CN114345316A - TiO22Preparation method of magnesium lithium silicate composite photocatalyst - Google Patents
TiO22Preparation method of magnesium lithium silicate composite photocatalyst Download PDFInfo
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- CN114345316A CN114345316A CN202210030476.4A CN202210030476A CN114345316A CN 114345316 A CN114345316 A CN 114345316A CN 202210030476 A CN202210030476 A CN 202210030476A CN 114345316 A CN114345316 A CN 114345316A
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- lithium silicate
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- IPGANOYOHAODGA-UHFFFAOYSA-N dilithium;dimagnesium;dioxido(oxo)silane Chemical compound [Li+].[Li+].[Mg+2].[Mg+2].[O-][Si]([O-])=O.[O-][Si]([O-])=O.[O-][Si]([O-])=O IPGANOYOHAODGA-UHFFFAOYSA-N 0.000 title claims abstract description 67
- 239000011941 photocatalyst Substances 0.000 title claims abstract description 50
- 239000002131 composite material Substances 0.000 title claims abstract description 49
- 238000000034 method Methods 0.000 title description 7
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 37
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims abstract description 28
- 238000002360 preparation method Methods 0.000 claims abstract description 24
- 238000005406 washing Methods 0.000 claims abstract description 22
- 239000002243 precursor Substances 0.000 claims abstract description 21
- 238000006243 chemical reaction Methods 0.000 claims abstract description 15
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 14
- 238000001816 cooling Methods 0.000 claims abstract description 8
- 238000001035 drying Methods 0.000 claims abstract description 8
- 238000000227 grinding Methods 0.000 claims abstract description 8
- 229910052912 lithium silicate Inorganic materials 0.000 claims abstract description 7
- GCICAPWZNUIIDV-UHFFFAOYSA-N lithium magnesium Chemical compound [Li].[Mg] GCICAPWZNUIIDV-UHFFFAOYSA-N 0.000 claims abstract description 6
- PQXKHYXIUOZZFA-UHFFFAOYSA-M lithium fluoride Chemical compound [Li+].[F-] PQXKHYXIUOZZFA-UHFFFAOYSA-M 0.000 claims description 70
- 239000000243 solution Substances 0.000 claims description 65
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 42
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 36
- CSNNHWWHGAXBCP-UHFFFAOYSA-L Magnesium sulfate Chemical compound [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 claims description 35
- 238000005303 weighing Methods 0.000 claims description 29
- 239000008367 deionised water Substances 0.000 claims description 28
- 229910021641 deionized water Inorganic materials 0.000 claims description 28
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 21
- 239000006185 dispersion Substances 0.000 claims description 21
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 claims description 21
- 239000000347 magnesium hydroxide Substances 0.000 claims description 21
- 229910001862 magnesium hydroxide Inorganic materials 0.000 claims description 21
- 239000000377 silicon dioxide Substances 0.000 claims description 21
- 235000012239 silicon dioxide Nutrition 0.000 claims description 21
- 238000003756 stirring Methods 0.000 claims description 21
- 239000011268 mixed slurry Substances 0.000 claims description 19
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 14
- YHWCPXVTRSHPNY-UHFFFAOYSA-N butan-1-olate;titanium(4+) Chemical compound [Ti+4].CCCC[O-].CCCC[O-].CCCC[O-].CCCC[O-] YHWCPXVTRSHPNY-UHFFFAOYSA-N 0.000 claims description 14
- 239000007788 liquid Substances 0.000 claims description 14
- 238000000967 suction filtration Methods 0.000 claims description 14
- 239000007787 solid Substances 0.000 claims description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 9
- 235000019353 potassium silicate Nutrition 0.000 claims description 9
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims description 9
- 229910052943 magnesium sulfate Inorganic materials 0.000 claims description 7
- 235000019341 magnesium sulphate Nutrition 0.000 claims description 7
- 239000002244 precipitate Substances 0.000 claims description 7
- KKCBUQHMOMHUOY-UHFFFAOYSA-N sodium oxide Chemical compound [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 claims description 7
- 229910001948 sodium oxide Inorganic materials 0.000 claims description 7
- 239000011259 mixed solution Substances 0.000 claims description 6
- 239000000047 product Substances 0.000 claims description 6
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims description 5
