CN111704142A - Method for preparing sodium ferric silicate from diatomite for photo-reduction of Cr (VI) - Google Patents
Method for preparing sodium ferric silicate from diatomite for photo-reduction of Cr (VI) Download PDFInfo
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- CN111704142A CN111704142A CN202010557945.9A CN202010557945A CN111704142A CN 111704142 A CN111704142 A CN 111704142A CN 202010557945 A CN202010557945 A CN 202010557945A CN 111704142 A CN111704142 A CN 111704142A
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 47
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 title claims abstract description 28
- 238000000034 method Methods 0.000 title claims abstract description 21
- 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 title claims abstract description 13
- 229910052708 sodium Inorganic materials 0.000 title claims abstract description 13
- 239000011734 sodium Substances 0.000 title claims abstract description 13
- 238000007540 photo-reduction reaction Methods 0.000 title claims abstract description 10
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 48
- 239000007864 aqueous solution Substances 0.000 claims abstract description 21
- 239000011941 photocatalyst Substances 0.000 claims abstract description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 19
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 12
- OOIOHEBTXPTBBE-UHFFFAOYSA-N [Na].[Fe] Chemical compound [Na].[Fe] OOIOHEBTXPTBBE-UHFFFAOYSA-N 0.000 claims abstract description 12
- -1 polytetrafluoroethylene Polymers 0.000 claims abstract description 12
- 239000012153 distilled water Substances 0.000 claims abstract description 11
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims abstract description 11
- 239000004810 polytetrafluoroethylene Substances 0.000 claims abstract description 11
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 9
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000000843 powder Substances 0.000 claims abstract description 8
- 239000000243 solution Substances 0.000 claims abstract description 8
- 239000002994 raw material Substances 0.000 claims abstract description 7
- 238000002156 mixing Methods 0.000 claims abstract description 6
- 238000006243 chemical reaction Methods 0.000 claims description 16
- 238000001035 drying Methods 0.000 claims description 11
- 239000011259 mixed solution Substances 0.000 claims description 10
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 9
- 238000003756 stirring Methods 0.000 claims description 9
- 230000000694 effects Effects 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 5
- 238000002161 passivation Methods 0.000 claims description 5
- 238000004321 preservation Methods 0.000 claims description 5
- 238000001179 sorption measurement Methods 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- 238000009210 therapy by ultrasound Methods 0.000 claims description 4
- 235000006408 oxalic acid Nutrition 0.000 claims description 3
- 239000000725 suspension Substances 0.000 claims description 3
- 238000010531 catalytic reduction reaction Methods 0.000 claims description 2
- 239000007788 liquid Substances 0.000 claims description 2
- 239000011651 chromium Substances 0.000 abstract description 15
- 229910001385 heavy metal Inorganic materials 0.000 abstract description 7
- 238000006722 reduction reaction Methods 0.000 abstract description 6
- JOPOVCBBYLSVDA-UHFFFAOYSA-N chromium(6+) Chemical compound [Cr+6] JOPOVCBBYLSVDA-UHFFFAOYSA-N 0.000 abstract description 5
- SOCTUWSJJQCPFX-UHFFFAOYSA-N dichromate(2-) Chemical compound [O-][Cr](=O)(=O)O[Cr]([O-])(=O)=O SOCTUWSJJQCPFX-UHFFFAOYSA-N 0.000 abstract description 3
- 229910052500 inorganic mineral Inorganic materials 0.000 abstract description 3
- 150000002500 ions Chemical class 0.000 abstract description 3
- 239000011707 mineral Substances 0.000 abstract description 3
- 238000004065 wastewater treatment Methods 0.000 abstract description 3
- 230000007613 environmental effect Effects 0.000 abstract description 2
- 238000004064 recycling Methods 0.000 abstract description 2
- 238000002360 preparation method Methods 0.000 abstract 1
- 239000000203 mixture Substances 0.000 description 11
- 239000005909 Kieselgur Substances 0.000 description 8
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 7
- 229910052804 chromium Inorganic materials 0.000 description 7
- 230000001699 photocatalysis Effects 0.000 description 7
- 239000010865 sewage Substances 0.000 description 4
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 229910052710 silicon Inorganic materials 0.000 description 3
- 239000010703 silicon Substances 0.000 description 3
- 231100000419 toxicity Toxicity 0.000 description 3
- 230000001988 toxicity Effects 0.000 description 3
- 238000007146 photocatalysis Methods 0.000 description 2
- 239000002351 wastewater Substances 0.000 description 2
- 229910021578 Iron(III) chloride Inorganic materials 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 238000002835 absorbance Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 238000002159 adsorption--desorption isotherm Methods 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 238000009388 chemical precipitation Methods 0.000 description 1
