CN105289569A - Preparation method of Al-Ce-ZrO2 catalysis material - Google Patents
Preparation method of Al-Ce-ZrO2 catalysis material Download PDFInfo
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- CN105289569A CN105289569A CN201510651804.2A CN201510651804A CN105289569A CN 105289569 A CN105289569 A CN 105289569A CN 201510651804 A CN201510651804 A CN 201510651804A CN 105289569 A CN105289569 A CN 105289569A
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Abstract
The invention provides a preparation method of an Al-Ce-ZrO2 catalysis material, and relates to the technical field of a novel nanometer catalysis material. The method comprises the following steps of weighing ZrOCl2 8H2O, C<19>H<42>BrN, Al2O3 3H2O and Ce(SO4)2 4H2O into a beaker; pouring dilute ammonia water into the breaker; dripping a plurality of drips of absolute ethyl alcohol; dripping the dilute ammonia water during stirring until the pH value of the solution is about 8; covering the breaker by a preservative film; stirring the materials for two hours; pouring the solution into a reaction kettle; putting the reaction kettle in a baking oven for taking a hydrothermal reaction; washing a reaction product by absolute ethyl alcohol; then, performing suction filtration and repeated washing; putting the product into a crucible; putting the crucible into the baking oven again to be dried; finely grinding the product which is taken out from the baking oven by a grinding pot to obtain the Al-Ce-ZrO2 catalysis material. The Al-Ce-ZrO2 catalysis material has the advantages of high photocatalysis activity, high thermal stability, high powder dispersion performance and the like, and can be perfectly applied to the field of catalysis materials.
Description
Technical field
The present invention relates to novel nano catalysis material technical field, specifically relate to a kind of Al-Ce-ZrO
2the preparation method of catalysis material.
Background technology
Material is the material base that the mankind depend on for existence and development, plays a very important role in national economy and social development.Along with electronics and new material industry are just at development, nanometer ZrO
2and its composite will be widely used, be particularly applied to catalysis material technical field, research boom definitely will certainly be caused.
Zirconium dioxide (ZrO
2) be an important function and structural material in modern industry and Material Field, it has very excellent physics and chemistry character, and hardness is inferior to diamond.Pure ZrO
2be a kind of crystal of colorless and odorless, be insoluble in water, hydrochloric acid and dilute sulfuric acid, its chemical property torpescence, fusing point is high, hardness is large, resistivity and refractive index also all higher, and there is low thermal coefficient of expansion.But because its forbidden band is very wide, photocatalytic activity and heat endurance is lower, powder dispersibility is poor, therefore, it well cannot adapt to the requirement of catalysis material.
Chinese patent CN104475095A zirconium dioxide photochemical catalyst disclosing a kind of Ag doping and preparation method thereof, by to doping metals silver element in zirconium dioxide, to change the energy gap of zirconium dioxide, make it there is response at visible region, to improve the activity of zirconium dioxide.First preparation method calcines zirconium dioxide, then instills the aqueous solution of silver ion, is then prepared by hydro-thermal reaction.But this preparation method compares when Separation of Solid and Liquid and washing and is difficult to process, easily causes secondary pollution.The product obtained easily is reunited, and is not easy to be separated, and product powder dispersibility is poor, therefore needs when being applied to industrial production to add dispersant or surfactant.The reactor that this preparation method uses simultaneously is also very easy to be corroded.
Summary of the invention
In order to overcome the above-mentioned defect existed in prior art, an object of the present invention there are provided a kind of Al-Ce-ZrO
2the preparation method of catalysis material, the catalysis material that photocatalytic activity is high to prepare, Heat stability is good, powder dispersibility are high.
For realizing this object, present invention employs following technical scheme: a kind of Al-Ce-ZrO
2the preparation method of catalysis material, step is as follows:
1. the ZrOCl of 9.6675g, is taken
28H
2the C of O, 1.0000g
19h
42the Al of BrN, 0.4119g
2o
33H
2ce (the SO of O and 1.0674g
4)
24H
2o puts into beaker;
2., measure 2.5mL concentrated ammonia liquor, adding distil water is diluted to 100mL, and the ammoniacal liquor after taking-up 50mL is diluted is poured in beaker, and drips several absolute ethyl alcohols, drips weak aqua ammonia while stirring with glass bar, until the pH value of solution stops dripping 7.5 ~ 8.5 time;
3., by magneton put into beaker, encase beaker with preservative film, prevent solution from exposing for a long time oxidized in atmosphere, by magnetic stirrer two hours;
4., by the solution after stirred pour in reactor, then be placed in baking oven by reactor, temperature is set to 80 DEG C, carries out hydro-thermal reaction, takes out after 24 hours;
5., after the cooling of the temperature of question response still, take out product, with after absolute ethanol washing with the multiplex vavuum pump suction filtration of circulating water type, cyclic washing suction filtration 3 times;
6., be placed in crucible by the product that suction filtration is good, again put into baking oven, temperature is still set to 80 DEG C, takes out after 24 hours;
7., the product mortar porphyrize that takes out, obtain end product---Al-Ce-ZrO
2catalysis material.