- 229910052744 lithium Inorganic materials 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 5
- 230000003197 catalytic effect Effects 0.000 claims description 4
- 239000011777 magnesium Substances 0.000 claims description 4
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 3
- 230000015556 catabolic process Effects 0.000 claims description 3
- 238000006731 degradation reaction Methods 0.000 claims description 3
- 229910052749 magnesium Inorganic materials 0.000 claims description 3
- 229910052710 silicon Inorganic materials 0.000 claims description 3
- 239000010703 silicon Substances 0.000 claims description 3
- 239000002351 wastewater Substances 0.000 claims description 3
- 230000004048 modification Effects 0.000 claims description 2
- 238000012986 modification Methods 0.000 claims description 2
- 230000001699 photocatalysis Effects 0.000 abstract description 12
- 239000011229 interlayer Substances 0.000 abstract description 9
- 238000001179 sorption measurement Methods 0.000 abstract description 7
- 238000007873 sieving Methods 0.000 abstract description 6
- 238000006460 hydrolysis reaction Methods 0.000 abstract description 5
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 229910010413 TiO 2 Inorganic materials 0.000 abstract description 3
- 230000015572 biosynthetic process Effects 0.000 abstract 1
- RBTBFTRPCNLSDE-UHFFFAOYSA-N 3,7-bis(dimethylamino)phenothiazin-5-ium Chemical compound C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 RBTBFTRPCNLSDE-UHFFFAOYSA-N 0.000 description 12
- 229960000907 methylthioninium chloride Drugs 0.000 description 12
- 239000003054 catalyst Substances 0.000 description 5
- 238000010586 diagram Methods 0.000 description 4
- 229910001416 lithium ion Inorganic materials 0.000 description 4
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 4
- 239000010410 layer Substances 0.000 description 3
- HCWCAKKEBCNQJP-UHFFFAOYSA-N magnesium orthosilicate Chemical compound [Mg+2].[Mg+2].[O-][Si]([O-])([O-])[O-] HCWCAKKEBCNQJP-UHFFFAOYSA-N 0.000 description 3
- 239000000391 magnesium silicate Substances 0.000 description 3
- 229910052919 magnesium silicate Inorganic materials 0.000 description 3
- 235000019792 magnesium silicate Nutrition 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 239000004408 titanium dioxide Substances 0.000 description 3
- 101100152731 Arabidopsis thaliana TH2 gene Proteins 0.000 description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 239000004927 clay Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000009830 intercalation Methods 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- 229910052719 titanium Inorganic materials 0.000 description 2
- 239000010936 titanium Substances 0.000 description 2
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- JLVVSXFLKOJNIY-UHFFFAOYSA-N Magnesium ion Chemical compound [Mg+2] JLVVSXFLKOJNIY-UHFFFAOYSA-N 0.000 description 1
- 229910019092 Mg-O Inorganic materials 0.000 description 1
- 229910019395 Mg—O Inorganic materials 0.000 description 1
- 229910018557 Si O Inorganic materials 0.000 description 1
- 238000002835 absorbance Methods 0.000 description 1
- 239000003463 adsorbent Substances 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000000593 degrading effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- PAZHGORSDKKUPI-UHFFFAOYSA-N lithium metasilicate Chemical compound [Li+].[Li+].[O-][Si]([O-])=O PAZHGORSDKKUPI-UHFFFAOYSA-N 0.000 description 1
- FUJCRWPEOMXPAD-UHFFFAOYSA-N lithium oxide Chemical compound [Li+].[Li+].[O-2] FUJCRWPEOMXPAD-UHFFFAOYSA-N 0.000 description 1
- 229910001947 lithium oxide Inorganic materials 0.000 description 1
- 229910001425 magnesium ion Inorganic materials 0.000 description 1
- 239000000395 magnesium oxide Substances 0.000 description 1
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 1
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Inorganic materials [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000002522 swelling effect Effects 0.000 description 1
- 238000009281 ultraviolet germicidal irradiation Methods 0.000 description 1
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Classifications
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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
- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/06—Silicon, titanium, zirconium or hafnium; Oxides or hydroxides thereof
- B01J21/063—Titanium; Oxides or hydroxides thereof
