CN109289829B - Method for preparing zinc gadolinium oxide powder by vapor deposition - Google Patents
Method for preparing zinc gadolinium oxide powder by vapor deposition Download PDFInfo
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- CN109289829B CN109289829B CN201811202125.7A CN201811202125A CN109289829B CN 109289829 B CN109289829 B CN 109289829B CN 201811202125 A CN201811202125 A CN 201811202125A CN 109289829 B CN109289829 B CN 109289829B
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- 239000000843 powder Substances 0.000 title claims abstract description 42
- OZKRUQCUAKLSTB-UHFFFAOYSA-N zinc gadolinium(3+) oxygen(2-) Chemical compound [O-2].[Zn+2].[Gd+3] OZKRUQCUAKLSTB-UHFFFAOYSA-N 0.000 title claims abstract description 41
- 238000007740 vapor deposition Methods 0.000 title claims abstract description 17
- 238000000034 method Methods 0.000 title claims abstract description 13
- 239000000243 solution Substances 0.000 claims abstract description 36
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 24
- 239000010453 quartz Substances 0.000 claims abstract description 22
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 22
- RFYTWKQWFTUQKQ-UHFFFAOYSA-N [Zn].[Gd] Chemical compound [Zn].[Gd] RFYTWKQWFTUQKQ-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000002243 precursor Substances 0.000 claims abstract description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 14
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 12
- YRKCREAYFQTBPV-UHFFFAOYSA-N acetylacetone Chemical compound CC(=O)CC(C)=O YRKCREAYFQTBPV-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000010438 heat treatment Methods 0.000 claims abstract description 12
- 238000002347 injection Methods 0.000 claims abstract description 11
- 239000007924 injection Substances 0.000 claims abstract description 11
- NWGKJDSIEKMTRX-AAZCQSIUSA-N Sorbitan monooleate Chemical compound CCCCCCCC\C=C/CCCCCCCC(=O)OC[C@@H](O)[C@H]1OC[C@H](O)[C@H]1O NWGKJDSIEKMTRX-AAZCQSIUSA-N 0.000 claims abstract description 6
- ZOIORXHNWRGPMV-UHFFFAOYSA-N acetic acid;zinc Chemical compound [Zn].CC(O)=O.CC(O)=O ZOIORXHNWRGPMV-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000001354 calcination Methods 0.000 claims abstract description 6
- 238000001816 cooling Methods 0.000 claims abstract description 6
- 239000008367 deionised water Substances 0.000 claims abstract description 6
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 6
- 239000003995 emulsifying agent Substances 0.000 claims abstract description 6
- MWFSXYMZCVAQCC-UHFFFAOYSA-N gadolinium(iii) nitrate Chemical compound [Gd+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O MWFSXYMZCVAQCC-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000011259 mixed solution Substances 0.000 claims abstract description 6
- 238000002156 mixing Methods 0.000 claims abstract description 6
- 238000003756 stirring Methods 0.000 claims abstract description 6
- 239000004246 zinc acetate Substances 0.000 claims abstract description 6
- 239000000463 material Substances 0.000 claims description 14
- 230000001699 photocatalysis Effects 0.000 claims description 11
- 239000002131 composite material Substances 0.000 claims description 10
- 238000002360 preparation method Methods 0.000 claims description 7
- 239000002245 particle Substances 0.000 claims description 6
- 239000011148 porous material Substances 0.000 claims description 6
- 239000000126 substance Substances 0.000 claims description 6
- 239000002994 raw material Substances 0.000 claims description 5
- 238000000746 purification Methods 0.000 abstract description 6
- 238000005286 illumination Methods 0.000 abstract description 4
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 8
- 229910052688 Gadolinium Inorganic materials 0.000 description 5
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 5
- UIWYJDYFSGRHKR-UHFFFAOYSA-N gadolinium atom Chemical compound [Gd] UIWYJDYFSGRHKR-UHFFFAOYSA-N 0.000 description 5
- 229910052725 zinc Inorganic materials 0.000 description 5
- 239000011701 zinc Substances 0.000 description 5
- 239000011787 zinc oxide Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 2
- 239000003344 environmental pollutant Substances 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 239000002957 persistent organic pollutant Substances 0.000 description 2
- 231100000719 pollutant Toxicity 0.000 description 2