Compared with prior art, beneficial effect of the present invention shows:
Can be found out by SEM figure be doped with Fe and Al and Ce, Fe and Al, the carrier surface of Fe and Ce and Al and Ce is made up of numerous fine particles, there is abundanter surface texture, prove thus, the element of doping is more, grain surface is long-pending larger, and doped metallic elements effectively avoids the reunion of particle.Al-Ce-ZrO simultaneously
2catalysis material also has that photocatalytic activity is high, Heat stability is good, powder dispersibility advantages of higher, perfection can be applied to catalysis material field.
Accompanying drawing explanation
Fig. 1 is the thermogravimetric analysis figure of target product prepared by embodiment 1 ~ 4.
Fig. 2 is the infrared spectrogram of target product prepared by embodiment 1 ~ 4.
Fig. 3 is the ultraviolet spectrogram of target product prepared by embodiment 1 ~ 4.
Fig. 4 is the electron scanning micrograph of target product prepared by embodiment 1 ~ 4.
Fig. 5 is the X-ray diffracting spectrum of target product prepared by embodiment 1 ~ 4.
Fig. 6 is the photocatalytic degradation Experimental comparison figure of target product prepared by embodiment 1 ~ 4.
Detailed description of the invention
Below in conjunction with embodiment, the present invention is described in further detail.
Embodiment 1
Fe-Al-Ce-ZrO
2the preparation of catalysis material:
1. the ZrOCl of 9.6675g, is taken
28H
2the C of O, 1.0000g
19h
42the FeCl of BrN, 0.4757g
36H
2the Al of O, 0.2746g
2o
33H
2ce (the SO of O and 0.7116g
4)
24H
2o puts into beaker.
2., measure 2.5mL concentrated ammonia liquor, adding distil water is diluted to 100mL, and the ammoniacal liquor after taking-up 50mL is diluted is poured in beaker, and drips several absolute ethyl alcohols, drips weak aqua ammonia while stirring with glass bar, until the pH value of solution stops dripping about 8 time.
3., by magneton put into beaker, encase beaker with preservative film, prevent solution from exposing for a long time oxidized in atmosphere, by magnetic stirrer two hours.
4., by the solution after stirred pour in reactor, then be placed in baking oven by reactor, temperature is set to 80 DEG C, carries out hydro-thermal reaction, takes out after 24 hours.
5., after the cooling of the temperature of question response still, take out product, with after absolute ethanol washing with the multiplex vavuum pump suction filtration of circulating water type, cyclic washing suction filtration 3 times.
6., be placed in crucible by the product that suction filtration is good, again put into baking oven, temperature is still set to 80 DEG C, takes out after 24 hours.
7., the product mortar porphyrize that takes out, obtain end product---Fe-Al-Ce-ZrO
2catalysis material.
Embodiment 2
Fe-Al-ZrO
2the preparation of catalysis material:
1. the ZrOCl of 9.6675g, is taken
28H
2the C of O, 1.0000g
19h
42the FeCl of BrN, 0.7136g
36H
2the Al of O and 0.4119g
2o
33H
2o puts into beaker.
2., measure 2.5mL concentrated ammonia liquor, adding distil water is diluted to 100mL, and the ammoniacal liquor after taking-up 50mL is diluted is poured in beaker, and drips several absolute ethyl alcohols, drips weak aqua ammonia while stirring with glass bar, until the pH value of solution stops dripping about 8 time.
3., by magneton put into beaker, encase beaker with preservative film, prevent solution from exposing for a long time oxidized in atmosphere, by magnetic stirrer two hours.
4., by the solution after stirred pour in reactor, then be placed in baking oven by reactor, temperature is set to 80 DEG C, carries out hydro-thermal reaction, takes out after 24 hours.
5., after the cooling of the temperature of question response still, take out product, with after absolute ethanol washing with the multiplex vavuum pump suction filtration of circulating water type, cyclic washing suction filtration 3 times.
6., be placed in crucible by the product that suction filtration is good, again put into baking oven, temperature is still set to 80 DEG C, takes out after 24 hours.
7., the product mortar porphyrize that takes out, obtain end product---Fe-Al-ZrO
2catalysis material.