-
- 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
- B01J23/02—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the alkali- or alkaline earth metals or beryllium
- B01J23/04—Alkali metals
-
- B01J35/39—
-
- 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
-
- 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
- C02F2101/30—Organic compounds
- C02F2101/308—Dyes; Colorants; Fluorescent agents
-
- 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
The invention relates to the technical field of photocatalysts and discloses a preparation method of a TiO 2/magnesium lithium silicate composite photocatalyst2The precursor solution is mixed and then put into a hydrothermal high-pressure reaction kettle for hydrothermal reaction for 3 to 24 hours at the temperature of 160-210 ℃, and TiO is added into the hydrothermal high-pressure reaction kettle while magnesium lithium silicate is formed2The precursor of (2) can also generate a hydrolysis reaction to generate TiO2TiO, since the formation of both is essentially simultaneous2More easily enter the interlayer of the magnesium lithium silicate. After the reaction is finished, cooling the obtained product to room temperature, and then centrifuging, washing, drying, grinding and sieving the product to finally obtain TiO2Magnesium lithium silicate product. The preparation method of the TiO 2/lithium magnesium silicate composite photocatalyst has the advantages of simple operation conditions, low production cost, increased interlayer spacing and specific surface area of the prepared photocatalyst, enhanced adsorption performance, good stability and higher photocatalytic activity.
Description
Technical Field
The invention relates to the technical field of photocatalysis, in particular to TiO2A preparation method of a magnesium lithium silicate composite photocatalyst.
Background
TiO2Is a typical n-type semiconductor material, is widely applied to the field of photocatalytic degradation of organic pollutants, has the advantages of no toxicity, low cost, good chemical and physical stability and the like, is considered to be one of the most promising photocatalysts at present, and is pure TiO2The band gap energy is higher, the sunlight utilization efficiency is low, the surface area and the porosity are small, the recycling is difficult, and the application range is limited.
The magnesium lithium silicate is a 2:1 layered clay which is formed by arranging Si-O tetrahedra and Mg-O octahedra in a 2:1 order in the vertical direction, the average interlayer spacing is about 1nm, the diameter is about 30nm, and Mg in a lamellar layer2+Is covered with Li+Instead of negatively charged, interlayer adsorption of Li+，Na+The cations between magnesium silicate and lithium are mainly Li+，Na+Compared with other 2:1 type clay materials, the material has better adsorption capacity, ion exchange property and swelling property, and is a good adsorbent and catalyst carrier.
At present TiO2The lithium magnesium silicate composite material is prepared by dispersing lithium magnesium silicate with water to form a dispersion, and then dispersing TiO2Adding the precursor solution into the dispersion, and reacting the mixed system at 60-90 ℃ for a period of time to ensure that the TiO is2Hydrolysis of the precursor to form TiO2Intercalation of lithium magnesium silicate between layers to give TiO2Magnesium lithium silicate photocatalyst.
Preparation of TiO by the above method2Magnesium lithium silicate photocatalyst, complex operation, long reaction time and formed TiO2It is often difficult to access siliconThe photocatalytic activity between the magnesium oxide and the lithium oxide is limited to a certain extent.
Disclosure of Invention
Technical problem to be solved
Aiming at the defects of the prior art, the invention provides a preparation method of a TiO 2/lithium magnesium silicate composite photocatalyst, which has the advantages of simple operation conditions, low production cost, increased interlayer spacing and specific surface area of the prepared photocatalyst, enhanced adsorption performance, good stability, higher photocatalytic activity and the like, and solves the problems that the traditional method for preparing the composite photocatalyst has longer reaction time and the formed TiO has higher photocatalytic activity2The interlayer of magnesium silicate and lithium silicate is difficult to enter, and the photocatalytic activity is limited.
