CN111495371A - Rapid preparation method of cobalt spinel catalyst - Google Patents
Rapid preparation method of cobalt spinel catalyst Download PDFInfo
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- 239000003054 catalyst Substances 0.000 title claims abstract description 65
- 229910052596 spinel Inorganic materials 0.000 title claims abstract description 22
- 239000011029 spinel Substances 0.000 title claims abstract description 22
- 229910017052 cobalt Inorganic materials 0.000 title claims abstract description 18
- 239000010941 cobalt Substances 0.000 title claims abstract description 18
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 title claims abstract description 18
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 37
- 239000008367 deionised water Substances 0.000 claims abstract description 30
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 30
- 230000032683 aging Effects 0.000 claims abstract description 12
- UFMZWBIQTDUYBN-UHFFFAOYSA-N cobalt dinitrate Chemical compound [Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O UFMZWBIQTDUYBN-UHFFFAOYSA-N 0.000 claims abstract description 10
- 229910001981 cobalt nitrate Inorganic materials 0.000 claims abstract description 10
- 150000001879 copper Chemical class 0.000 claims abstract description 10
- 238000002156 mixing Methods 0.000 claims abstract description 9
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229910000013 Ammonium bicarbonate Inorganic materials 0.000 claims abstract description 8
- 235000012538 ammonium bicarbonate Nutrition 0.000 claims abstract description 8
- 239000001099 ammonium carbonate Substances 0.000 claims abstract description 8
- 238000001035 drying Methods 0.000 claims abstract description 6
- 238000000034 method Methods 0.000 claims abstract description 6
- 238000003756 stirring Methods 0.000 claims abstract description 6
- 238000005406 washing Methods 0.000 claims abstract description 6
- 238000001354 calcination Methods 0.000 claims abstract description 3
- 239000000203 mixture Substances 0.000 claims abstract description 3
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 abstract description 39
- 230000003197 catalytic effect Effects 0.000 abstract description 19
- 238000006243 chemical reaction Methods 0.000 abstract description 4
- 238000000975 co-precipitation Methods 0.000 abstract description 2
- 239000000523 sample Substances 0.000 description 16
- 238000005516 engineering process Methods 0.000 description 15
- 239000012855 volatile organic compound Substances 0.000 description 13
- 230000000052 comparative effect Effects 0.000 description 12
- 229910003119 ZnCo2O4 Inorganic materials 0.000 description 6
- 238000005303 weighing Methods 0.000 description 6
- 229910016506 CuCo2O4 Inorganic materials 0.000 description 5
- UBEWDCMIDFGDOO-UHFFFAOYSA-N cobalt(II,III) oxide Inorganic materials [O-2].[O-2].[O-2].[O-2].[Co+2].[Co+3].[Co+3] UBEWDCMIDFGDOO-UHFFFAOYSA-N 0.000 description 5
- 230000006872 improvement Effects 0.000 description 5
- 229910005949 NiCo2O4 Inorganic materials 0.000 description 4
- 238000002441 X-ray diffraction Methods 0.000 description 4
- 238000007084 catalytic combustion reaction Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 239000010949 copper Substances 0.000 description 3
- XTVVROIMIGLXTD-UHFFFAOYSA-N copper(II) nitrate Chemical compound [Cu+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XTVVROIMIGLXTD-UHFFFAOYSA-N 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 229910016507 CuCo Inorganic materials 0.000 description 2
- 229910003266 NiCo Inorganic materials 0.000 description 2
- 238000002485 combustion reaction Methods 0.000 description 2
- 230000006378 damage Effects 0.000 description 2
- 230000036541 health Effects 0.000 description 2
- 229910000510 noble metal Inorganic materials 0.000 description 2
- 239000012716 precipitator Substances 0.000 description 2
- 230000000630 rising effect Effects 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 229910021281 Co3O4In Inorganic materials 0.000 description 1
- 239000006004 Quartz sand Substances 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 150000001299 aldehydes Chemical class 0.000 description 1
- 150000001335 aliphatic alkanes Chemical class 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