- 239000010865 sewage Substances 0.000 description 2
- 231100000331 toxic Toxicity 0.000 description 2
- 230000002588 toxic effect Effects 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 238000002306 biochemical method Methods 0.000 description 1
- 230000033558 biomineral tissue development Effects 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000033116 oxidation-reduction process Effects 0.000 description 1
- 239000011941 photocatalyst Substances 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
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
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/10—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of rare earths
-
- 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
-
- 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
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/10—Photocatalysts
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Hydrology & Water Resources (AREA)
- Water Supply & Treatment (AREA)
- Environmental & Geological Engineering (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Toxicology (AREA)
- Catalysts (AREA)
- Luminescent Compositions (AREA)
Abstract
A method for preparing zinc gadolinium oxide powder by vapor deposition comprises sequentially adding ethanol, zinc acetate, span 80 as emulsifier, and acetylacetone into flask, heating the solution to 65 deg.C, and maintaining the temperature at the temperature to obtain solution A; sequentially adding deionized water, ethanol, gadolinium nitrate and 1mol/L hydrochloric acid solution into a beaker, and uniformly stirring to obtain a solution B; and uniformly mixing the solution A and the solution B, heating the mixed solution to 65 ℃, and preserving heat at the temperature to obtain the zinc-gadolinium precursor. Introducing a quartz tube from the outside of the box-type electric furnace to the center of the furnace chamber, and keeping the temperature of the electric furnace at 660-710 ℃; injecting a zinc-gadolinium precursor into the electric furnace from the quartz tube; and after the injection is finished, continuously calcining at 660-710 ℃, and cooling to obtain the zinc gadolinium oxide powder. The zinc gadolinium oxide powder can degrade organic matters in water into inorganic micromolecules under illumination, and is suitable for various water purification fields of industry, civil use and the like.
Description
Technical Field
The invention belongs to the field of water purification materials, and particularly relates to a method for preparing zinc gadolinium oxide powder by vapor deposition.
Background
Sewage contains a wide variety of pollutants including many toxic and harmful organic pollutants. Conventional water treatment methods such as biochemical methods have difficulty in acting on such pollutants, and are replaced with advanced oxidation techniques such as photocatalytic purification techniques. The photocatalytic purification technology can excite the photocatalyst under the action of illumination and generate substances with high-efficiency oxidation-reduction capability, so that toxic and harmful organic pollutants in sewage can be oxidized and decomposed, and the effect of complete mineralization and decomposition is achieved. To achieve this, it is necessary to provide a photocatalytic material having a strong activity. In the last 50 years, research and exploration on various novel photocatalytic materials are one of the most important research contents in the field. In addition to the most common photocatalytic materials based on titanium oxide, zinc-containing gadolinium-containing materials are also an important class of photocatalytic materials, but research on such materials is still lacking, and products with real practical value are lacking. The influence of different preparation methods on the material properties is enormous, and intensive research on various preparation methods is required in order to obtain materials with excellent properties.
Disclosure of Invention
Aiming at the problems in the prior art, the invention aims to provide a method for preparing zinc gadolinium oxide powder by vapor deposition. The zinc gadolinium oxide powder can degrade organic matters in water into inorganic micromolecules under illumination, and is suitable for various water purification fields of industry, civil use and the like.
