CN108620053B - Method for preparing sodium metatitanate-potassium tetratitanate composite catalytic material by molten salt method - Google Patents
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- 238000000034 method Methods 0.000 title claims abstract description 45
- 239000000463 material Substances 0.000 title claims abstract description 30
- 229910052700 potassium Inorganic materials 0.000 title claims abstract description 28
- 239000011591 potassium Substances 0.000 title claims abstract description 28
- 230000003197 catalytic effect Effects 0.000 title claims abstract description 26
- 239000002131 composite material Substances 0.000 title claims abstract description 26
- 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 25
- 229910052708 sodium Inorganic materials 0.000 title claims abstract description 25
- 239000011734 sodium Substances 0.000 title claims abstract description 25
- 150000003839 salts Chemical class 0.000 title claims abstract description 19
- 239000002994 raw material Substances 0.000 claims abstract description 15
- 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 abstract description 14
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 14
- 238000002360 preparation method Methods 0.000 claims abstract description 13
- 239000002243 precursor Substances 0.000 claims abstract description 12
- 229910002651 NO3 Inorganic materials 0.000 claims abstract description 11
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims abstract description 11
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 23
- 238000001035 drying Methods 0.000 claims description 10
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Inorganic materials [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 claims description 10
- 238000001354 calcination Methods 0.000 claims description 8
- 238000002156 mixing Methods 0.000 claims description 7
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Inorganic materials [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 claims description 7
- 238000005406 washing Methods 0.000 claims description 7
- 229910019016 NaNO3—KNO3 Inorganic materials 0.000 claims description 6
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 5
- 238000002844 melting Methods 0.000 claims description 5
- 230000008018 melting Effects 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- 238000005119 centrifugation Methods 0.000 claims description 3
- 238000001291 vacuum drying Methods 0.000 claims description 3
- 230000007062 hydrolysis Effects 0.000 claims 1
- 238000006460 hydrolysis reaction Methods 0.000 claims 1
- 239000002127 nanobelt Substances 0.000 abstract description 8
- 238000004519 manufacturing process Methods 0.000 abstract description 7
- 239000006184 cosolvent Substances 0.000 abstract description 6
- 230000001699 photocatalysis Effects 0.000 abstract description 4
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 abstract 1
- 239000003344 environmental pollutant Substances 0.000 abstract 1
- 229910052739 hydrogen Inorganic materials 0.000 abstract 1
- 239000001257 hydrogen Substances 0.000 abstract 1
- 238000013033 photocatalytic degradation reaction Methods 0.000 abstract 1
- 231100000719 pollutant Toxicity 0.000 abstract 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 10
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 8
- 239000004408 titanium dioxide Substances 0.000 description 8
- 238000005245 sintering Methods 0.000 description 5
- 238000002474 experimental method Methods 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 238000004321 preservation Methods 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 238000002425 crystallisation Methods 0.000 description 3
- NJLLQSBAHIKGKF-UHFFFAOYSA-N dipotassium dioxido(oxo)titanium Chemical compound [K+].[K+].[O-][Ti]([O-])=O NJLLQSBAHIKGKF-UHFFFAOYSA-N 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 229910052783 alkali metal Inorganic materials 0.000 description 2
- -1 alkali metal cations Chemical class 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 230000008025 crystallization Effects 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000005342 ion exchange Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000002070 nanowire Substances 0.000 description 2
- 239000004323 potassium nitrate Substances 0.000 description 2
- 235000010333 potassium nitrate Nutrition 0.000 description 2
- 239000002002 slurry Substances 0.000 description 2
- 239000004317 sodium nitrate Substances 0.000 description 2
- 235000010344 sodium nitrate Nutrition 0.000 description 2
- 238000003746 solid phase reaction Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000003917 TEM image Methods 0.000 description 1
- 229910003083 TiO6 Inorganic materials 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000012024 dehydrating agents Substances 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- 238000007716 flux method Methods 0.000 description 1
- 238000007499 fusion processing Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 230000003301 hydrolyzing effect Effects 0.000 description 1
