling treatment at the speed of 600-800 r/min, and cleaning and drying to obtain anti-pollution powder;
4. uniformly mixing water, (part of) anti-pollution powder, a composite low-temperature sintering auxiliary agent, a dispersing agent, a slurry rheological agent and a defoaming agent, mechanically stirring for 2-2.5 hours to obtain middle-layer slurry, spraying the middle-layer slurry onto a ceramic membrane base membrane by using a spray gun, drying, and firing at 850-950 ℃ to obtain an anti-pollution ceramic membrane;
5. under the condition of ice-water bath, metakaolin (another part) of anti-pollution powder and H 2 O 2 Mixing a foaming agent, silica sol and alkali excitation solution, and carrying out ultrasonic and mechanical stirring uniformly to obtain inorganic polymer slurry;
6. immersing the anti-pollution ceramic membrane in water for 6-8 h, coating inorganic polymer slurry on the immersed anti-pollution ceramic membrane, and performing heat treatment at 100-180 ℃ for 1-2 h to obtain a low-temperature sintered anti-pollution ceramic membrane;
wherein in the second step, the alumina powder is 90-95 parts by weight (additive amount), the composite low-temperature sintering auxiliary agent is 5-10 parts by weight, the pore-forming agent is 10-20 parts by weight, the binder is 5-20 parts by weight, and the water is 5-10 parts by weight.
According to the embodiment, the low-temperature adhesive is prepared, and the negatively charged separation layer can be fired at a lower temperature on the ceramic membrane, so that the adhesion of the pollutants on the surface of the membrane and the deposition in the membrane holes are reduced by means of the interaction of the charges of the membrane and the charges of the pollutants based on the electrostatic action principle, the membrane pollution is slowed down, and the anti-pollution effect is achieved.
The second embodiment is as follows: the first difference between the present embodiment and the specific embodiment is that in the first step, the mass ratio of the powder a to the powder B is 2:1 are mixed and ball-milled for 1 to 1.5 hours.
And a third specific embodiment: the difference between the present embodiment and the first or second embodiment is that the pore-forming agent in the second step is yellow dextrin, starch or graphite powder.
The specific embodiment IV is as follows: the present embodiment differs from the first to third embodiments in that the binder in the second step is methylcellulose, polyvinyl alcohol, or sodium hypromellose.
Fifth embodiment: the difference between the present embodiment and the first to fourth embodiments is that the alumina powder in the second step (added amount) is 92.5 parts by mass, the composite low-temperature sintering aid is 7.5 parts by mass, the pore-forming agent is 15 parts by mass, the binder is 5 parts by mass, and the water is 10 parts by mass.
Specific embodiment six: the present embodiment differs from one of the first to fifth embodiments in that the calcination treatment is performed at a temperature of 900 to 950 ℃ for 2 to 3 hours in the second step.
Seventh embodiment: in the second step, the fine powder mixture and the alumina fibers are placed in a mixer, water and a lubricant are added, and the mixture is kneaded to form a green body.
In the embodiment, the alumina fiber is doped in the green body, so that the mechanical strength of the alumina fiber is high, and the flexural strength of the ceramic membrane is improved.
Eighth embodiment: the difference between the present embodiment and one of the first to seventh embodiments is that the wet ball milling treatment time in the third step is 1.5 to 3 hours.
Detailed description nine: this embodiment differs from one to eight embodiments in that the dispersant in step four is a polycarboxylate dispersant and the slurry rheology agent is a polyamide wax.
Detailed description ten: the present embodiment differs from one of the first to ninth embodiments in that the alkali-activated solution described in the fifth step is a NaOH solution.
Eleventh embodiment: this embodiment differs from the one to one tenth embodiments in that the apparent viscosity of the inorganic polymer slurry is controlled to 1000 to 2000pa·s in the fifth step.
This embodiment requires controlling the viscosity of the inorganic polymer slurry so that the inorganic polymer slurry is coated and the formed inorganic polymer acts as a separation layer.
