CN113546527B - Silver and lanthanum ion water purification composite ceramic membrane process - Google Patents
Silver and lanthanum ion water purification composite ceramic membrane process Download PDFInfo
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- CN113546527B CN113546527B CN202110857278.0A CN202110857278A CN113546527B CN 113546527 B CN113546527 B CN 113546527B CN 202110857278 A CN202110857278 A CN 202110857278A CN 113546527 B CN113546527 B CN 113546527B
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- 239000000919 ceramic Substances 0.000 title claims abstract description 99
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 62
- 239000012528 membrane Substances 0.000 title claims abstract description 49
- 239000002131 composite material Substances 0.000 title claims abstract description 26
- 229910052709 silver Inorganic materials 0.000 title claims abstract description 22
- 239000004332 silver Substances 0.000 title claims abstract description 22
- 238000000034 method Methods 0.000 title claims abstract description 19
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 title claims abstract description 17
- CZMAIROVPAYCMU-UHFFFAOYSA-N lanthanum(3+) Chemical compound [La+3] CZMAIROVPAYCMU-UHFFFAOYSA-N 0.000 title claims abstract description 15
- 238000000746 purification Methods 0.000 title claims abstract description 14
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 150
- 239000000243 solution Substances 0.000 claims abstract description 81
- VYFYYTLLBUKUHU-UHFFFAOYSA-N dopamine Chemical compound NCCC1=CC=C(O)C(O)=C1 VYFYYTLLBUKUHU-UHFFFAOYSA-N 0.000 claims abstract description 76
- 239000007864 aqueous solution Substances 0.000 claims abstract description 75
- 239000000843 powder Substances 0.000 claims abstract description 57
- 238000001035 drying Methods 0.000 claims abstract description 54
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 46
- 229910021638 Iridium(III) chloride Inorganic materials 0.000 claims abstract description 43
- DANYXEHCMQHDNX-UHFFFAOYSA-K trichloroiridium Chemical compound Cl[Ir](Cl)Cl DANYXEHCMQHDNX-UHFFFAOYSA-K 0.000 claims abstract description 43
- 229910004664 Cerium(III) chloride Inorganic materials 0.000 claims abstract description 42
- VYLVYHXQOHJDJL-UHFFFAOYSA-K cerium trichloride Chemical compound Cl[Ce](Cl)Cl VYLVYHXQOHJDJL-UHFFFAOYSA-K 0.000 claims abstract description 42
- 229960003638 dopamine Drugs 0.000 claims abstract description 38
- 238000005406 washing Methods 0.000 claims abstract description 30
- 239000007983 Tris buffer Substances 0.000 claims abstract description 28
- LENZDBCJOHFCAS-UHFFFAOYSA-N tris Chemical compound OCC(N)(CO)CO LENZDBCJOHFCAS-UHFFFAOYSA-N 0.000 claims abstract description 28
- 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 abstract description 24
- 229910052708 sodium Inorganic materials 0.000 claims abstract description 24
- 239000011734 sodium Substances 0.000 claims abstract description 24
- 239000004408 titanium dioxide Substances 0.000 claims abstract description 23
- 239000008367 deionised water Substances 0.000 claims abstract description 21
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 21
- 238000002791 soaking Methods 0.000 claims abstract description 20
- 239000007790 solid phase Substances 0.000 claims abstract description 20
- 238000001354 calcination Methods 0.000 claims abstract description 13
- -1 silver ions Chemical class 0.000 claims abstract description 12
- 238000003825 pressing Methods 0.000 claims abstract description 11
- 229910052746 lanthanum Inorganic materials 0.000 claims abstract description 8
- 239000000203 mixture Substances 0.000 claims description 40
- 238000003756 stirring Methods 0.000 claims description 28
- 238000001816 cooling Methods 0.000 claims description 27
- 239000012065 filter cake Substances 0.000 claims description 27
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 20
- 238000010438 heat treatment Methods 0.000 claims description 20
- 238000002156 mixing Methods 0.000 claims description 18
- 238000000967 suction filtration Methods 0.000 claims description 18
- 239000007788 liquid Substances 0.000 claims description 17
- 238000001914 filtration Methods 0.000 claims description 14
- 229910052786 argon Inorganic materials 0.000 claims description 10
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 10
- 230000007935 neutral effect Effects 0.000 claims description 10
- 239000002244 precipitate Substances 0.000 claims description 10
- 238000004321 preservation Methods 0.000 claims description 10
- 238000007789 sealing Methods 0.000 claims description 10
- 239000006228 supernatant Substances 0.000 claims description 10
- 238000011049 filling Methods 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims description 2
- 230000001681 protective effect Effects 0.000 claims 1
- 239000010865 sewage Substances 0.000 abstract description 9
- 238000002360 preparation method Methods 0.000 abstract description 5
- 229910021645 metal ion Inorganic materials 0.000 abstract description 3
- 230000001988 toxicity Effects 0.000 abstract description 3
- 231100000419 toxicity Toxicity 0.000 abstract description 3