The technical scheme is as follows:
a method for preparing zinc gadolinium oxide powder by vapor deposition comprises the following preparation steps:
firstly, preparing a zinc-gadolinium precursor
Step 1: adding 390mL of ethanol, 12-17 g of zinc acetate, 7-10 g of emulsifier span 80 and 3-5 mL of acetylacetone into a 500mL flask in sequence, heating the solution to 65 ℃, and preserving the temperature for 60min at the temperature to obtain a solution A, wherein the used chemical raw materials are pure materials;
step 2: sequentially adding 150mL of deionized water, 120mL of ethanol, 9-12 g of gadolinium nitrate and 6-8 mL of 1mol/L hydrochloric acid solution into a beaker, and uniformly stirring to obtain a solution B, wherein the used chemical raw materials are pure materials;
and step 3: and uniformly mixing the solution A and the solution B, heating the mixed solution to 65 ℃, and preserving heat for 60min at the temperature to obtain the zinc-gadolinium precursor.
Second, vapor deposition
And 4, step 4: introducing a quartz tube from the outside of the box-type electric furnace to the center of the furnace chamber, wherein the inner diameter of the quartz tube is 7mm, the inner diameter of the quartz tube at the tail end outlet of the center of the furnace chamber is 0.6mm, and the temperature of the electric furnace is kept at 660-710 ℃;
and 5: injecting the zinc-gadolinium precursor prepared in the step (3) into an electric furnace from a quartz tube, wherein the injection flow is 20 mL/min;
step 6: and after the injection is finished, continuously calcining for 3 hours at the temperature of 660-710 ℃, and cooling to obtain the zinc gadolinium oxide powder.
The prepared zinc gadolinium oxide powder has the following technical characteristics: the zinc gadolinium oxide powder consists of zinc and gadolinium composite oxides, wherein the mass percentage of zinc oxide is 70-90%; the particle size range of the zinc gadolinium oxide powder is 3-10 μm, and the specific surface area is 160-230 m2(ii) a total pore volume of 0.12 to 0.20cm3(ii)/g; the zinc gadolinium oxide powder can be excited by light with the wavelength less than 530nm to generate photocatalytic activity.
Compared with the prior art, the method for preparing the zinc gadolinium oxide powder by vapor deposition has the advantages that:
the zinc-gadolinium precursor is injected into a high-temperature box type electric furnace, and the zinc-gadolinium oxide powder is prepared through vapor deposition oxidation, so that the agglomeration of fine powder can be inhibited, and the composite zinc-gadolinium oxide powder with narrow particle size range, large specific surface area and large pore volume can be prepared. The zinc gadolinium oxide powder can degrade organic matters in water into inorganic micromolecules under illumination, and is suitable for various water purification fields of industry, civil use and the like.
Detailed Description
The chemical raw materials used in the following examples are all pure materials.
Example 1
A method for preparing zinc gadolinium oxide powder by vapor deposition comprises the following preparation steps:
firstly, preparing a zinc-gadolinium precursor
Step 1: adding 390mL of ethanol, 12g of zinc acetate, 7g of emulsifier span 80 and 3mL of acetylacetone into a 500mL flask in sequence, heating the solution to 65 ℃, and preserving heat for 60min at the temperature to obtain a solution A;
step 2: sequentially adding 150mL of deionized water, 120mL of ethanol, 9g of gadolinium nitrate and 6mL of 1mol/L hydrochloric acid solution into a beaker, and uniformly stirring to obtain a solution B;
and step 3: and uniformly mixing the solution A and the solution B, heating the mixed solution to 65 ℃, and preserving heat for 60min at the temperature to obtain the zinc-gadolinium precursor.
Second, vapor deposition
And 4, step 4: introducing a quartz tube from the outside of the box-type electric furnace to the center of the furnace chamber, wherein the inner diameter of the quartz tube is 7mm, the inner diameter of the quartz tube at the tail end outlet of the center of the furnace chamber is 0.6mm, and the temperature of the electric furnace is kept at 660 ℃;
and 5: injecting the zinc-gadolinium precursor prepared in the step (3) into an electric furnace from a quartz tube, wherein the injection flow is 20 mL/min;
step 6: after the injection is finished, continuously calcining for 3h at 660 ℃, and cooling to obtain the zinc gadolinium oxide powder.