(II) technical scheme
In order to achieve the purpose, the invention adopts the following technical scheme:
TiO22The preparation method of the magnesium lithium silicate composite photocatalyst comprises the following steps:
s1, preparing a precursor solution of the lithium magnesium silicate, and recording the precursor solution as a solution A;
s2 preparation of TiO2Adding the solution B into the solution A in S1 and fully mixing to carry out modification and inclusion on the magnesium lithium silicate;
s3, fully stirring the mixed solution of the solution A and the solution B, putting the mixed solution into a hydrothermal high-pressure reaction kettle, and carrying out hydrothermal reaction for 3-24h at the temperature of 160-210 ℃;
s4, after the reaction is finished, cooling the hydrothermal high-pressure reaction kettle to room temperature, pouring out a product, and centrifuging, washing, drying and grinding the product to obtain TiO2Magnesium lithium silicate composite photocatalyst.
Preferably, the preparation of the precursor of lithium magnesium silicate in step S1 specifically includes the following steps:
s1.1, weighing lithium fluoride, putting the lithium fluoride into a beaker, and adding deionized water for dispersing to obtain a lithium fluoride dispersion liquid;
s1.2, weighing anhydrous magnesium sulfate, putting the anhydrous magnesium sulfate into a beaker, adding deionized water to dissolve the anhydrous magnesium sulfate to obtain a magnesium sulfate solution, adding sodium hydroxide to react fully to obtain magnesium hydroxide precipitate, then performing suction filtration, washing with the deionized water, transferring the washed magnesium hydroxide into the lithium fluoride dispersion liquid in the S1.1, and stirring to form uniform mixed slurry;
s1.3, weighing water glass, wherein the water glass comprises 26% of silicon dioxide and 8.2% of sodium oxide by weight, sequentially adding water and hydrochloric acid, fully reacting to obtain solid silicon dioxide, carrying out suction filtration, washing with deionized water, and transferring the washed silicon dioxide to the mixed slurry of magnesium hydroxide and lithium fluoride in the S1.2 to obtain a precursor solution of the lithium magnesium silicate.
Preferably, TiO is prepared in the step S22The precursor specifically comprises the following steps:
s2.1, weighing tetrabutyl titanate and absolute ethyl alcohol;
s2.2, uniformly stirring tetrabutyl titanate and absolute ethyl alcohol;
and S2.3, adding the mixed solution obtained by mixing in the S2.2 into a precursor solution of the magnesium lithium silicate.
Preferably, the lithium content of the precursor solution of magnesium lithium silicate in step S1.3 is: magnesium: the molar ratio of silicon is (0.5-3.2): (5.5-4.4): 8.
preferably, the TiO is under ultraviolet light conditions2The magnesium lithium silicate composite photocatalyst is applied to catalytic degradation of organic dye wastewater.
(III) advantageous effects
The invention provides a TiO2The preparation method of the magnesium lithium silicate composite photocatalyst has the following advantages:
the invention directly adds magnesium lithium silicate precursor and TiO into the system2The precursor is subjected to hydrolysis reaction of titanium dioxide while preparing magnesium lithium silicate through one-step hydrothermal reaction, and TiO is directly prepared2The magnesium silicate lithium composite photocatalyst can change the negative charge carried by the layer surface by regulating and controlling the molar ratio of magnesium ions to lithium ions, and further influences the amount of titanium positive ions entering the interlayer, thereby influencing the structure of the composite.
The invention has short production process flow, simple operation condition and low production cost, and is prepared by TiO2Intercalation, the prepared photocatalyst has increased interlayer spacing and specific surface area, enhanced adsorption performance, good stability, easy recovery and higher photocatalytic activity.