- 238000004064 recycling Methods 0.000 abstract description 2
- 230000002349 favourable effect Effects 0.000 abstract 1
- 230000000052 comparative effect Effects 0.000 description 15
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000004907 flux Effects 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 description 2
- FOIXSVOLVBLSDH-UHFFFAOYSA-N Silver ion Chemical compound [Ag+] FOIXSVOLVBLSDH-UHFFFAOYSA-N 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 239000010842 industrial wastewater Substances 0.000 description 1
- FYDKNKUEBJQCCN-UHFFFAOYSA-N lanthanum(3+);trinitrate Chemical compound [La+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O FYDKNKUEBJQCCN-UHFFFAOYSA-N 0.000 description 1
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000008213 purified water Substances 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 229910001961 silver nitrate Inorganic materials 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
- 229910001928 zirconium oxide Inorganic materials 0.000 description 1
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
- B01D71/024—Oxides
-
- 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
- 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
- B01D71/024—Oxides
- B01D71/025—Aluminium oxide
-
- 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
- B01D71/024—Oxides
- B01D71/027—Silicium oxide
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/44—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/46—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on titanium oxides or titanates
- C04B35/462—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on titanium oxides or titanates based on titanates
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
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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
- C04B35/50—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on rare-earth compounds
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
- C04B38/04—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof by dissolving-out added substances
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3224—Rare earth oxide or oxide forming salts thereof, e.g. scandium oxide
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3224—Rare earth oxide or oxide forming salts thereof, e.g. scandium oxide
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3231—Refractory metal oxides, their mixed metal oxides, or oxide-forming salts thereof
- C04B2235/3232—Titanium oxides or titanates, e.g. rutile or anatase
- C04B2235/3234—Titanates, not containing zirconia
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- Separation Using Semi-Permeable Membranes (AREA)
Abstract
The invention discloses a silver and lanthanum ion water purification composite ceramic membrane process, which comprises the following steps: step one, reacting titanium dioxide powder with concentrated sodium hydroxide solution to obtain sodium trititanate powder; soaking sodium trititanate powder in a mixed aqueous solution of cerium trichloride and iridium trichloride, and then calcining to obtain solid-phase powder A; step three, pressing the solid-phase powder A into a tablet sample, and calcining to obtain a ceramic chip B; and step four, placing the ceramic wafer B in a dopamine aqueous solution, then placing the dopamine aqueous solution in a vacuum box, vacuumizing the box, then taking out the ceramic wafer, placing the ceramic wafer in a Tris buffer solution, soaking for 18-20 hours, then taking out the ceramic wafer, washing with deionized water, and drying to obtain the composite ceramic membrane. The preparation process of the ceramic membrane is optimized, and the prepared ceramic membrane can intercept a large amount of free silver ions and lanthanum ions in the sewage, is favorable for recycling metal ions in the sewage, and can reduce the toxicity of the sewage.
Description
Technical Field
The invention relates to the technical field of new energy materials, in particular to a silver and lanthanum ion water purification composite ceramic membrane process.
Background
Ceramic Membrane (Ceramic Membrane) is one of inorganic membranes, and is made of inorganic Ceramic material such as alumina (Al)2O3) Titanium dioxide (TiO)2) Zirconium oxide (ZrO)2) Or silicon dioxide (SiO)2) And the like through processes of surface coating, high-temperature sintering, extrusion forming and the like. The use of inorganic ceramic membranes originated from gas separation technology in the 20 th century, but with the advancement of process technology and the gradual decline of manufacturing cost, research on ceramic membranes has been developed in more and more fields. Especially, because of the characteristics of high mechanical strength and high chemical stability, the composite material has a plurality of application potentials which can be explored in modern industry. At present, more researches on ceramic membranes mainly focus on gas separation, industrial wastewater treatment, membrane material preparation and the like, and the applications of the ceramic membranes in purified water are relatively insufficient.