- 238000007405 data analysis Methods 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000005189 flocculation Methods 0.000 description 1
- 230000016615 flocculation Effects 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 239000002135 nanosheet Substances 0.000 description 1
- 229910052754 neon Inorganic materials 0.000 description 1
- GKAOGPIIYCISHV-UHFFFAOYSA-N neon atom Chemical compound [Ne] GKAOGPIIYCISHV-UHFFFAOYSA-N 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 230000033116 oxidation-reduction process Effects 0.000 description 1
- 230000002085 persistent effect Effects 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 150000005838 radical anions Chemical class 0.000 description 1
- 238000006479 redox reaction Methods 0.000 description 1
- 230000027756 respiratory electron transport chain Effects 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 238000000870 ultraviolet spectroscopy Methods 0.000 description 1
- 229910052724 xenon Inorganic materials 0.000 description 1
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/20—Silicates
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/002—Mixed oxides other than spinels, e.g. perovskite
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/78—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with alkali- or alkaline earth metals
-
- B01J35/39—
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
- B01J37/10—Heat treatment in the presence of water, e.g. steam
-
- 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
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
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- 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
- C02F1/70—Treatment of water, waste water, or sewage by reduction
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2523/00—Constitutive chemical elements of heterogeneous catalysts
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
- C01P2002/85—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by XPS, EDX or EDAX data
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/16—Pore diameter
- C01P2006/17—Pore diameter distribution
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- 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
- C02F2101/22—Chromium or chromium compounds, e.g. chromates
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/10—Photocatalysts
Abstract
A method for preparing sodium ferric silicate by diatomite for photo-reduction of Cr (VI), belonging to the fields of heavy metal ion wastewater treatment technology and nonmetallic mineral utilization; the method comprises the following steps: (1) pretreating diatomite, (2) uniformly mixing raw materials, and (3) carrying out hydrothermal reaction; the concrete method is that the diatomite is dispersed in the sodium hydroxide water solution to be evenly dispersed, reacted in a bath kettle, cleaned and dried; firstly, adding pretreated diatomite and sodium hydroxide aqueous solution into polytetrafluoroethylene lining, and continuously stirringStirring and sonicating, and finally, dropwise adding Fe (Cl)3)3Aqueous solution, and then hydrothermal reaction. The powder is synthesized and then washed and dried by distilled water and ethanol. The invention provides the preparation of the bundle-structure sodium iron silicate photocatalyst, which has the characteristics of stable structure, low price, recycling and the like, has excellent performance of photo-reducing hexavalent chromium, has a reduction rate of 60mg/L dichromate of 80 percent, and realizes good economic and environmental values.
Description
Technical Field
The invention belongs to the field of heavy metal ion wastewater treatment technology and nonmetallic mineral utilization, and relates to a method for preparing sodium ferric silicate from diatomite for photoreduction of Cr (VI).
Background
Heavy metal pollution has been one of the major challenges in sewage treatment in recent years, and heavy metal ions pose a persistent threat to the food chain due to their non-biodegradability. At present, the treatment methods of heavy metal polluted wastewater are more than ten, including membrane separation, electrochemical flocculation, ion exchange, adsorption, photocatalysis technology and the like. In contrast, for chromium heavy metal sewage, a photocatalytic reduction technology is widely adopted, and the principle is to utilize the light absorption and photocatalytic performance of a photocatalyst to accelerate the electron transfer between variable valence metal ions in the reaction and promote the oxidation reduction reaction of inorganic matters and organic matters in the sewage. Chromium in the water body exists in the form of acid radical anions, and is difficult to remove by methods such as adsorption, chemical precipitation and the like. Moreover, the toxicity of chromium is very strong, and the safety threshold value in water is only 0.01mg/L, so that the toxicity degradation is very important in the treatment process of chromium-containing heavy metal sewage. The toxicity of the trivalent chromium is far lower than that of the hexavalent chromium, and the highly toxic hexavalent chromium is reduced into the trivalent chromium, so that the significance of chromium-containing wastewater treatment is realized.