Twelve specific embodiments: the embodiment is different from one to one tenth of the specific embodiments in that 30 to 40 parts of metakaolin, 8 to 15 parts of anti-pollution powder and 0.5 to 2 parts of H are mixed according to parts by mass in the fifth step 2 O 2 The foaming agent, 15-25 parts of silica sol and alkali excitation solution are mixed.
Embodiment one: the preparation method of the low-temperature sintered anti-pollution ceramic membrane is realized according to the following steps:
1. the mass ratio is 1:1:4 Li is 2 O、B 2 O 3 And SiO 2 Placing the powder into a polytetrafluoroethylene ball milling tank, and grinding for 3.5 hours to obtain powder A; the mass ratio is 1:0.8 CuO and H 3 BO 3 Putting the mixture into a polytetrafluoroethylene ball milling tank, and grinding the mixture for 3.5 hours to obtain powder B; the mass ratio of the powder A to the powder B is 2:1, ball milling for 1h after mixing to obtain a composite low-temperature sintering aid;
2. 92.5 parts of alumina powder (the grain size of the raw materials is 5 mu m), 7.5 parts of composite low-temperature sintering additive, 15 parts of yellow dextrin and 5 parts of hydroxypropyl methylcellulose sodium are put into a planetary ball mill according to parts by weight, ball-milling and mixing are carried out at the speed of 400r/min, and then sieving is carried out, the fine powder mixture is obtained, then the fine powder mixture is put into a mixer, 10 parts of water and 1.5 parts of lubricant are added, after mixing, pressing and kneading are carried out, green bodies are formed, the green bodies are repeatedly pugged by a vacuum pugging machine, mixed pug is obtained after standing and ageing, and ceramic membrane base membranes are obtained after calcining treatment for 2 hours at 900 ℃;
3. the mass ratio is 3:1:1.5 adding zeolite particles, alumina powder and silicon dioxide powder into a ball mill, adding NaCl solution with the concentration of 2mol/L, performing wet ball milling at the speed of 600r/min for 1h, and obtaining anti-pollution powder after cleaning and drying at 60 ℃;
4. uniformly mixing 60 parts of water, 60 parts of anti-pollution powder, 5 parts of composite low-temperature sintering auxiliary agent, 1 part of polycarboxylate dispersant, 1 part of polyamide wax and 0.2 part of NXZ defoamer according to parts by weight, mechanically stirring for 2 hours to obtain middle-layer slurry, spraying the middle-layer slurry onto a ceramic membrane base membrane by using a spray gun, drying, and firing at 900 ℃ for 40 minutes to obtain an anti-pollution ceramic membrane;
5. 30 parts of metakaolin, 12 parts of anti-pollution powder and 1.5 parts of H in parts by weight under the condition of ice water bath at 0 DEG C 2 O 2 Mixing a foaming agent, 20 parts of silica sol and an alkali excitation solution, wherein the alkali excitation solution is an NaOH solution, and the mass part of NaOH is 6 parts, and carrying out ultrasonic and mechanical stirring uniformly to obtain inorganic polymer slurry;
6. immersing the anti-pollution ceramic membrane in 50 ℃ water for 6 hours, coating inorganic polymer slurry on the immersed anti-pollution ceramic membrane, performing heat treatment at 100 ℃ for 1.5 hours, and finally washing and drying by deionized water to obtain the low-temperature sintered anti-pollution ceramic membrane, wherein the thickness of the ceramic membrane is 4mm.
The flexural strength of the low-temperature sintered anti-pollution ceramic film obtained by the test through the three-point bending test is 40.5MPa.
The surface potential of the low temperature sintered anti-pollution ceramic film of this example was measured using a solid surface Zeta potential analyzer. At ph=7, the Zeta potential of the low temperature sintered antipollution ceramic membrane was-75 mV.