Embodiment 3
Fe-Ce-ZrO
2the preparation of catalysis material:
1. the ZrOCl of 9.6675g, is taken
28H
2the C of O, 1.0000g
19h
42the FeCl of BrN, 0.7136g
36H
2ce (the SO of O and 1.0674g
4)
24H
2o puts into beaker.
2., measure 2.5mL concentrated ammonia liquor, adding distil water is diluted to 100mL, and the ammoniacal liquor after taking-up 50mL is diluted is poured in beaker, and drips several absolute ethyl alcohols, drips weak aqua ammonia while stirring with glass bar, until the pH value of solution stops dripping about 8 time.
3., by magneton put into beaker, encase beaker with preservative film, prevent solution from exposing for a long time oxidized in atmosphere, by magnetic stirrer two hours.
4., by the solution after stirred pour in reactor, then be placed in baking oven by reactor, temperature is set to 80 DEG C, carries out hydro-thermal reaction, takes out after 24 hours.
5., after the cooling of the temperature of question response still, take out product, with after absolute ethanol washing with the multiplex vavuum pump suction filtration of circulating water type, cyclic washing suction filtration 3 times.
6., be placed in crucible by the product that suction filtration is good, again put into baking oven, temperature is still set to 80 DEG C, takes out after 24 hours.
7., the product mortar porphyrize that takes out, obtain end product---Fe-Ce-ZrO
2catalysis material.
Embodiment 4
Al-Ce-ZrO
2the preparation of catalysis material:
1. the ZrOCl of 9.6675g, is taken
28H
2the C of O, 1.0000g
19h
42the Al of BrN, 0.4119g
2o
33H
2ce (the SO of O and 1.0674g
4)
24H
2o puts into beaker.
2., measure 2.5mL concentrated ammonia liquor, adding distil water is diluted to 100mL, and the ammoniacal liquor after taking-up 50mL is diluted is poured in beaker, and drips several absolute ethyl alcohols, drips weak aqua ammonia while stirring with glass bar, until the pH value of solution stops dripping about 8 time.
3., by magneton put into beaker, encase beaker with preservative film, prevent solution from exposing for a long time oxidized in atmosphere, by magnetic stirrer two hours.
4., by the solution after stirred pour in reactor, then be placed in baking oven by reactor, temperature is set to 80 DEG C, carries out hydro-thermal reaction, takes out after 24 hours.
5., after the cooling of the temperature of question response still, take out product, with after absolute ethanol washing with the multiplex vavuum pump suction filtration of circulating water type, cyclic washing suction filtration 3 times.
6., be placed in crucible by the product that suction filtration is good, again put into baking oven, temperature is still set to 80 DEG C, takes out after 24 hours.
7., the product mortar porphyrize that takes out, obtain end product---Al-Ce-ZrO
2catalysis material.
Thermogravimetric differential thermal measuring instrument (TG/DSC), fourier transform infrared spectroscopy (FT-IR), ultraviolet-visible spectrophotometer (UV-Vis), field emission scanning electron microscope (FE-SEM) and X-ray powder diffraction (XRD) is selected to characterize parameters such as its structure, pattern and compositions respectively to target product prepared by embodiment 1 ~ 4 below.
Fig. 1 a ~ Fig. 1 d is the thermogravimetric analysis figure of target product prepared by embodiment 1 ~ 4 successively, can find out that a stronger exothermic peak appears 269.87 DEG C time in temperature by Fig. 1 a, may be organic decomposition and oxidation and Tetragonal ZrO in material
2the formation of crystalline solid, and weightlessness is larger in the process.Find out from Fig. 1 b, there is a weak peak in temperature in 54.18 DEG C, may be the volatilization of organic solvent, and temperature there will be the strongest exothermic peak 264.82 DEG C time, obviously weightless in this process.Find out from Fig. 1 c, all occur similar strong and weak exothermic peak when 65.53 DEG C and 163.92 DEG C.Find out from Fig. 1 d, there is a weak peak in temperature in 56.70 DEG C, and temperature there will be the strongest exothermic peak 266.71 DEG C time, obviously weightless in this process.
In Fig. 2, a ~ d curve is the infrared spectrogram of target product prepared by embodiment 1 ~ 4 successively, go out to have a little absworption peak 1630 as seen in Figure 2, this can be attributed to the O-H vibration of water and hydroxyl, and there is individual absworption peak at 2300 places, being C=O vibration, may be the CO in air
2cause, there is an absworption peak at 1415 places, may be C-H singly-bounds.