The prepared zinc gadolinium oxide powder has the following technical characteristics: the zinc gadolinium oxide powder consists of zinc and gadolinium composite oxides, wherein the mass percent of zinc oxide is 70%; the particle size range of the zinc gadolinium oxide powder is 3-10 mu m, and the specific surface area is 230m2G, total pore volume 0.20cm3(ii)/g; the zinc gadolinium oxide powder can be excited by light with the wavelength less than 530nm to generate photocatalytic activity.
Example 2
A method for preparing zinc gadolinium oxide powder by vapor deposition comprises the following preparation steps:
firstly, preparing a zinc-gadolinium precursor
Step 1: adding 390mL of ethanol, 15g of zinc acetate, 8g of emulsifier span 80 and 4mL of acetylacetone into a 500mL flask in sequence, heating the solution to 65 ℃, and preserving heat for 60min at the temperature to obtain a solution A;
step 2: sequentially adding 150mL of deionized water, 120mL of ethanol, 10g of gadolinium nitrate and 7mL of 1mol/L hydrochloric acid solution into a beaker, and uniformly stirring to obtain a solution B;
and step 3: and uniformly mixing the solution A and the solution B, heating the mixed solution to 65 ℃, and preserving heat for 60min at the temperature to obtain the zinc-gadolinium precursor.
Second, vapor deposition
And 4, step 4: introducing a quartz tube from the outside of the box-type electric furnace to the center of the furnace chamber, wherein the inner diameter of the quartz tube is 7mm, the inner diameter of the quartz tube at the tail end outlet of the center of the furnace chamber is 0.6mm, and the temperature of the electric furnace is kept at 680 ℃;
and 5: injecting the zinc-gadolinium precursor prepared in the step (3) into an electric furnace from a quartz tube, wherein the injection flow is 20 mL/min;
step 6: after the injection is finished, continuously calcining for 3h at 680 ℃, and cooling to obtain the zinc gadolinium oxide powder.
The prepared zinc gadolinium oxide powder has the following technical characteristics: the zinc gadolinium oxide powder consists of a composite oxide of zinc and gadolinium, wherein the mass percent of zinc oxide is 80%; the particle size range of the zinc gadolinium oxide powder is 3-10 mu m, and the specific surface area is 190m2G, total pore volume 0.16cm3(ii)/g; the zinc gadolinium oxide powder can be excited by light with the wavelength less than 530nm to generate photocatalytic activity.
Example 3
A method for preparing zinc gadolinium oxide powder by vapor deposition comprises the following preparation steps:
firstly, preparing a zinc-gadolinium precursor
Step 1: adding 390mL of ethanol, 17g of zinc acetate, 10g of emulsifier span 80 and 5mL of acetylacetone into a 500mL flask in sequence, heating the solution to 65 ℃, and preserving heat for 60min at the temperature to obtain a solution A;
step 2: sequentially adding 150mL of deionized water, 120mL of ethanol, 12g of gadolinium nitrate and 8mL of 1mol/L hydrochloric acid solution into a beaker, and uniformly stirring to obtain a solution B;
and step 3: and uniformly mixing the solution A and the solution B, heating the mixed solution to 65 ℃, and preserving heat for 60min at the temperature to obtain the zinc-gadolinium precursor.
Second, vapor deposition
And 4, step 4: introducing a quartz tube from the outside of the box-type electric furnace to the center of the furnace chamber, wherein the inner diameter of the quartz tube is 7mm, the inner diameter of the quartz tube at the tail end outlet of the center of the furnace chamber is 0.6mm, and the temperature of the electric furnace is kept at 710 ℃;
and 5: injecting the zinc-gadolinium precursor prepared in the step (3) into an electric furnace from a quartz tube, wherein the injection flow is 20 mL/min;
step 6: after the injection is finished, continuously calcining for 3h at 710 ℃, and cooling to obtain the zinc gadolinium oxide powder.