- -1 aromatics Chemical class 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 238000002144 chemical decomposition reaction Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 229940116318 copper carbonate Drugs 0.000 description 1
- QKSIFUGZHOUETI-UHFFFAOYSA-N copper;azane Chemical compound N.N.N.N.[Cu+2] QKSIFUGZHOUETI-UHFFFAOYSA-N 0.000 description 1
- GEZOTWYUIKXWOA-UHFFFAOYSA-L copper;carbonate Chemical compound [Cu+2].[O-]C([O-])=O GEZOTWYUIKXWOA-UHFFFAOYSA-L 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 150000002170 ethers Chemical class 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(II) nitrate Inorganic materials [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 description 1
- 230000008520 organization Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 238000005504 petroleum refining Methods 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 230000001699 photocatalysis Effects 0.000 description 1
- 239000010970 precious metal Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000002336 sorption--desorption measurement Methods 0.000 description 1
- 229910052566 spinel group Inorganic materials 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 229920002994 synthetic fiber Polymers 0.000 description 1
- LITQZINTSYBKIU-UHFFFAOYSA-F tetracopper;hexahydroxide;sulfate Chemical compound [OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[Cu+2].[Cu+2].[Cu+2].[Cu+2].[O-]S([O-])(=O)=O LITQZINTSYBKIU-UHFFFAOYSA-F 0.000 description 1
- 229910000314 transition metal oxide Inorganic materials 0.000 description 1
- ONDPHDOFVYQSGI-UHFFFAOYSA-N zinc nitrate Inorganic materials [Zn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ONDPHDOFVYQSGI-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
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/74—Iron group metals
- B01J23/75—Cobalt
-
- 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
- B01J35/60—Catalysts, in general, characterised by their form or physical properties characterised by their surface properties or porosity
- B01J35/61—Surface area
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F23—COMBUSTION APPARATUS; COMBUSTION PROCESSES
- F23G—CREMATION FURNACES; CONSUMING WASTE PRODUCTS BY COMBUSTION
- F23G7/00—Incinerators or other apparatus for consuming industrial waste, e.g. chemicals
- F23G7/06—Incinerators or other apparatus for consuming industrial waste, e.g. chemicals of waste gases or noxious gases, e.g. exhaust gases
- F23G7/07—Incinerators or other apparatus for consuming industrial waste, e.g. chemicals of waste gases or noxious gases, e.g. exhaust gases in which combustion takes place in the presence of catalytic material
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Environmental & Geological Engineering (AREA)
- Mechanical Engineering (AREA)
- General Engineering & Computer Science (AREA)
- Catalysts (AREA)
Abstract
The invention relates to the field of catalyst preparation by adopting a coprecipitation method, in particular to a rapid preparation method of a cobalt spinel catalyst. Mixing cobalt nitrate and copper salt, dissolving the mixture in deionized water to form a solution A, and dissolving ammonium bicarbonate in the deionized water to form a solution B; then mixing and stirring the two solutions, and then aging for 6 hours at 30 ℃; and washing the catalyst with deionized water after aging, drying the catalyst, and calcining the catalyst for 3 hours at 300 ℃ to obtain the cobalt spinel catalyst. Compared with the traditional preparation method of spinel, the preparation method of the catalyst is short in time consumption and greatly saves the preparation time; compared with the prior spinel catalyst, the catalyst prepared by the invention has larger specific surface area which is more than 100m2(ii)/g; meanwhile, the catalyst has high catalytic performance, and the conversion rate of toluene at 230 ℃ of the optimal catalyst can reach 90%.
Description
Technical Field
The invention relates to the field of catalyst preparation by adopting a coprecipitation method, in particular to a rapid preparation method of a cobalt spinel catalyst. The invention takes cobalt nitrate as a metal source and ammonium bicarbonate as a precipitator, prepares a high-performance catalyst by controlling the dosage of the precipitator, can be used for catalytic oxidation of volatile organic compounds, and belongs to the field of purification treatment.