Disclosure of Invention
Based on the technical problem, the invention provides a silver and lanthanum ion water purification composite ceramic membrane process, which comprises the following steps:
mixing titanium dioxide powder and a concentrated sodium hydroxide solution to obtain a mixture, stirring the mixture for 10-20 min, then quickly pouring the mixture into a hydrothermal reaction kettle, sealing the kettle body, heating to 180-200 ℃, preserving heat, cooling to normal temperature after heat preservation, then opening the kettle body, standing the mixture, removing supernatant, washing a lower-layer white precipitate with deionized water until a washing solution is neutral, and obtaining sodium trititanate powder;
step two, preparing a mixed aqueous solution of cerium trichloride and iridium trichloride, adding the sodium trititanate powder into the mixed aqueous solution of cerium trichloride and iridium trichloride, stirring for 3-5 min, then carrying out suction filtration, drying a filter cake at 80-100 ℃, placing the dried filter cake into the mixed aqueous solution of cerium trichloride and iridium trichloride again, stirring for 3-5 min, carrying out suction filtration again, and drying the filter cake at 80-100 ℃; repeating the steps of soaking, filtering and drying for 6-8 times, drying for the last time, treating at 400-450 ℃ for 1-2 h, and cooling to normal temperature along with the furnace to obtain solid-phase powder A;
step three, pressing the solid-phase powder A into a tablet sample, putting the tablet sample into a muffle furnace, heating the tablet sample to 800 +/-10 ℃ along with the furnace, and calcining the tablet sample to obtain a ceramic chip B;
step four, preparing a Tris buffer solution, preparing a dopamine aqueous solution, placing the ceramic wafer B in the dopamine aqueous solution, then placing the dopamine aqueous solution in a vacuum box, filling the vacuum box with vacuum until no bubbles emerge in the solution, then taking out the ceramic wafer, placing the ceramic wafer in the Tris buffer solution, soaking for 18-20 hours, then taking out the ceramic wafer, washing with deionized water, and drying to obtain the composite ceramic membrane.
Further, in the concentrated sodium hydroxide solution, the concentration of sodium hydroxide is 8-10 mol/L, and the balance is water; the mixing ratio of the titanium dioxide powder and the concentrated sodium hydroxide solution is 0.3-0.6 g/100 mL.
Further, in the mixed water solution of cerium trichloride and iridium trichloride, the concentration of cerium trichloride is 3-7 g/100mL, the concentration of iridium trichloride is 0.6-1.3 g/100mL, and the balance is water; the solid-liquid mass ratio of the sodium trititanate powder added into the mixed aqueous solution of cerium trichloride and iridium trichloride is 1: 8-10.
Further, in the third step, the calcination time at 800 +/-10 ℃ is 2-3 h, and the calcined wafer sample is cooled to normal temperature along with the furnace in the argon protection atmosphere to obtain the ceramic wafer B.
Further, the concentration of the Tris buffer solution is 0.01mol/L, and the concentration of the dopamine aqueous solution is 2-2.3 g/L.
The invention also discloses an application of the composite ceramic membrane, and the composite ceramic membrane is used for filtering and removing free silver ions and lanthanum ions in a water body.
According to the technical scheme, the invention has the advantages that: the preparation method optimizes the preparation process of the ceramic membrane, and the prepared ceramic membrane can intercept a large amount of free silver ions and lanthanum ions in the sewage, is beneficial to recycling of metal ions in the sewage, and can reduce the toxicity of the sewage.
Detailed Description
The following is a detailed description with reference to examples:
example 1
A silver and lanthanum ion water purification composite ceramic membrane process comprises the following steps:
step one, preparing a concentrated sodium hydroxide solution, wherein the concentration of sodium hydroxide in the concentrated sodium hydroxide solution is 8mol/L, and the balance is water; mixing titanium dioxide powder and concentrated sodium hydroxide solution according to the proportion of 0.3g/100mL of mixed titanium dioxide/concentrated sodium hydroxide solution to obtain a mixture, stirring the mixture at the speed of 80r/min for 10min, then quickly pouring the mixture into a hydrothermal reaction kettle, sealing the kettle body, heating to 190 +/-10 ℃, preserving heat for 70h, cooling to normal temperature after the heat preservation is finished, then opening the kettle body, standing the mixture, removing the supernatant, washing the lower white precipitate with deionized water until the washing liquid is neutral, and drying at the temperature of 80 ℃ to obtain sodium trititanate powder;
preparing a mixed aqueous solution of cerium trichloride and iridium trichloride, wherein in the mixed aqueous solution of cerium trichloride and iridium trichloride, the concentration of cerium trichloride is 3g/100mL, the concentration of iridium trichloride is 1.3g/100mL, and the balance is water; adding the sodium trititanate powder into the mixed aqueous solution of cerium trichloride and iridium trichloride according to the solid-liquid mass ratio of 1:8, stirring for 5min at 60r/min, then carrying out suction filtration, drying a filter cake at 80 ℃, then placing the dried filter cake into the mixed aqueous solution of cerium trichloride and iridium trichloride again, stirring for 5min at 60r/min, carrying out suction filtration again, and drying the filter cake at 80 ℃; repeating the steps of soaking, suction filtering and drying for 6 times, drying for the last time, treating at 400 ℃ for 2 hours, and then cooling to normal temperature along with the furnace to obtain solid-phase powder A;
pressing the solid-phase powder A into a sheet sample under the pressure of 4MPa, keeping the pressure for 5min, keeping the thickness of the sheet sample to be 0.6mm, then putting the sheet sample into a muffle furnace, heating the sheet sample to 800 +/-10 ℃ along with the furnace at the speed of 5 ℃/min, calcining the sheet sample for 2h, and cooling the calcined sheet sample to the normal temperature along with the furnace in the argon protection atmosphere to obtain a ceramic sheet B;
step four, preparing a Tris buffer solution and preparing a dopamine aqueous solution, wherein the concentration of the Tris buffer solution is 0.01mol/L, and the concentration of the dopamine aqueous solution is 2 g/L; and placing the ceramic wafer B in the dopamine aqueous solution, then placing the dopamine aqueous solution in a vacuum box, vacuumizing the box until no bubbles emerge in the solution, then taking out the ceramic wafer, placing the ceramic wafer in the Tris buffer solution, soaking for 18 hours, then taking out the ceramic wafer, washing with deionized water, and drying at 80 ℃ to obtain the composite ceramic membrane.