In Fig. 3, a ~ d curve is the ultraviolet spectrogram of target product prepared by embodiment 1 ~ 4 successively, within the scope of 375nm, absorption region is wider as seen in Figure 3, this phenomenon mainly by zirconia nanocrystals valence-band electrons to conduction band transitions absorption caused by.In figure, a and c curve overlaps substantially, illustrates that the absorption of Al on zirconium dioxide does not affect substantially.
Fig. 4 a ~ Fig. 4 d is the electron scanning micrograph of target product prepared by embodiment 1 ~ 4 successively, be doped with Fe and Al and Ce, Fe and Al as seen in Figure 4 respectively, the carrier surface of Fe and Ce and Al and Ce is made up of numerous fine particles, there is abundanter surface texture, prove thus, the element of doping is more, grain surface is long-pending larger, and doped metallic elements effectively avoids the reunion of particle.
In Fig. 5, a ~ d curve is the X-ray diffracting spectrum of target product prepared by embodiment 1 ~ 4 successively, each component has a stronger peak at about 33 ° as seen in Figure 3, this peak is generally the characteristic peak of Tetragonal zirconium, not seeing the characteristic peak of Fe, Al and Ce, is because these elements are well dispersed in zirconium dioxide.
Fig. 6 a ~ Fig. 6 d is followed successively by the photocatalytic degradation Experimental comparison figure of target product prepared by embodiment 1 ~ 4.First the sample taking 0.02g, in test tube, adds the distilled water of methyl orange solution that 10mL prepares and 40mL, first adsorption/desorption 30min, carry out light-catalyzed reaction again, get a sample when starting to react, then get a sample every 20min, each component gets 3 samples.As seen in Figure 6, target product prepared by embodiment 1 ~ 4 all has photocatalysis effect, all effectively can improve photocatalysis performance.
Claims (1)
1. an Al-Ce-ZrO
2the preparation method of catalysis material, is characterized in that step is as follows:
1. the ZrOCl of 9.6675g, is taken
28H
2the C of O, 1.0000g
19h
42the Al of BrN, 0.4119g
2o
33H
2ce (the SO of O and 1.0674g
4)
24H
2o puts into beaker;
2., measure 2.5mL concentrated ammonia liquor, adding distil water is diluted to 100mL, and the ammoniacal liquor after taking-up 50mL is diluted is poured in beaker, and drips several absolute ethyl alcohols, drips weak aqua ammonia while stirring with glass bar, until the pH value of solution stops dripping 7.5 ~ 8.5 time;
3., by magneton put into beaker, encase beaker with preservative film, prevent solution from exposing for a long time oxidized in atmosphere, by magnetic stirrer two hours;
4., by the solution after stirred pour in reactor, then be placed in baking oven by reactor, temperature is set to 80 DEG C, carries out hydro-thermal reaction, takes out after 24 hours;
5., after the cooling of the temperature of question response still, take out product, with after absolute ethanol washing with the multiplex vavuum pump suction filtration of circulating water type, cyclic washing suction filtration 3 times;
6., be placed in crucible by the product that suction filtration is good, again put into baking oven, temperature is still set to 80 DEG C, takes out after 24 hours;
7., the product mortar porphyrize that takes out, obtain end product---Al-Ce-ZrO
2catalysis material.
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Cited By (1)
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---|---|---|---|---|
CN113304743A (en) * | 2021-05-14 | 2021-08-27 | 安徽海华科技集团有限公司 | Method for preparing high-purity carvacrol by using o-cresol |
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CN102407164A (en) * | 2011-10-09 | 2012-04-11 | 南京大学 | Cerium zirconium aluminum nanometer composite with mesoporous structure and preparation method and use thereof |
-
2015
- 2015-10-09 CN CN201510651804.2A patent/CN105289569A/en active Pending
Patent Citations (2)
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US20110058999A1 (en) * | 2009-09-10 | 2011-03-10 | Cummins Ip, Inc | Low temperature selective catalytic reduction catalyst and associated systems and methods |
CN102407164A (en) * | 2011-10-09 | 2012-04-11 | 南京大学 | Cerium zirconium aluminum nanometer composite with mesoporous structure and preparation method and use thereof |
Non-Patent Citations (2)
Title |
---|
QIANG YU等: "Mesoporous ceria-zirconia-alumina nanocomposite-supported copper as a superior catalyst for simultaneous catalytic elimination of NO-CO", 《CATALYSIS COMMUNICATIONS》 * |
吴其胜: "醇水加热-水热法制备稳定Y-Ce-ZrO2纳米粉体", 《硅酸盐学报》 * |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN113304743A (en) * | 2021-05-14 | 2021-08-27 | 安徽海华科技集团有限公司 | Method for preparing high-purity carvacrol by using o-cresol |
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