- 238000010335 hydrothermal treatment Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000011229 interlayer Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 150000002736 metal compounds Chemical class 0.000 description 1
- 229910000000 metal hydroxide Inorganic materials 0.000 description 1
- 150000004692 metal hydroxides Chemical class 0.000 description 1
- MEFBJEMVZONFCJ-UHFFFAOYSA-N molybdate Chemical compound [O-][Mo]([O-])(=O)=O MEFBJEMVZONFCJ-UHFFFAOYSA-N 0.000 description 1
- 125000000896 monocarboxylic acid group Chemical group 0.000 description 1
- 239000002121 nanofiber Substances 0.000 description 1
- 239000002074 nanoribbon Substances 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Substances [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 description 1
- 229910000027 potassium carbonate Inorganic materials 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- GROMGGTZECPEKN-UHFFFAOYSA-N sodium metatitanate Chemical compound [Na+].[Na+].[O-][Ti](=O)O[Ti](=O)O[Ti]([O-])=O GROMGGTZECPEKN-UHFFFAOYSA-N 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- PBYZMCDFOULPGH-UHFFFAOYSA-N tungstate Chemical compound [O-][W]([O-])(=O)=O PBYZMCDFOULPGH-UHFFFAOYSA-N 0.000 description 1
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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
- 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
-
- 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
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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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
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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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/40—Catalysts, in general, characterised by their form or physical properties characterised by dimensions, e.g. grain size
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01J2523/00—Constitutive chemical elements of heterogeneous catalysts
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Abstract
The invention relates to a method for preparing a sodium metatitanate-potassium tetratitanate composite catalytic material by a molten salt method with mixed nitrate as a cosolvent, belonging to the technical field of material preparation. The invention takes tetrabutyl titanate as raw material to prepare TiO by a hydrothermal method2And adding mixed nitrate as a cosolvent into the material precursor, and preparing the sodium metatitanate-potassium tetratitanate composite catalytic material by a nitrate molten salt method. The method has the advantages of simple and controllable preparation conditions, simple equipment and process, high yield, low cost and the like. The obtained product is a nanobelt which is 6-13 microns long and about 200 nanometers wide, and has wide application prospects in the aspects of photocatalytic degradation of pollutants, photocatalytic hydrogen production and the like.
Description
Technical Field
The invention relates to a method for preparing a sodium metatitanate-potassium tetratitanate composite catalytic material by a melting method, belonging to the technical field of material preparation.
Background
Titanates are semiconductor layered metal compounds with high photocatalytic activity discovered at present, and have the advantages of good photo-corrosion resistance, high activity and the like, so that extensive research attention is drawn. The layered titanate has a layered skeleton made of octahedral TiO6Are connected with each other in a mode of being in common edges or common angles, spread to form two-dimensional layered oxide with negative charges, and alkali metal cations are contained between the layers with the negative charges. And the alkali metal cations have interlayer ion exchange performance, excellent adsorption performance and higher chemical activity. In addition, the layered structure can keep good stability during ion exchange, and can adsorb harmful heavy metal ions, thereby achieving the effect of purifying water quality. At present, many methods for preparing titanates are widely studied, mainly including a melting method, a cosolvent method, a sintering method, a kdc (sintering crystallization) method, and a hydrothermal method.
The melting method is characterized in that titanium dioxide and carbonate are used as raw materials, the titanium dioxide and the carbonate are uniformly mixed in proportion, the mixture is melted at a high temperature of 1200-1500 ℃, and then cooling crystallization is carried out to prepare titanate whiskers finally. The method can obtain single crystals with higher purity, the product has good crystallinity, but the yield is lower, and the reaction temperature is higher. Shen et al reported the preparation of potassium titanate nanowires by the fusion process, using TiO2And K2CO3Raw materials are adopted, and the mass ratio of the materials is 3: 1 are mixed togetherGrinding uniformly, roasting at 1000 ℃ for 2 hours, and finally preparing the potassium titanate nanofiber.