Example 2
A silver and lanthanum ion water purification composite ceramic membrane process comprises the following steps:
step one, preparing a concentrated sodium hydroxide solution, wherein the concentration of sodium hydroxide in the concentrated sodium hydroxide solution is 9mol/L, and the balance is water; mixing titanium dioxide powder and concentrated sodium hydroxide solution according to the mixing ratio of 0.4g/100mL of titanium dioxide/concentrated sodium hydroxide solution to obtain a mixture, stirring the mixture at the speed of 80r/min for 10min, then quickly pouring the mixture into a hydrothermal reaction kettle, sealing the kettle body, heating to 190 +/-10 ℃, preserving heat for 70h, cooling to normal temperature after the heat preservation is finished, then opening the kettle body, standing the mixture, removing the supernatant, washing the white precipitate at the lower layer with deionized water until the washing liquid is neutral, and drying at the temperature of 80 ℃ to obtain sodium trititanate powder;
preparing a mixed aqueous solution of cerium trichloride and iridium trichloride, wherein in the mixed aqueous solution of cerium trichloride and iridium trichloride, the concentration of cerium trichloride is 5g/100mL, the concentration of iridium trichloride is 1g/100mL, and the balance is water; adding the sodium trititanate powder into the mixed aqueous solution of cerium trichloride and iridium trichloride according to the solid-liquid mass ratio of 1:8, stirring for 5min at 60r/min, then carrying out suction filtration, drying a filter cake at 80 ℃, then placing the dried filter cake into the mixed aqueous solution of cerium trichloride and iridium trichloride again, stirring for 5min at 60r/min, carrying out suction filtration again, and drying the filter cake at 80 ℃; repeating the steps of soaking, suction filtering and drying for 7 times, drying for the last time, treating at 420 ℃ for 2 hours, and then cooling to normal temperature along with the furnace to obtain solid-phase powder A;
pressing the solid-phase powder A into a sheet sample under the pressure of 4MPa, keeping the pressure for 5min, keeping the thickness of the sheet sample to be 0.6mm, then putting the sheet sample into a muffle furnace, heating the sheet sample to 800 +/-10 ℃ along with the furnace at the speed of 5 ℃/min, calcining the sheet sample for 2h, and cooling the calcined sheet sample to the normal temperature along with the furnace in the argon protection atmosphere to obtain a ceramic sheet B;
step four, preparing a Tris buffer solution and preparing a dopamine aqueous solution, wherein the concentration of the Tris buffer solution is 0.01mol/L, and the concentration of the dopamine aqueous solution is 2.1 g/L; and placing the ceramic wafer B in the dopamine aqueous solution, then placing the dopamine aqueous solution in a vacuum box, vacuumizing the box until no bubbles emerge in the solution, then taking out the ceramic wafer, placing the ceramic wafer in the Tris buffer solution, soaking for 18h, then taking out the ceramic wafer, washing with deionized water, and drying at 80 ℃ to obtain the composite ceramic membrane.