Drawings
FIG. 1 shows TiO of the present invention2SEM image of magnesium lithium silicate composite photocatalyst;
FIG. 2 shows TiO of the present invention2XRD pattern of the magnesium lithium silicate composite photocatalyst;
FIG. 3 shows TiO under UV irradiation2A photocatalytic degradation diagram of the magnesium lithium silicate composite photocatalyst on MB.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1:
the invention provides a TiO2The preparation method of the magnesium lithium silicate composite photocatalyst comprises the following specific steps:
s1, weighing 0.1872g of lithium fluoride, putting the lithium fluoride into a beaker, and adding 200ml of deionized water for dispersion to obtain a lithium fluoride dispersion liquid;
s2, weighing 6.768g of anhydrous magnesium sulfate, placing the anhydrous magnesium sulfate into a beaker, adding 100ml of deionized water to dissolve the anhydrous magnesium sulfate to obtain a magnesium sulfate solution, adding 56.4ml of a 2mol/L sodium hydroxide solution, fully reacting to obtain a magnesium hydroxide precipitate, then performing suction filtration, washing with deionized water, transferring the washed magnesium hydroxide into the lithium fluoride dispersion liquid, and stirring to form uniform mixed slurry;
s3, weighing 18.46g of water glass (weight content: 26% of silicon dioxide and 8.2% of sodium oxide), adding 100ml of water, adding 16ml of 3mol/L hydrochloric acid, fully reacting to obtain solid silicon dioxide, then carrying out suction filtration, washing with deionized water, transferring the washed solid silicon dioxide into the mixed slurry of magnesium hydroxide and lithium fluoride, and uniformly stirring;
s4, weighing 1.1295g of tetrabutyl titanate, dissolving the tetrabutyl titanate in 10ml of absolute ethyl alcohol, fully stirring the solution for 30 minutes to form a transparent light yellow solution, adding the transparent light yellow solution into the mixed slurry obtained in the S3, putting the solution into a hydrothermal high-pressure reaction kettle, and carrying out hydrothermal reaction for 12 hours at 170 ℃;
fifthly, cooling the solution after the hydrothermal reaction to room temperature, centrifuging, washing, drying, grinding and sieving with a 400-mesh sieve to finally obtain TiO2The composite photocatalyst of magnesium lithium silicate is marked as TH-1.
Example 2:
the invention provides a TiO2The preparation method of the magnesium lithium silicate composite photocatalyst comprises the following specific steps:
s1, weighing 0.3432g of lithium fluoride, putting the lithium fluoride into a beaker, and adding 200ml of deionized water for dispersion to obtain a lithium fluoride dispersion liquid;
s2, weighing 6.408g of anhydrous magnesium sulfate, placing the anhydrous magnesium sulfate into a beaker, adding 100ml of deionized water to dissolve the anhydrous magnesium sulfate to obtain a magnesium sulfate solution, adding 53.3ml of 2mol/L sodium hydroxide solution, fully reacting to obtain magnesium hydroxide precipitate, then performing suction filtration, washing with deionized water, transferring the washed magnesium hydroxide into the lithium fluoride dispersion liquid, and stirring to form uniform mixed slurry;
s3, weighing 18.46g of water glass (weight content: 26% of silicon dioxide and 8.2% of sodium oxide), adding 100ml of water, adding 16ml of 3mol/L hydrochloric acid, fully reacting to obtain solid silicon dioxide, then carrying out suction filtration, and washing with deionized water. Transferring the washed solid silicon dioxide into the mixed slurry of the magnesium hydroxide and the lithium fluoride, and uniformly stirring;
s4, weighing 1.1295g of tetrabutyl titanate, dissolving the tetrabutyl titanate in 10ml of absolute ethyl alcohol, fully stirring the solution for 30 minutes to form a transparent light yellow solution, adding the transparent light yellow solution into the mixed slurry obtained in the S3, putting the solution into a hydrothermal high-pressure reaction kettle, and carrying out hydrothermal reaction for 4 hours at the temperature of 210 ℃;
s5, cooling the solution after the hydrothermal reaction to room temperature, centrifuging, washing, drying, grinding and sieving with a 400-mesh sieve to obtain TiO2The composite photocatalyst of magnesium lithium silicate is marked as TH-2.