The flux method is characterized in that titanium dioxide and carbonate are used as raw materials, corresponding tungstate or molybdate is used as a flux to be mixed with the raw materials, the mixture is melted at the high temperature of 900-1300 ℃, so that supersaturated molten liquid is formed, crystals are separated out from the supersaturated molten liquid, and the titanate nanobelt is obtained. The method has high yield and good crystallinity, but the fluxing agent and the separation cost are high, and the cost is higher.
The sintering method is to take titanium dioxide and carbonate as raw materials, mix the raw materials evenly, and then place the mixture at a high temperature of 600-1200 ℃ for solid phase reaction, and finally prepare the titanate nanoribbon. The method has the advantages of low cost, simple process, convenient operation, high yield of the finally prepared titanate and suitability for industrial production, but has the defects of overhigh reaction temperature, long production period, high energy consumption, high crystallinity of the prepared product and the like. In addition, some improved methods, such as a rapid cooling sintering crystallization method, are provided, wherein titanium dioxide and carbonate are used as raw materials, the raw materials are uniformly mixed and then placed at the temperature of 900-1200 ℃ for solid phase reaction, then a sample is rapidly cooled in the air, and finally titanate whiskers are prepared through heat treatment. However, the method needs two times of high-temperature treatment, and has high energy consumption and high production cost. The KDC method also belongs to an improved sintering method, and the method is characterized in that titanium dioxide and carbonate are used as raw materials and mixed with water to form slurry, and the slurry is dried and then reacts at the temperature of 1000-1100 ℃ to prepare titanate whiskers. The product prepared by the method has better crystallinity, but the process is more complicated. Alnano et al prepared P25 as a starting material by hydrothermal reaction in 17M KOH at 110 ℃. The products after hydrothermal treatment are respectively treated with CH3And washing the COOH aqueous solution and deionized water, and roasting at 400-700 ℃ to finally prepare the potassium titanate nanowire.
The hydrothermal method is to take metal hydroxide and carbonate as raw materials, carry out hydrothermal reaction on aqueous solution and titanium dioxide under high pressure, and finally prepare titanate nano-whisker. The method has high yield, can obtain the crystal whisker with larger diameter and length, but needs to strictly control parameters such as temperature, alkalinity, reaction time and the like, and has high cost and danger. And preparing the potassium hexatitanate whisker by using Gier and Salzberg under the conditions of 600-700 ℃ and 500-4000 atm. Toshitaka and the like adopt hydrated titanium dioxide as a raw material, and metal Zn is used as a dehydrating agent to prepare potassium hexatitanate whiskers at 390 ℃ and 150-200 atm.
The method needs to prepare the sample under the high-temperature condition, and the invention adopts a molten salt method, replaces carbonate with nitrate with lower melting point, lowers the calcining temperature and prepares the titanate material. In addition, the titanate photocatalysis performance is improved through the compounding of the titanates with different shapes.
Disclosure of Invention
The invention aims to provide a method for preparing a sodium metatitanate-potassium tetratitanate composite catalytic material by a molten salt method with mixed nitrate as a cosolvent; the method takes tetrabutyl titanate as a raw material to prepare TiO by hydrothermal method2Preparing a sodium metatitanate-potassium tetratitanate composite catalytic material by a molten salt method by taking mixed nitrate as a cosolvent; the method has the advantages of convenient and controllable preparation conditions, simple equipment and process, high product yield, low cost and the like; the obtained sodium metatitanate-potassium tetratitanate composite catalytic material is in a shape of a nanobelt, the surface of the nanobelt is smooth, edges and corners are clear, the length is about 6-13 microns, and the width is about 200 nanometers. The composite material has excellent photocatalytic performance.