The low-temperature sintered anti-pollution ceramic membrane of the embodiment is arranged in a filtering device, nitrogen is introduced into the filtering device to maintain the pressure difference of two sides of the ceramic membrane to be 0.01MPa, and the pure water permeation flux of the low-temperature sintered anti-pollution ceramic membrane is 4000L/(m) 2 hbar)。
Preparing an acidic solution with pH=3 by using HCl, immersing the low-temperature sintered anti-pollution ceramic membrane in the acidic solution for 72 hours, taking out the ceramic membrane, washing and drying, and calculating the mass loss rate of the ceramic membrane before and after acid etching to be 5.0%.
Preparing an alkaline solution with pH value of 10 by using NaOH, immersing the low-temperature sintered anti-pollution ceramic membrane in the alkaline solution for 72 hours, taking out the ceramic membrane, washing and drying, and calculating the mass loss rate of the ceramic membrane before and after alkaline etching to be 7.8%.
Humic acid with the concentration of 50mg/L is used as a trapped substance for filtration, nitrogen is introduced into a filtering device to maintain the pressure difference at two sides of a ceramic membrane to be 0.01MPa, and under the condition of continuous operation, the trapping rate of the anti-pollution ceramic membrane to the humic acid is 48%. The flux of the anti-pollution ceramic membrane reaches a plateau phase after being attenuated to 40%, and the anti-pollution ceramic membrane can be recovered to about 88% after backwashing.
The wastewater treatment test is carried out by adopting the low-temperature sintering anti-pollution ceramic membrane, the raw water adopts papermaking wastewater, COD in the wastewater is 385mg/L, SS is 33mg/L, under the condition that the pressure difference of two sides of the ceramic membrane is 0.01MPa, after the low-temperature sintering anti-pollution ceramic membrane is used for interception and filtration, the COD of the effluent is 80.6mg/L, and the SS is 1.8mg/L, so that the excellent interception and filtration effect is shown.
Embodiment two: the first embodiment is different from the first embodiment in that 92.5 parts of alumina powder (the particle size of the raw material is 5 mu m), 7.5 parts of composite low-temperature sintering aid, 15 parts of yellow dextrin and 5 parts of hydroxypropyl methylcellulose sodium are put into a planetary ball mill according to parts by weight, ball-milling and mixing are carried out at a speed of 400r/min, then sieving is carried out, the fine powder mixture is obtained, then the fine powder mixture is put into a mixer, 10 parts of water, 1.5 parts of lubricant and 8 parts of alumina fiber are added, the mixture is pressed and kneaded to form a green body, the green body is repeatedly pug-kneaded by a vacuum pug mill, the mixture pug is obtained after standing and aging, and the ceramic membrane base membrane is obtained after calcining treatment for 2 hours at 950 ℃.
The flexural strength of the low-temperature sintered anti-pollution ceramic film of the embodiment obtained through the test by the three-point bending test is 46MPa.
Claims (10)
1. The preparation method of the low-temperature sintered anti-pollution ceramic membrane is characterized by comprising the following steps of:
1. the mass ratio is 1:1:4 Li is 2 O、B 2 O 3 And SiO 2 Placing the powder into a polytetrafluoroethylene ball milling tank, and grinding for 3.5-4.5 h to obtain powder A; the mass ratio is 1:0.8 CuO and H 3 BO 3 Grinding in a polytetrafluoroethylene ball milling tank for 3.5-4.5 h to obtain powder B; the mass ratio of the powder A to the powder B is (1.8-3): 1 are mixed and ball-milled for 1 to 2 hours to obtain a complexMixing with a low-temperature sintering auxiliary agent;
2. placing alumina powder, a composite low-temperature sintering auxiliary agent, a pore-forming agent and a binder into a planetary ball mill, ball-milling and mixing at a speed of 400-500 r/min, sieving to obtain a fine powder mixture, placing the fine powder mixture into a mixer, adding water and a lubricant, mixing, kneading to form a green body, repeatedly pugging the green body by a vacuum pugging machine, standing and ageing to obtain a mixed pug, and calcining to obtain a ceramic membrane base membrane;