Diatomite is a natural porous mineral, mainly consists of silicon dioxide, and becomes an ideal silicon source for preparing silicate materials due to the advantages of no toxicity, low cost and rich reserves. This also allows silicate photocatalysts to have good structural stability and lower cost compared to other photocatalytic materials. Sodium iron silicate, commonly referred to as neon, is a chain silicate that is an emerging photocatalyst and has little been studied for its potential use in catalyzing the oxidation-reduction of pollutants in wastewater.
In the method, kieselguhr is used as a silicon source, a surfactant is not required to be introduced, and a one-step hydrothermal method is adopted to prepare the NaFeSi with the beam-shaped structure assembled by nano sheets2O6And further adding NaFeSi2O6As a photocatalyst in the visible (420 nm) range<λ<800nm), the performance of the hexavalent chromium is explored, and factors influencing the photoreduction activity are investigated.
Disclosure of Invention
The invention aims to provide a method for preparing sodium ferric silicate from diatomite for photo-reduction of Cr (VI). the method adopts a one-step hydrothermal method to uniformly mix raw materials of diatomite and ferric chloride, and simultaneously controls the relative content of components; then under the conditions of high temperature and high pressure, the bundle-shaped sodium iron silicate photocatalytic material is obtained, and the photocatalyst prepared by the method has excellent photoreduction performance.
A method for preparing sodium ferric silicate by diatomite comprises the following steps:
(1) pretreating diatomite: before the diatomite participates in the reaction, pretreatment is needed to remove a surface passivation layer and activate the reaction activity; dispersing 6g of diatomite in a sodium hydroxide aqueous solution, and performing ultrasonic treatment to uniformly disperse the diatomite; then, placing the mixed solution in a water bath kettle at 90 ℃ for heat preservation for at least 2h, finally, washing with distilled water, and placing in a drying oven for drying for later use;
preferably, every 6g of diatomite corresponds to 300mL of 0.15-0.3 mol/L sodium hydroxide aqueous solution;
(2) uniformly mixing the raw materials: firstly adding pretreated diatomite into a polytetrafluoroethylene lining, then adding a sodium hydroxide aqueous solution, continuously stirring and carrying out ultrasonic treatment for 2 minutes, and then stirring for at least 20 minutes; finally, dropwise addition of Fe (Cl)3)3Continuously stirring the aqueous solution for at least 20min to obtain a uniformly mixed solution;
preferably, the amount of the pretreated diatomaceous earth is 8mL or 5mL of a 0.03mol/L Fe (Cl) aqueous solution of sodium hydroxide at a concentration of 0.125 to 0.2mol/L per 0.2g of pretreated diatomaceous earth3)3An aqueous solution.
(3) Hydrothermal reaction: putting the polytetrafluoroethylene lining into a reaction kettle, heating to 160-200 ℃ along with a furnace (preferably 180 ℃), and preserving heat for 20-30h (such as 24 h); after the powder is synthesized, the powder is washed by distilled water and ethanol and is placed in a drying oven for drying, and then the sodium ferric silicate is obtained.
The sodium ferric silicate obtained by the invention is used as a photocatalyst, is further used for photo-reduction of Cr (VI), and can be reduced under the condition of visible light. The specific method comprises the following steps: adding the photocatalyst of the invention into Cr2O7 2-And (3) in the solution, standing the suspension liquid for 30min under a dark condition to achieve adsorption balance, then adding oxalic acid, and carrying out light catalytic reduction under a visible light condition.
The invention takes the diatomite as a silicon source, and the provided bundle-structure sodium iron silicate photocatalyst has the characteristics of stable structure, low price, recycling and the like, and shows excellent performance of photo-reducing hexavalent chromium, the reduction rate of 60mg/L dichromate can reach 80%, and good economic and environmental values are realized.