The molten salt method for preparing the sodium metatitanate-potassium tetratitanate composite catalytic material is characterized in that tetrabutyl titanate is hydrolyzed and then mixed nitrate is molten to prepare the sodium metatitanate-potassium tetratitanate composite catalytic material, and the molten salt method comprises the following steps:
(1) taking tetrabutyl titanate solution as a raw material, carrying out hydrothermal reaction, and then carrying out centrifugation, washing and drying to prepare TiO2A precursor;
(2) the obtained TiO is2Precursor and NaNO3-KNO3And uniformly mixing the mixed salt, calcining, naturally cooling, washing and drying to obtain the sodium metatitanate-potassium tetratitanate composite catalytic material.
In the above production method, the tetrabutyl titanate and the nitrate in the step (1) are respectively commercially available tetrabutyl titanate.
In the above production method, the operation in the step (1) is carried out under stirring.
In the above preparation method, in the step (1), TiO is prepared by a hydrothermal method2In the precursor, the temperature of the hydrothermal reaction is 80-200 ℃.
In the preparation method, the heat preservation time at the hydrothermal reaction temperature in the step (1) is 12 to 48 hours.
In the preparation method, the drying mode in the steps (1) and (2) adopts vacuum drying at 50-100 ℃.
In the above preparation method, the mixed salt in the step (2) is commercially available NaNO3And KNO3。
In the above production method, NaNO in the step (2)3And KNO3The mixed mass ratio is controlled to be 5: 1 to 1: 5, or more.
In the above production method, TiO in the step (2)2Precursor sample and NaNO3-KNO3The mixing mass ratio of the mixed salt is controlled to be 5: 1 to 1: 5, or more.
In the above preparation method, the calcination temperature in the step (2) is 300-800 ℃.
In the preparation method, the heat preservation time at the calcining temperature in the step (2) is 2-6 hours.
The sodium metatitanic acid-potassium tetratitanate composite catalytic material prepared by the technology has the characteristics of simple equipment and process, strict and controllable preparation conditions, high product yield, low cost and the like, and the obtained sodium metatitanic acid-potassium tetratitanate composite catalytic material is in a nano-belt shape and has excellent catalytic performance.
Drawings
FIG. 1 is an XRD spectrum of a sodium metatitanate-potassium tetratitanate composite catalytic material prepared in example 1 of the present invention
FIG. 2 is a transmission electron micrograph of a sodium metatitanate-potassium tetratitanate composite catalytic material prepared in example 1 of the present invention
Detailed Description
The technical solution of the present invention is further illustrated by the following examples.
The invention provides a method for preparing a sodium metatitanate-potassium tetratitanate composite catalytic material by a molten salt method with mixed nitrate as a cosolvent, which is characterized in that the method prepares the sodium metatitanate-potassium tetratitanate composite catalytic material by hydrolyzing tetrabutyl titanate and using nitrate molten salt, and comprises the following steps and contents:
(1) the adopted tetrabutyl titanate, sodium nitrate and potassium nitrate are respectively tetrabutyl titanate, sodium nitrate and potassium nitrate which are sold in the market.
(2) The experimental work was carried out with stirring.
(3) The hydrothermal reaction of tetrabutyl titanate was slowly carried out, followed by centrifugation and drying.
(4) The hydrothermal reaction temperature of the experiment is 80-200 ℃, and the heat preservation time is 12-48 hours.
(5) The experimental drying temperature is 50-100 ℃.
(6) The obtained TiO is2Precursor sample and NaNO3-KNO3Mixing the mixed salt, calcining, naturally cooling, fully washing and drying to obtain the sodium metatitanate-potassium tetratitanate composite catalytic material.
(7) NaNO in the experiment3And KNO3The mixed mass ratio is controlled to be 5: 1 to 1: 5, or more.
(8) In the experiment TiO2Precursor sample and NaNO3-KNO3The mixing mass ratio of the mixed salt is controlled to be 5: 1 to 1: 5 between
(9) The calcination temperature of the experiment is 300-800 ℃, and the heat preservation time is 2-6 hours.
The prepared sodium metatitanate-potassium tetratitanate composite catalytic material is white powder in appearance.