3. according to the mass ratio of (3-5): (1-2): (1-2) adding zeolite particles, alumina powder and silicon dioxide powder into a ball mill, adding NaCl solution with the concentration of 2-3 mol/L, performing wet ball milling treatment at the speed of 600-800 r/min, and cleaning and drying to obtain anti-pollution powder;
4. uniformly mixing water, anti-pollution powder, a composite low-temperature sintering auxiliary agent, a dispersing agent, a slurry rheological agent and a defoaming agent, mechanically stirring for 2-2.5 hours to obtain middle-layer slurry, spraying the middle-layer slurry onto a ceramic membrane base membrane by using a spray gun, drying, and firing at 850-950 ℃ to obtain the anti-pollution ceramic membrane;
5. under the condition of ice-water bath, metakaolin, anti-pollution powder and H 2 O 2 Mixing a foaming agent, silica sol and alkali excitation solution, and carrying out ultrasonic and mechanical stirring uniformly to obtain inorganic polymer slurry;
6. immersing the anti-pollution ceramic membrane in water for 6-8 h, coating inorganic polymer slurry on the immersed anti-pollution ceramic membrane, and performing heat treatment at 100-180 ℃ for 1-2 h to obtain a low-temperature sintered anti-pollution ceramic membrane;
wherein in the second step, the alumina powder is 90-95 parts by weight, the composite low-temperature sintering auxiliary agent is 5-10 parts by weight, the pore-forming agent is 10-20 parts by weight, the binder is 5-20 parts by weight, and the water is 5-10 parts by weight.
2. The method for preparing the low-temperature sintered anti-pollution ceramic membrane according to claim 1, wherein in the first step, the mass ratio of powder A to powder B is 2:1 are mixed and ball-milled for 1 to 1.5 hours.
3. The method for preparing the low-temperature sintered anti-pollution ceramic membrane according to claim 1, wherein the pore-forming agent in the second step is yellow dextrin, starch or graphite powder.
4. The method for preparing a low-temperature sintered anti-pollution ceramic membrane according to claim 1, wherein the binder in the second step is methylcellulose, polyvinyl alcohol or sodium hypromellose.
5. The method for preparing the low-temperature sintered anti-pollution ceramic membrane according to claim 1, wherein in the second step, the alumina powder is 92.5 parts by weight, the composite low-temperature sintering aid is 7.5 parts by weight, the pore-forming agent is 15 parts by weight, the binder is 5 parts by weight, and the water is 10 parts by weight.
6. The method for preparing a low temperature sintered anti-pollution ceramic membrane according to claim 1, wherein in the second step, the calcination treatment is performed at 900-950 ℃ for 2-3 hours.
7. The method for preparing a low temperature sintered anti-pollution ceramic membrane according to claim 1, wherein in the second step, the fine powder mixture and alumina fiber are placed in a mixer, water and lubricant are added, and the mixture is kneaded to form a green body.
8. The method for preparing a low temperature sintered anti-fouling ceramic membrane according to claim 1, wherein the dispersant in the fourth step is a polycarboxylate dispersant, and the slurry rheological agent is polyamide wax.
9. The method for preparing a low-temperature sintered anti-pollution ceramic membrane according to claim 1, wherein the alkali excitation solution in the fifth step is NaOH solution.
10. The method for producing a low-temperature sintered anti-fouling ceramic membrane according to claim 1, wherein the apparent viscosity of the inorganic polymer slurry is controlled to be 1000 to 2000 Pa-s in the fifth step.
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| CN110922204A (en) * | 2019-12-08 | 2020-03-27 | 浙江理工大学 | Preparation method of low-temperature sintered alumina ceramic membrane |
| CN114618313A (en) * | 2021-12-13 | 2022-06-14 | 宁波水艺膜科技发展有限公司 | High-flux anti-pollution reverse osmosis composite membrane and preparation method thereof |
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| CN110922204A (en) * | 2019-12-08 | 2020-03-27 | 浙江理工大学 | Preparation method of low-temperature sintered alumina ceramic membrane |
| CN114618313A (en) * | 2021-12-13 | 2022-06-14 | 宁波水艺膜科技发展有限公司 | High-flux anti-pollution reverse osmosis composite membrane and preparation method thereof |
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