Drawings
FIG. 1 is an XRD pattern of the photocatalyst sodium iron silicate prepared in example 1;
FIG. 2 is N of the photocatalyst sodium iron silicate prepared in example 12Adsorption-desorption isotherms and pore size distributions;
FIG. 3 is an SEM photograph of the photocatalyst sodium iron silicate prepared in example 1;
FIG. 4 is a graph of the reduction efficiency of the photocatalyst sodium iron silicate prepared in example 1 for different concentrations of dichromate solution;
FIG. 5 is a XPS-Fe2p plot of sodium iron silicate before and after photocatalysis in example 1;
FIG. 6 is a graph showing the band gap and VB-XPS of the photocatalyst sodium iron silicate prepared in example 1.
Detailed Description
The present invention will be described in further detail with reference to the following examples, but the scope of the present invention is not limited to the following examples.
Example 1:
(1) pretreating diatomite: before the diatomite participates in the reaction, pretreatment is needed to remove a surface passivation layer and activate the reaction activity. 6g of diatomaceous earth was dispersed in 300mL of a 0.15mol/L aqueous solution of sodium hydroxide and the mixture was sonicated for 2min to disperse the diatomaceous earth uniformly. And then, placing the mixed solution in a water bath kettle at 90 ℃ for heat preservation for 2h, finally, washing with distilled water, and placing in an oven for drying at 60 ℃ for 12h for later use.
(2) Uniformly mixing the raw materials: 0.2g of pretreated diatomite is firstly added into the polytetrafluoroethylene lining, 8mL of sodium hydroxide aqueous solution with the concentration of 0.125mol/L is then added, the mixture is continuously stirred and ultrasonically treated for 2min, and then the mixture is stirred for 20min on a magnetic stirrer. Finally, 5mL of 0.03mol/L Fe (Cl) was added dropwise3)3·6H2And placing the O aqueous solution on a magnetic stirrer, and stirring for 20min to obtain a uniformly mixed solution.
(3) Hydrothermal reaction: and (3) putting the polytetrafluoroethylene lining into a reaction kettle, heating to 180 ℃ along with a furnace, and preserving heat for 24 hours. The powder is cleaned by distilled water and ethanol after being synthesized, and is dried for 12 hours in an oven at the temperature of 60 ℃ to obtain the photocatalyst.
Example 2:
(1) pretreating diatomite: before the diatomite participates in the reaction, pretreatment is needed to remove a surface passivation layer and activate the reaction activity. 6g of diatomaceous earth was dispersed in 300mL of a 0.3mol/L aqueous solution of sodium hydroxide and the mixture was sonicated for 2min to disperse the diatomaceous earth uniformly. And then, placing the mixed solution in a water bath kettle at 90 ℃ for heat preservation for 2h, finally, washing with distilled water, and placing in an oven for drying at 60 ℃ for 12h for later use.
(2) Uniformly mixing the raw materials: 0.2g of pretreated diatomite is firstly added into the polytetrafluoroethylene lining, 8mL of sodium hydroxide aqueous solution with the concentration of 0.2mol/L is then added, the mixture is continuously stirred and ultrasonically treated for 2min, and then the mixture is stirred for 20min on a magnetic stirrer. Finally, 5mL of 0.03mol/L Fe (Cl) was added dropwise3)3·6H2And placing the O aqueous solution on a magnetic stirrer, and stirring for 20min to obtain a uniformly mixed solution.
(3) Hydrothermal reaction: and (3) putting the polytetrafluoroethylene lining into a reaction kettle, heating to 180 ℃ along with a furnace, and preserving heat for 24 hours. The powder is cleaned by distilled water and ethanol after being synthesized, and is dried for 12 hours in an oven at the temperature of 60 ℃ to obtain the photocatalyst.
Example 3:
(1) pretreating diatomite: before the diatomite participates in the reaction, pretreatment is needed to remove a surface passivation layer and activate the reaction activity. 6g of diatomaceous earth was dispersed in 300mL of a 0.2mol/L aqueous solution of sodium hydroxide and the mixture was sonicated for 2min to disperse the diatomaceous earth uniformly. And then, placing the mixed solution in a water bath kettle at 90 ℃ for heat preservation for 2h, finally, washing with distilled water, and placing in an oven for drying at 60 ℃ for 12h for later use.