Example 3:
the invention provides a TiO2The preparation method of the magnesium lithium silicate composite photocatalyst comprises the following specific steps:
s1, weighing 0.4992g of lithium fluoride, putting the lithium fluoride into a beaker, and adding 200ml of deionized water for dispersion to obtain a lithium fluoride dispersion liquid;
s2, weighing 6.048g of anhydrous magnesium sulfate, placing the anhydrous magnesium sulfate into a beaker, adding 100ml of deionized water to dissolve the anhydrous magnesium sulfate to obtain a magnesium sulfate solution, adding 50.4ml of 2mol/L sodium hydroxide solution, fully reacting to obtain magnesium hydroxide precipitate, then performing suction filtration, washing with deionized water, transferring the washed magnesium hydroxide into the lithium fluoride dispersion liquid, and stirring to form uniform mixed slurry;
s3, weighing 18.46g of water glass (weight content: 26% of silicon dioxide and 8.2% of sodium oxide), adding 100ml of water, adding 16ml of 3mol/L hydrochloric acid, fully reacting to obtain solid silicon dioxide, then carrying out suction filtration, washing with deionized water, transferring the washed solid silicon dioxide into the mixed slurry of the magnesium hydroxide and the lithium fluoride, and uniformly stirring;
s4, weighing 1.1295g of tetrabutyl titanate, dissolving the tetrabutyl titanate in 10ml of absolute ethyl alcohol, fully stirring the solution for 30 minutes to form a transparent light yellow solution, adding the transparent light yellow solution into the mixed slurry obtained in the S3, putting the solution into a hydrothermal high-pressure reaction kettle, and carrying out hydrothermal reaction for 10 hours at 180 ℃;
s5, cooling the solution after the hydrothermal reaction to room temperature, centrifuging, washing, drying, grinding and sieving with a 400-mesh sieve to obtain TiO2The composite photocatalyst of magnesium lithium silicate is marked as TH-3.
Example 4:
the invention provides a TiO2The preparation method of the magnesium lithium silicate composite photocatalyst comprises the following specific steps:
s1, weighing 0.6552g of lithium fluoride, putting the lithium fluoride into a beaker, and adding 200ml of deionized water for dispersion to obtain a lithium fluoride dispersion liquid;
s2, weighing 5.688g of anhydrous magnesium sulfate, placing the anhydrous magnesium sulfate into a beaker, adding 100ml of deionized water to dissolve the anhydrous magnesium sulfate to obtain a magnesium sulfate solution, adding 47.4ml of 2mol/L sodium hydroxide solution, fully reacting to obtain magnesium hydroxide precipitate, then performing suction filtration, washing with deionized water, transferring the washed magnesium hydroxide into the lithium fluoride dispersion liquid, and stirring to form uniform mixed slurry;
s3, weighing 18.46g of water glass (weight content: 26% of silicon dioxide and 8.2% of sodium oxide), adding 100ml of water, adding 16ml of 3mol/L hydrochloric acid, fully reacting to obtain solid silicon dioxide, then carrying out suction filtration, washing with deionized water, transferring the washed solid silicon dioxide into the mixed slurry of the magnesium hydroxide and the lithium fluoride, and uniformly stirring;
s4, weighing 1.1295g of tetrabutyl titanate, dissolving the tetrabutyl titanate in 10ml of absolute ethyl alcohol, fully stirring the solution for 30 minutes to form a transparent light yellow solution, adding the transparent light yellow solution into the mixed slurry obtained in the S3, putting the solution into a hydrothermal high-pressure reaction kettle, and carrying out hydrothermal reaction for 8 hours at 190 ℃;
s5, cooling the solution after the hydrothermal reaction to room temperature, centrifuging, washing, drying, grinding and sieving with a 400-mesh sieve to obtain TiO2The composite photocatalyst of magnesium lithium silicate is marked as TH-4.
Example 5:
the invention provides a TiO2The preparation method of the magnesium lithium silicate composite photocatalyst comprises the following specific steps:
s1, weighing 0.8112g of lithium fluoride, putting the lithium fluoride into a beaker, and adding 200ml of deionized water for dispersion to obtain a lithium fluoride dispersion liquid;
s2, weighing 5.328g of anhydrous magnesium sulfate, placing the anhydrous magnesium sulfate into a beaker, adding 100ml of deionized water to dissolve the anhydrous magnesium sulfate to obtain a magnesium sulfate solution, adding 44.4ml of 2mol/L sodium hydroxide solution, fully reacting to obtain magnesium hydroxide precipitate, then performing suction filtration, washing with deionized water, transferring the washed magnesium hydroxide into the lithium fluoride dispersion liquid, and stirring to form uniform mixed slurry;
s3, weighing 18.46g of water glass (weight content: 26% of silicon dioxide and 8.2% of sodium oxide), adding 100ml of water, adding 16ml of 3mol/L hydrochloric acid, fully reacting to obtain solid silicon dioxide, then carrying out suction filtration, washing with deionized water, transferring the washed solid silicon dioxide into the mixed slurry of the magnesium hydroxide and the lithium fluoride, and uniformly stirring;
s4, weighing 1.1295g of tetrabutyl titanate, dissolving the tetrabutyl titanate in 10ml of absolute ethyl alcohol, fully stirring the solution for 30 minutes to form a transparent light yellow solution, adding the transparent light yellow solution into the mixed slurry obtained in the S3, putting the solution into a hydrothermal high-pressure reaction kettle, and carrying out hydrothermal reaction for 12 hours at 180 ℃;
s5, cooling the solution after the hydrothermal reaction to room temperature, centrifuging, washing, drying, grinding and sieving with a 400-mesh sieve to obtain TiO2The composite photocatalyst of magnesium lithium silicate is marked as TH-5.