Under a transmission electron microscope, a large amount of nano-belt-shaped substances can be observed, the surface of the nano-belt is smooth, the edge angle is clear, the length is about 6-13 micrometers, and the width is about 200 nanometers. XRD measurements showed sodium metatitanate and potassium tetratitanate.
In conclusion, the composite catalytic material of sodium metatitanate-potassium tetratitanate can be obtained by the technology.
Example (b): slowly mixing 5ml of acetic acid solution with 2ml of tetrabutyl titanate under the stirring action, continuously stirring for 30min, carrying out hydrothermal reaction at 150 ℃ for 24h, and carrying out vacuum drying on the centrifuged sample at 60 ℃ to obtain TiO2And (3) precursor samples.
Then adding TiO2Precursor sample, NaNO3And KNO3And (3) adding the following components in percentage by weight of 5: 1: 1, calcining for 4 hours at 350 ℃, fully washing and drying to obtain the sodium metatitanate-potassium tetratitanate composite catalytic material.
The prepared sodium metatitanate-potassium tetratitanate composite catalytic material (shown in figure 1) is in a nano-belt shape, the surface of the nano-belt is smooth, edges and corners are clear, the length is about 6-13 microns, and the width is about 200 nanometers (shown in figure 2).
Claims (1)
1. The molten salt preparation method of the sodium metatitanate-potassium tetratitanate composite catalytic material is characterized by comprising the following steps of: the method prepares the sodium metatitanate-potassium tetratitanate composite catalytic material by hydrolysis of tetrabutyl titanate and melting action of nitrate, and comprises the following steps:
(1) taking tetrabutyl titanate solution as a raw material, slowly adding tetrabutyl titanate under the stirring action, carrying out hydrothermal reaction at the temperature of 80-200 ℃, keeping the temperature for 12-48 hours, then carrying out centrifugation, washing and drying, and carrying out vacuum drying at the temperature of 50-100 ℃ in a drying mode to obtain TiO2A precursor;
(2) the obtained TiO is2Precursor and NaNO3-KNO3Mixing the mixed salt with NaNO3And KNO3The mass ratio of (A) is controlled to be 5: 1 to 1: 5 between, TiO2Precursor and NaNO3-KNO3The mixing mass ratio of the mixed salt is also controlled to be 5: 1 to 1: and 5, calcining at the temperature of 300-800 ℃, keeping the temperature for 2-6 hours, naturally cooling, washing and drying to obtain the sodium metatitanate-potassium tetratitanate composite catalytic material.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103881662A (en) * | 2013-01-25 | 2014-06-25 | 深圳市爱能森科技有限公司 | Ternary nitric acid nano-molten salt heat transfer and storage medium, preparation method and application thereof |
| CN103894177A (en) * | 2014-04-01 | 2014-07-02 | 江西理工大学 | Method for synthesizing rare earth doped potassium titanate powder with photocatalytic activity |
| CN106554035A (en) * | 2015-09-24 | 2017-04-05 | 中国科学院上海硅酸盐研究所 | The method that Sr titanate powder is prepared using molten-salt growth method |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103881662A (en) * | 2013-01-25 | 2014-06-25 | 深圳市爱能森科技有限公司 | Ternary nitric acid nano-molten salt heat transfer and storage medium, preparation method and application thereof |
| CN103894177A (en) * | 2014-04-01 | 2014-07-02 | 江西理工大学 | Method for synthesizing rare earth doped potassium titanate powder with photocatalytic activity |
| CN106554035A (en) * | 2015-09-24 | 2017-04-05 | 中国科学院上海硅酸盐研究所 | The method that Sr titanate powder is prepared using molten-salt growth method |
Non-Patent Citations (1)
| Title |
|---|
| Enhanced visible photocatalytic activity of nitrogen doped singlecrystal-like TiO2 by synergistic treatment with urea and mixed nitrates;Chenxi Li et al.;《J. Mater. Res.》;20170228;第32卷(第4期);摘要部分，第738页左栏最后1段至右栏第1段，结论部分 * |
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