Example 3
A silver and lanthanum ion water purification composite ceramic membrane process comprises the following steps:
step one, preparing a concentrated sodium hydroxide solution, wherein the concentration of sodium hydroxide in the concentrated sodium hydroxide solution is 9mol/L, and the balance is water; mixing titanium dioxide powder and concentrated sodium hydroxide solution according to the mixing ratio of 0.5g/100mL of titanium dioxide/concentrated sodium hydroxide solution to obtain a mixture, stirring the mixture at the speed of 80r/min for 10min, then quickly pouring the mixture into a hydrothermal reaction kettle, sealing the kettle body, heating to 190 +/-10 ℃, preserving heat for 70h, cooling to normal temperature after the heat preservation is finished, then opening the kettle body, standing the mixture, removing the supernatant, washing the white precipitate at the lower layer with deionized water until the washing liquid is neutral, and drying at the temperature of 80 ℃ to obtain sodium trititanate powder;
preparing a mixed aqueous solution of cerium trichloride and iridium trichloride, wherein in the mixed aqueous solution of cerium trichloride and iridium trichloride, the concentration of cerium trichloride is 6g/100mL, the concentration of iridium trichloride is 0.8g/100mL, and the balance is water; adding the sodium trititanate powder into the mixed aqueous solution of cerium trichloride and iridium trichloride according to the solid-liquid mass ratio of 1:8, stirring for 5min at 60r/min, then carrying out suction filtration, drying a filter cake at 80 ℃, then placing the dried filter cake into the mixed aqueous solution of cerium trichloride and iridium trichloride again, stirring for 5min at 60r/min, carrying out suction filtration again, and drying the filter cake at 80 ℃; repeating the steps of soaking, suction filtering and drying for 7 times, drying for the last time, treating at 440 ℃ for 1h, and then cooling to normal temperature along with the furnace to obtain solid-phase powder A;
pressing the solid-phase powder A into a sheet sample under the pressure of 4MPa, keeping the pressure for 5min, keeping the thickness of the sheet sample to be 0.6mm, then putting the sheet sample into a muffle furnace, heating the sheet sample to 800 +/-10 ℃ along with the furnace at the speed of 5 ℃/min, calcining the sheet sample for 2h, and cooling the calcined sheet sample to the normal temperature along with the furnace in the argon protection atmosphere to obtain a ceramic sheet B;
step four, preparing a Tris buffer solution and preparing a dopamine aqueous solution, wherein the concentration of the Tris buffer solution is 0.01mol/L, and the concentration of the dopamine aqueous solution is 2.2 g/L; and placing the ceramic wafer B in the dopamine aqueous solution, then placing the dopamine aqueous solution in a vacuum box, vacuumizing the box until no bubbles emerge in the solution, then taking out the ceramic wafer, placing the ceramic wafer in the Tris buffer solution, soaking for 18h, then taking out the ceramic wafer, washing with deionized water, and drying at 80 ℃ to obtain the composite ceramic membrane.
Example 4
A silver and lanthanum ion water purification composite ceramic membrane process comprises the following steps:
step one, preparing a concentrated sodium hydroxide solution, wherein the concentration of sodium hydroxide in the concentrated sodium hydroxide solution is 10mol/L, and the balance is water; mixing titanium dioxide powder and concentrated sodium hydroxide solution according to the mixing ratio of 0.6g/100mL of titanium dioxide/concentrated sodium hydroxide solution to obtain a mixture, stirring the mixture at the speed of 80r/min for 10min, then quickly pouring the mixture into a hydrothermal reaction kettle, sealing the kettle body, heating to 190 +/-10 ℃, preserving heat for 70h, cooling to normal temperature after the heat preservation is finished, then opening the kettle body, standing the mixture, removing the supernatant, washing the white precipitate at the lower layer with deionized water until the washing liquid is neutral, and drying at the temperature of 80 ℃ to obtain sodium trititanate powder;
preparing a mixed aqueous solution of cerium trichloride and iridium trichloride, wherein in the mixed aqueous solution of cerium trichloride and iridium trichloride, the concentration of cerium trichloride is 7g/100mL, the concentration of iridium trichloride is 0.6g/100mL, and the balance is water; adding the sodium trititanate powder into the mixed aqueous solution of cerium trichloride and iridium trichloride according to the solid-liquid mass ratio of 1:8, stirring for 5min at 60r/min, then carrying out suction filtration, drying a filter cake at 80 ℃, then placing the dried filter cake into the mixed aqueous solution of cerium trichloride and iridium trichloride again, stirring for 5min at 60r/min, carrying out suction filtration again, and drying the filter cake at 80 ℃; repeating the steps of soaking, suction filtering and drying for 8 times, drying for the last time, treating at 450 ℃ for 1h, and then cooling to normal temperature along with the furnace to obtain solid-phase powder A;
pressing the solid-phase powder A into a sheet sample under the pressure of 4MPa, keeping the pressure for 5min, keeping the thickness of the sheet sample to be 0.6mm, then putting the sheet sample into a muffle furnace, heating the sheet sample to 800 +/-10 ℃ along with the furnace at the speed of 5 ℃/min, calcining the sheet sample for 2h, and cooling the calcined sheet sample to the normal temperature along with the furnace in the argon protection atmosphere to obtain a ceramic sheet B;
step four, preparing a Tris buffer solution and preparing a dopamine aqueous solution, wherein the concentration of the Tris buffer solution is 0.01mol/L, and the concentration of the dopamine aqueous solution is 2.3 g/L; and placing the ceramic wafer B in the dopamine aqueous solution, then placing the dopamine aqueous solution in a vacuum box, vacuumizing the box until no bubbles emerge in the solution, then taking out the ceramic wafer, placing the ceramic wafer in the Tris buffer solution, soaking for 18h, then taking out the ceramic wafer, washing with deionized water, and drying at 80 ℃ to obtain the composite ceramic membrane.