Referring to fig. 1, in fig. 1: a is an SEM atlas of the magnesium lithium silicate synthesized by adopting the prior art; b is the TiO prepared in example 12SEM atlas of composite magnesium lithium silicate photocatalyst (TH-1); c is TiO prepared in example 22SEM atlas of composite magnesium lithium silicate photocatalyst (TH-2); d is the TiO prepared in example 32SEM atlas of composite magnesium lithium silicate photocatalyst (TH-3); e is the TiO prepared in example 42SEM atlas of composite magnesium lithium silicate photocatalyst (TH-4); f is the TiO prepared in example 52SEM atlas of composite magnesium lithium silicate photocatalyst (TH-5);
from the obtained SEM spectrum result, compared with the magnesium lithium silicate with lamellar structure, the magnesium lithium silicate with lamellar structure is processed by TiO2The particle size of the intercalated lithium magnesium silicate composite material is obviously reduced, the intercalated lithium magnesium silicate composite material is shown to be a looser structure, and meanwhile, obvious pores can be observed, so that the specific surface area is increased, the adsorption performance is improved, and the photocatalytic performance is further improved.
Referring to fig. 2, TiO prepared in example 1, example 2, example 3, example 4 and example 5 are shown in fig. 2 from bottom to top, respectively2The XRD pattern corresponding to the magnesium lithium silicate composite photocatalyst shows that anatase phase TiO with good crystallinity is formed in all composite samples2The diffraction peaks of other impurity phases were small, and the partial diffraction peaks of magnesium lithium silicate were reduced or disappeared, indicating that the layered structure of magnesium lithium silicate was destroyed, but the skeleton remained.
The comprehensive analysis of examples 1 to 5 revealed that:
under the same condition, the hydrolysis reaction of the precursor for preparing the magnesium lithium silicate and the titanium dioxide is synchronously carried out, so that the titanium dioxide generated by hydrolysis can more easily enter the interlayer of the magnesium lithium silicate to obtain the titanium dioxideThe obtained product is subjected to physical treatment to finally obtain TiO2The composite material has the advantages of small particle size, high specific surface area, good stability and the like, and the preparation process flow is simple, the raw materials are easy to obtain, and the preparation process is clean and pollution-free, according to the SEN diagram of FIG. 1 and the XRD diagram of FIG. 2.
Experimental example:
TiO exposed to UV light as illustrated with reference to FIG. 32A photocatalytic degradation diagram of the magnesium lithium silicate composite photocatalyst on MB.
TiO2The photocatalytic performance of the magnesium lithium silicate composite photocatalyst is evaluated by the following method;
weighing 3mg TiO2Mixing the magnesium lithium silicate composite photocatalyst with 100ml of Methylene Blue (MB) solution with the concentration of 10mg/L, carrying out a photocatalytic experiment under the irradiation of 125w ultraviolet light after dark reaction for 30 minutes, taking samples every 10 minutes, centrifuging, taking supernate, and measuring the absorbance value of the supernate by using an ultraviolet spectrophotometer;
the removal rate R of MB is calculated by the following equation:
wherein R is the removal rate of MB, C0Initial concentration of MB solution, CtThe concentration of MB in the solution corresponding to time t is shown.
C in FIG. 30The initial concentration of the MB solution is shown, and C is the solution concentration of the MB corresponding to different time t; from the calculated removal rate R, TiO was found2The magnesium lithium silicate composite photocatalyst can obviously improve the photocatalytic activity of the catalyst, has smaller particle size and larger specific surface area, further improves the adsorption performance and the photocatalytic activity of the catalyst, and is prepared when the ratio of lithium: magnesium: the molar ratio of silicon is 1.32: 5.34: and 8, the photocatalytic degradation effect of the catalyst is best, and the removal rate of MB reaches 97.75 percent after the catalyst is irradiated by ultraviolet light for 60 minutes.