The prepared zinc gadolinium oxide powder has the following technical characteristics: the zinc gadolinium oxide powder consists of zinc and gadolinium composite oxides, wherein the mass percent of zinc oxide is 70%; the particle size range of the zinc gadolinium oxide powder is 3-10 mu m, and the specific surface area is 160m2G, total pore volume 0.12cm3(ii)/g; the zinc gadolinium oxide powder can be excited by light with the wavelength less than 530nm to generate photocatalytic activity.
Claims (1)
1. The method for preparing the composite zinc gadolinium oxide powder by vapor deposition is characterized by comprising the following preparation steps:
firstly, preparing a zinc-gadolinium precursor
Step 1: adding 390mL of ethanol, 12-17 g of zinc acetate, 7-10 g of emulsifier span 80 and 3-5 mL of acetylacetone into a 500mL flask in sequence, heating the solution to 65 ℃, and preserving the temperature for 60min at the temperature to obtain a solution A, wherein the used chemical raw materials are pure materials;
step 2: sequentially adding 150mL of deionized water, 120mL of ethanol, 9-12 g of gadolinium nitrate and 6-8 mL of 1mol/L hydrochloric acid solution into a beaker, and uniformly stirring to obtain a solution B, wherein the used chemical raw materials are pure materials;
and step 3: uniformly mixing the solution A and the solution B, heating the mixed solution to 65 ℃, and preserving heat for 60min at the temperature to prepare a zinc-gadolinium precursor;
second, vapor deposition
And 4, step 4: introducing a quartz tube from the outside of the box-type electric furnace to the center of the furnace chamber, wherein the inner diameter of the quartz tube is 7mm, the inner diameter of the quartz tube at the tail end outlet of the center of the furnace chamber is 0.6mm, and the temperature of the electric furnace is kept at 660-710 ℃;
and 5: injecting the zinc-gadolinium precursor prepared in the step (3) into an electric furnace from a quartz tube, wherein the injection flow is 20 mL/min;
step 6: after the injection is finished, continuously calcining for 3 hours at the temperature of 660-710 ℃, and cooling to obtain composite zinc gadolinium oxide powder;
the prepared composite zinc gadolinium oxide powder has the following technical characteristics: the particle size range of the composite zinc gadolinium oxide powder is 3-10 mu m, and the specific surface area is 160-230 m2(ii) a total pore volume of 0.12 to 0.20cm3(ii)/g; the composite zinc gadolinium oxide powder can be excited by light with the wavelength less than 530nm to generate photocatalytic activity.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1772375A (en) * | 2005-10-27 | 2006-05-17 | 南京大学 | Nanometer doped zinc oxide and its prepn and application in photocatalysis to degrade organic matter and kill bacteria |
| CN108380199A (en) * | 2018-03-16 | 2018-08-10 | 沈阳理工大学 | A method of preparing europium-titanium composite nano oxide powder |
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| EP2499677B1 (en) * | 2009-11-10 | 2022-03-30 | Immunolight, LLC | Up coversion system for production of light for treatment of a cell proliferation related disorder |
| FR2981790A1 (en) * | 2011-10-19 | 2013-04-26 | Solarwell | METHOD FOR GROWTH IN THICKNESS OF COLLOIDAL SHEETS AND MATERIALS COMPOSED OF SHEETS |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1772375A (en) * | 2005-10-27 | 2006-05-17 | 南京大学 | Nanometer doped zinc oxide and its prepn and application in photocatalysis to degrade organic matter and kill bacteria |
| CN108380199A (en) * | 2018-03-16 | 2018-08-10 | 沈阳理工大学 | A method of preparing europium-titanium composite nano oxide powder |
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