Comparative example 1
A ceramic membrane process comprising the steps of:
step one, preparing a concentrated sodium hydroxide solution, wherein the concentration of sodium hydroxide in the concentrated sodium hydroxide solution is 10mol/L, and the balance is water; mixing titanium dioxide powder and concentrated sodium hydroxide solution according to the proportion of 0.6g/100mL of mixed titanium dioxide/concentrated sodium hydroxide solution to obtain a mixture, stirring the mixture at the speed of 80r/min for 10min, then quickly pouring the mixture into a hydrothermal reaction kettle, sealing the kettle body, heating to 190 +/-10 ℃, preserving heat for 70h, cooling to normal temperature after the heat preservation is finished, then opening the kettle body, standing the mixture, removing the supernatant, washing the lower white precipitate with deionized water until the washing liquid is neutral, and drying at the temperature of 80 ℃ to obtain sodium trititanate powder;
secondly, pressing the sodium trititanate powder into a sheet sample under the pressure of 4MPa, keeping the pressure for 5min, wherein the thickness of the sheet sample is 0.6mm, then putting the sheet sample into a muffle furnace, heating the sheet sample to 800 +/-10 ℃ along with the furnace at the speed of 5 ℃/min, calcining the sheet sample for 2h, and cooling the calcined sheet sample to the normal temperature along with the furnace in the argon protection atmosphere to obtain a ceramic sheet A;
step three, preparing a Tris buffer solution and preparing a dopamine aqueous solution, wherein the concentration of the Tris buffer solution is 0.01mol/L, and the concentration of the dopamine aqueous solution is 2.3 g/L; and placing the ceramic wafer A in the dopamine aqueous solution, then placing the dopamine aqueous solution in a vacuum box, vacuumizing the box until no bubbles emerge in the solution, then taking out the ceramic wafer, placing the ceramic wafer in the Tris buffer solution, soaking for 18 hours, then taking out the ceramic wafer, washing with deionized water, and drying at 80 ℃ to obtain the ceramic membrane of the comparative example.
Comparative example 2
A ceramic membrane process comprising the steps of:
step one, preparing a concentrated sodium hydroxide solution, wherein the concentration of sodium hydroxide in the concentrated sodium hydroxide solution is 10mol/L, and the balance is water; mixing titanium dioxide powder and concentrated sodium hydroxide solution according to the mixing ratio of 0.6g/100mL of titanium dioxide/concentrated sodium hydroxide solution to obtain a mixture, stirring the mixture at the speed of 80r/min for 10min, then quickly pouring the mixture into a hydrothermal reaction kettle, sealing the kettle body, heating to 190 +/-10 ℃, preserving heat for 70h, cooling to normal temperature after the heat preservation is finished, then opening the kettle body, standing the mixture, removing the supernatant, washing the white precipitate at the lower layer with deionized water until the washing liquid is neutral, and drying at the temperature of 80 ℃ to obtain sodium trititanate powder;
preparing an aqueous solution of cerium trichloride, wherein the concentration of the cerium trichloride is 7g/100mL, and the balance is water; adding the sodium trititanate powder into the aqueous solution of cerium trichloride according to the solid-liquid mass ratio of 1:8, stirring for 5min at 60r/min, then carrying out suction filtration, drying the filter cake at 80 ℃, placing the dried filter cake into the aqueous solution of cerium trichloride again, stirring for 5min at 60r/min, carrying out suction filtration again, and drying the filter cake at 80 ℃; repeating the steps of soaking, suction filtering and drying for 8 times, drying for the last time, treating at 450 ℃ for 1h, and then cooling to normal temperature along with the furnace to obtain solid-phase powder A;
pressing the solid-phase powder A into a sheet sample under the pressure of 4MPa, keeping the pressure for 5min, keeping the thickness of the sheet sample to be 0.6mm, then putting the sheet sample into a muffle furnace, heating the sheet sample to 800 +/-10 ℃ along with the furnace at the speed of 5 ℃/min, calcining the sheet sample for 2h, and cooling the calcined sheet sample to the normal temperature along with the furnace in the argon protection atmosphere to obtain a ceramic sheet B;
step four, preparing a Tris buffer solution and preparing a dopamine aqueous solution, wherein the concentration of the Tris buffer solution is 0.01mol/L, and the concentration of the dopamine aqueous solution is 2.3 g/L; and placing the ceramic wafer B in the dopamine aqueous solution, then placing the dopamine aqueous solution in a vacuum box, vacuumizing the box until no bubbles emerge in the solution, then taking out the ceramic wafer, placing the ceramic wafer in the Tris buffer solution, soaking for 18 hours, then taking out the ceramic wafer, washing with deionized water, and drying at 80 ℃ to obtain the ceramic membrane of the comparative example.