In conclusion, the TiO prepared by the process of the invention2Magnesium lithium silicate composite photocatalyst product, its preparation method and applicationThe catalytic performance of degrading methylene blue under the irradiation of ultraviolet light is excellent, and the method has wide application prospect in the field of treating organic dye wastewater through ultraviolet light catalytic degradation.
The above description is only for the purpose of illustrating certain embodiments of the present invention, and the scope of the present invention is not limited thereto, and any person skilled in the art can substitute or change the technical solution of the present invention and its inventive concept within the technical scope of the present invention.
Claims (5)
1. TiO22The preparation method of the magnesium lithium silicate composite photocatalyst is characterized by comprising the following steps:
s1, preparing a precursor solution of the lithium magnesium silicate, and recording the precursor solution as a solution A;
s2 preparation of TiO2Adding the solution B into the solution A in S1 and fully mixing to carry out modification and inclusion on the magnesium lithium silicate;
s3, fully stirring the mixed solution of the solution A and the solution B, putting the mixed solution into a hydrothermal high-pressure reaction kettle, and carrying out hydrothermal reaction for 3-24h at the temperature of 160-210 ℃;
s4, after the reaction is finished, cooling the hydrothermal high-pressure reaction kettle to room temperature, pouring out a product, and centrifuging, washing, drying and grinding the product to obtain TiO2Magnesium lithium silicate composite photocatalyst.
2. A TiO according to claim 12The preparation method of the magnesium lithium silicate composite photocatalyst is characterized in that the preparation of the precursor of the magnesium lithium silicate in the step S1 specifically comprises the following steps:
s1.1, weighing lithium fluoride, putting the lithium fluoride into a beaker, and adding deionized water for dispersing to obtain a lithium fluoride dispersion liquid;
s1.2, weighing anhydrous magnesium sulfate, putting the anhydrous magnesium sulfate into a beaker, adding deionized water to dissolve the anhydrous magnesium sulfate to obtain a magnesium sulfate solution, adding sodium hydroxide to react fully to obtain magnesium hydroxide precipitate, then performing suction filtration, washing with the deionized water, transferring the washed magnesium hydroxide into the lithium fluoride dispersion liquid in the S1.1, and stirring to form uniform mixed slurry;
s1.3, weighing water glass, wherein the water glass comprises 26% of silicon dioxide and 8.2% of sodium oxide by weight, sequentially adding water and hydrochloric acid, fully reacting to obtain solid silicon dioxide, carrying out suction filtration, washing with deionized water, and transferring the washed silicon dioxide to the mixed slurry of magnesium hydroxide and lithium fluoride in the S1.2 to obtain a precursor solution of the lithium magnesium silicate.
3. A TiO according to claim 22The preparation method of the magnesium lithium silicate composite photocatalyst is characterized in that lithium in a precursor solution of magnesium lithium silicate in the step S1.3 is as follows: magnesium: the molar ratio of silicon is (0.5-3.2): (5.5-4.4): 8.
4. a TiO according to claim 1 or 32The preparation method of the magnesium lithium silicate composite photocatalyst is characterized in that TiO is prepared in step S22The precursor specifically comprises the following steps:
s2.1, weighing tetrabutyl titanate and absolute ethyl alcohol;
s2.2, uniformly stirring tetrabutyl titanate and absolute ethyl alcohol;
and S2.3, adding the mixed solution obtained by mixing in the S2.2 into a precursor solution of the magnesium lithium silicate.
5. A TiO according to claim 42Preparation method of magnesium lithium silicate composite photocatalyst, and TiO prepared under ultraviolet light condition2The magnesium lithium silicate composite photocatalyst is applied to catalytic degradation of organic dye wastewater.
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| CN115770605A (en) * | 2022-12-29 | 2023-03-10 | 上海大学 | Preparation of graphite-phase carbon nitride/titanium dioxide/magnesium lithium silicate composite photocatalyst |
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