(2) Uniformly mixing the raw materials: 0.2g of pretreated diatomite is firstly added into the polytetrafluoroethylene lining, 8mL of sodium hydroxide aqueous solution with the concentration of 0.165mol/L is then added, the mixture is continuously stirred and ultrasonically treated for 2min, and then the mixture is stirred on a magnetic stirrer for 20 min. Finally, 5mL of 0.03mol/L Fe (Cl) was added dropwise3)3·6H2And placing the O aqueous solution on a magnetic stirrer, and stirring for 20min to obtain a uniformly mixed solution.
(3) Hydrothermal reaction: and (3) putting the polytetrafluoroethylene lining into a reaction kettle, heating to 180 ℃ along with a furnace, and preserving heat for 24 hours. The powder is cleaned by distilled water and ethanol after being synthesized, and is dried for 12 hours in an oven at the temperature of 60 ℃ to obtain the photocatalyst.
And (3) measuring the photocatalytic performance: taking 20mg of the photocatalyst of the invention, adding 60mL of Cr with the concentration of 60mg/L2O7 2-(with K)2Cr2O7Prepared) and the suspension is placed in the dark and kept still for 30min to reach the adsorption equilibrium. 40mg of oxalic acid was added, and the mixture was irradiated with light under visible light (300W xenon lamp) to repeat the test 3 times. In the photoreduction test, about 3mL of the solution was extracted at fixed time intervals using a 0.22 μm filter, and the absorbance of the solution was measured by an ultraviolet-visible spectrophotometer, and the reduction efficiency thereof was measured as the relative concentration C/C0The experimental data analysis shows that the reduction rate of the dichromate radical of 60mg/L can reach 80%.
Claims (7)
1. The method for preparing the sodium ferric silicate by using the diatomite is characterized by comprising the following steps:
(1) pretreating diatomite: before the diatomite participates in the reaction, pretreatment is needed to remove a surface passivation layer and activate the reaction activity; dispersing 6g of diatomite in a sodium hydroxide aqueous solution, and performing ultrasonic treatment to uniformly disperse the diatomite; then, placing the mixed solution in a water bath kettle at 90 ℃ for heat preservation for at least 2h, finally, washing with distilled water, and placing in a drying oven for drying for later use;
(2) uniformly mixing the raw materials: firstly adding pretreated diatomite into a polytetrafluoroethylene lining, then adding a sodium hydroxide aqueous solution, continuously stirring and carrying out ultrasonic treatment for 2 minutes, and then stirring for at least 20 minutes; finally, dropwise addition of Fe (Cl)3)3Continuously stirring the aqueous solution for at least 20min to obtain a uniformly mixed solution;
(3) hydrothermal reaction: putting the polytetrafluoroethylene lining into a reaction kettle, heating to 160-200 ℃ along with a furnace, and preserving heat for 20-30 h; after the powder is synthesized, the powder is washed by distilled water and ethanol and is placed in a drying oven for drying, and then the sodium ferric silicate is obtained.
2. The method for preparing sodium ferric silicate by using diatomite according to claim 1, wherein 300mL of 0.15-0.3 mol/L aqueous sodium hydroxide solution is used for every 6g of diatomite in the step (1).
3. The method for preparing sodium ferric silicate by using diatomite as claimed in claim 1, wherein the step (2) comprises using 8mL of aqueous sodium hydroxide solution with concentration of 0.125-0.2 mol/L and 5mL of Fe (Cl) with concentration of 0.03mol/L for every 0.2g of the pretreated diatomite3)3An aqueous solution.
4. The method for preparing sodium ferric silicate by using diatomite as claimed in claim 1, wherein the temperature of the step (3) is raised to 180 ℃ and kept for 24 h.
5. Sodium iron silicate obtainable by a process according to any one of claims 1 to 4.
6. Use of sodium iron silicate prepared according to the process of any one of claims 1 to 4 as a photocatalyst for the photoreduction of cr (vi) under visible light conditions.
7. Use according to claim 6, in particular by: adding photocatalyst into Cr2O7 2-And (3) in the solution, standing the suspension liquid for 30min under a dark condition to achieve adsorption balance, then adding oxalic acid, and carrying out light catalytic reduction under a visible light condition.
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| CN115121249B (en) * | 2022-05-29 | 2024-03-12 | 北京工业大学 | Preparation method and application of magnetic sodium iron silicate/hematite composite photocatalyst |
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