Comparative example 3
A ceramic membrane process comprising the steps of:
step one, preparing a concentrated sodium hydroxide solution, wherein the concentration of sodium hydroxide in the concentrated sodium hydroxide solution is 10mol/L, and the balance is water; mixing titanium dioxide powder and concentrated sodium hydroxide solution according to the mixing ratio of 0.6g/100mL of titanium dioxide/concentrated sodium hydroxide solution to obtain a mixture, stirring the mixture at the speed of 80r/min for 10min, then quickly pouring the mixture into a hydrothermal reaction kettle, sealing the kettle body, heating to 190 +/-10 ℃, preserving heat for 70h, cooling to normal temperature after the heat preservation is finished, then opening the kettle body, standing the mixture, removing the supernatant, washing the white precipitate at the lower layer with deionized water until the washing liquid is neutral, and drying at the temperature of 80 ℃ to obtain sodium trititanate powder;
preparing an iridium trichloride aqueous solution, wherein the concentration of iridium trichloride in the iridium trichloride aqueous solution is 0.6g/100mL, and the balance of water; adding the sodium trititanate powder into the iridium trichloride aqueous solution according to the solid-liquid mass ratio of 1:8, stirring for 5min at 60r/min, then carrying out suction filtration, drying the filter cake at 80 ℃, placing the dried filter cake into the iridium trichloride aqueous solution again, stirring for 5min at 60r/min, carrying out suction filtration again, and drying the filter cake at 80 ℃; repeating the steps of soaking, suction filtering and drying for 8 times, drying for the last time, treating at 450 ℃ for 1h, and then cooling to normal temperature along with the furnace to obtain solid-phase powder A;
pressing the solid-phase powder A into a sheet sample under the pressure of 4MPa, keeping the pressure for 5min, keeping the thickness of the sheet sample to be 0.6mm, then putting the sheet sample into a muffle furnace, heating the sheet sample to 800 +/-10 ℃ along with the furnace at the speed of 5 ℃/min, calcining the sheet sample for 2h, and cooling the calcined sheet sample to the normal temperature along with the furnace in the argon protection atmosphere to obtain a ceramic sheet B;
step four, preparing a Tris buffer solution and preparing a dopamine aqueous solution, wherein the concentration of the Tris buffer solution is 0.01mol/L, and the concentration of the dopamine aqueous solution is 2.3 g/L; and placing the ceramic wafer B in the dopamine aqueous solution, then placing the dopamine aqueous solution in a vacuum box, vacuumizing the box until no bubbles emerge in the solution, then taking out the ceramic wafer, placing the ceramic wafer in the Tris buffer solution, soaking for 18 hours, then taking out the ceramic wafer, washing with deionized water, and drying at 80 ℃ to obtain the ceramic membrane of the comparative example.
Comparative example 4
A ceramic membrane process comprising the steps of:
step one, preparing a concentrated sodium hydroxide solution, wherein the concentration of sodium hydroxide in the concentrated sodium hydroxide solution is 10mol/L, and the balance is water; mixing titanium dioxide powder and concentrated sodium hydroxide solution according to the mixing ratio of 0.6g/100mL of titanium dioxide/concentrated sodium hydroxide solution to obtain a mixture, stirring the mixture at the speed of 80r/min for 10min, then quickly pouring the mixture into a hydrothermal reaction kettle, sealing the kettle body, heating to 190 +/-10 ℃, preserving heat for 70h, cooling to normal temperature after the heat preservation is finished, then opening the kettle body, standing the mixture, removing the supernatant, washing the white precipitate at the lower layer with deionized water until the washing liquid is neutral, and drying at the temperature of 80 ℃ to obtain sodium trititanate powder;
preparing a mixed aqueous solution of cerium trichloride and iridium trichloride, wherein in the mixed aqueous solution of cerium trichloride and iridium trichloride, the concentration of cerium trichloride is 7g/100mL, the concentration of iridium trichloride is 0.6g/100mL, and the balance is water; adding the sodium trititanate powder into the mixed aqueous solution of cerium trichloride and iridium trichloride according to the solid-liquid mass ratio of 1:8, stirring for 5min at 60r/min, then carrying out suction filtration, drying a filter cake at 80 ℃, then placing the dried filter cake into the mixed aqueous solution of cerium trichloride and iridium trichloride again, stirring for 5min at 60r/min, carrying out suction filtration again, and drying the filter cake at 80 ℃; repeating the steps of soaking, suction filtering and drying for 8 times, drying for the last time, treating at 450 ℃ for 1h, and then cooling to normal temperature along with the furnace to obtain solid-phase powder A;
and step three, pressing the solid-phase powder A into a sheet sample under the pressure of 4MPa, keeping the pressure for 5min, keeping the thickness of the sheet sample to be 0.6mm, then putting the sheet sample into a muffle furnace, heating the sheet sample to 800 +/-10 ℃ along with the furnace at the speed of 5 ℃/min, calcining the sheet sample for 2h, and cooling the calcined sheet sample to the normal temperature along with the furnace in the argon protection atmosphere to obtain the ceramic membrane of the comparative example.
Example 5
Lanthanum nitrate and silver nitrate were added to deionized water to prepare wastewater containing silver and lanthanum ions, wherein the concentration of lanthanum ions was 0.21mmol/L and the concentration of silver was 1.35mmol/L, and the rejection rate of the ceramic membranes prepared in each example and comparative example to silver and lanthanum ions, which is (concentration before filtration-concentration after filtration)/concentration before filtration × 100%, was measured at a filtration pressure of 0.1MPa, and the results are shown in table 1.
TABLE 1
| Test group | Pure water flux (L/h.m)2) | Silver ion rejection rate | Lanthanum ion rejection rate |
| Example 1 | 0.328×103 | 96.9％ | 98.3％ |
| Example 2 | 0.309×103 | 97.2％ | 98.8％ |
| Example 3 | 0.317×103 | 97.6％ | 99.0％ |
| Example 4 | 0.320×103 | 97.5％ | 98.5％ |
| Comparative example 1 | 0.314×103 | 72.5％ | 79.7％ |
| Comparative example 2 | 0.324×103 | 81.0％ | 84.2％ |
| Comparative example 3 | 0.311×103 | 83.4％ | 84.7％ |
| Comparative example 4 | 0.316×103 | 82.9％ | 85.1％ |
As can be seen from Table 1, the composite ceramic membrane prepared by the invention has a large flux to water, which indicates that the pore structure of the ceramic membrane is beneficial to the water passage and does not influence the normal water passage. The comparative example and the comparative example show that after the preparation process of the ceramic membrane is optimized, the prepared ceramic membrane can intercept a large amount of free silver ions and lanthanum ions in sewage, the metal ions in the sewage can be recycled, and the toxicity of the sewage can be reduced.
The technical solutions provided by the present invention are described in detail above, and for those skilled in the art, the ideas according to the embodiments of the present invention may be changed in the specific implementation manners and the application ranges, and in summary, the content of the present description should not be construed as limiting the present invention.
Claims (6)
1. The process for preparing the silver and lanthanum ion water purification composite ceramic membrane is characterized by comprising the following steps of:
mixing titanium dioxide powder and a concentrated sodium hydroxide solution to obtain a mixture, stirring the mixture for 10-20 min, then quickly pouring the mixture into a hydrothermal reaction kettle, sealing the kettle body, heating to 180-200 ℃, preserving heat, cooling to normal temperature after heat preservation, then opening the kettle body, standing the mixture, removing supernatant, washing a lower-layer white precipitate with deionized water until a washing solution is neutral, and obtaining sodium trititanate powder;
step two, preparing a mixed aqueous solution of cerium trichloride and iridium trichloride, adding the sodium trititanate powder into the mixed aqueous solution of cerium trichloride and iridium trichloride, stirring for 3-5 min, then carrying out suction filtration, drying a filter cake at 80-100 ℃, placing the dried filter cake into the mixed aqueous solution of cerium trichloride and iridium trichloride again, stirring for 3-5 min, carrying out suction filtration again, and drying the filter cake at 80-100 ℃; repeating the steps of soaking, filtering and drying for 6-8 times, drying for the last time, treating at 400-450 ℃ for 1-2 h, and cooling to normal temperature along with the furnace to obtain solid-phase powder A;
thirdly, pressing the solid-phase powder A into a sample, putting the sample into a muffle furnace, and heating the sample to 800 +/-10 ℃ along with the furnace to calcine the sample to obtain a ceramic chip B;
step four, preparing a Tris buffer solution, preparing a dopamine aqueous solution, placing the ceramic wafer B in the dopamine aqueous solution, then placing the dopamine aqueous solution in a vacuum box, filling the vacuum box with vacuum until no bubbles emerge in the solution, then taking out the ceramic wafer, placing the ceramic wafer in the Tris buffer solution, soaking for 18-20 hours, then taking out the ceramic wafer, washing with deionized water, and drying to obtain the composite ceramic membrane.
2. The silver and lanthanum ion water purification composite ceramic membrane process according to claim 1, wherein in the concentrated sodium hydroxide solution, the concentration of sodium hydroxide is 8-10 mol/L, and the balance is water; the mixing ratio of the titanium dioxide powder to the concentrated sodium hydroxide solution is 0.3-0.6 g/100mL of titanium dioxide/concentrated sodium hydroxide solution.
3. The silver and lanthanum ion water purification composite ceramic membrane process according to claim 1, wherein in the mixed aqueous solution of cerium trichloride and iridium trichloride, the concentration of cerium trichloride is 3-7 g/100mL, the concentration of iridium trichloride is 0.6-1.3 g/100mL, and the balance is water; the solid-liquid mass ratio of the sodium trititanate powder added into the mixed aqueous solution of cerium trichloride and iridium trichloride is 1: 8-10.
4. The silver and lanthanum ion water purification composite ceramic membrane process according to claim 1, wherein in the third step, the calcination time at 800 ± 10 ℃ is 2-3 h, and the calcined wafer sample is furnace-cooled to normal temperature in an argon protective atmosphere to obtain the ceramic wafer B.
5. The silver and lanthanum ion water purification composite ceramic membrane process according to claim 1, wherein the concentration of the Tris buffer solution is 0.01mol/L, and the concentration of the dopamine aqueous solution is 2-2.3 g/L.
6. Use of a composite ceramic membrane according to any one of claims 1 to 5 for the filtration removal of free silver and lanthanum ions from a water body.
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