Background
VOCs are short for volatile organic compounds (volatile organic compounds). The definition of VOCs according to the World Health Organization (WHO) is: the total name of the volatile organic compounds with the melting point lower than room temperature and the boiling point between 50 ℃ and 260 ℃. The types of VOCs are various, and the number of VOCs identified at present is more than 300. VOCs can be divided into the following according to their chemical structures: and twenty species such as alkanes, alkenes, aromatics, alcohols, aldehydes, ketones, ethers, esters and the like. And the emission sources of VOCs are extremely wide, and the main emission sources relate to multiple industries of petrochemical industry, petroleum refining, transportation, synthetic materials and furniture manufacturing. The large discharge of VOCs poses a great threat to the environment and human health.
At present, two technologies for treating VOCs are mainly used, one is a physical recovery technology, and the other technology mainly comprises an adsorption technology, an absorption technology, a condensation technology and a membrane separation technology. The other is that the chemical degradation technology mainly comprises photocatalysis technology, plasma technology, thermal combustion technology, catalytic combustion technology and the like. Compared with other technologies, the catalytic combustion technology has the advantages of low operation temperature, no secondary pollution, strong processing capacity and wide application range.
The development of catalysts with high activity for catalytic combustion technology is the focus of current research. Existing catalysts mainly include noble metal catalysts and transition metal oxide catalysts. However, the precious metals are low in reserves, easy to deactivate and expensive. Therefore, research and development of inexpensive and high-performance non-noble metal catalysts (such as perovskites, spinels, etc.) are in great interest. At present, the problems of low activity, complex preparation process and long time consumption of the catalyst for catalytic combustion of VOCs generally exist.
Disclosure of Invention
The invention provides a rapid preparation method of a cobalt spinel catalyst, aiming at solving the problems of lower activity, complex preparation process and long time consumption of the existing catalyst.
The invention is realized by the following technical scheme, and adopts a rapid preparation method of a cobalt spinel catalyst, which comprises the following specific steps:
mixing cobalt nitrate and copper salt, dissolving the mixture in deionized water to form a solution A, and dissolving ammonium bicarbonate in the deionized water to form a solution B; then mixing and stirring the two solutions, and aging for 6h at 30 ℃; and washing the catalyst with deionized water after aging, drying the catalyst, and calcining the catalyst for 3 hours at 300 ℃ to obtain the cobalt spinel catalyst.
In the invention, the copper salt can be selected from basic copper carbonate, basic copper sulfate, copper ammonia complex, copper nitrate and the like.
As a further improvement of the technical scheme of the invention, the ratio of the amount of the copper salt to the cobalt nitrate substance in the solution A is 1: 2.
As a further improvement of the technical scheme of the invention, the amount of the substance of ammonium bicarbonate in the solution B is 2 times of the total amount of the copper salt and the cobalt nitrate.
As a further improvement of the technical scheme of the invention, the total concentration of the cobalt nitrate and the copper salt in the solution A is 0.06 mol/L.
As a further improvement of the technical scheme of the invention, the concentration of ammonium bicarbonate in the solution B is 0.12 mol/L.
Compared with the existing catalyst, the catalyst prepared by the invention has the outstanding characteristics and advantages that:
1) compared with the traditional preparation method of spinel, the preparation method has short time consumption and greatly saves the preparation time;
2) compared with the existing spinel catalyst, the catalyst prepared by the invention has larger specific surface area which is more than 100m2(ii)/g; meanwhile, the catalyst has high catalytic performance, and the conversion rate of toluene at 230 ℃ of the optimal catalyst can reach 90%.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly introduced below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to these drawings without creative efforts.
Fig. 1 is an XRD diffraction pattern of each cobalt-based spinel catalyst. From the XRD diffraction pattern of figure 1, it can be seen that the catalyst has obvious diffraction peaks when the 2 theta is 18.9 degrees, 31.2 degrees, 36.8 degrees, 44.8 degrees, 59.3 degrees and 65.2 degrees, which indicates that the catalyst has obvious spinel crystal form.
Fig. 2 is an SEM image of each cobalt-based spinel catalyst. From FIG. 2, Co can be seen3O4，CuCo2O4And NiCo2O4The shapes are all spherical, and ZnCo2O4The morphology of (a) may be due to the destruction of the Zn addition, resulting in an irregular shape.
Fig. 3 is a graph showing the toluene combustion catalytic performance of each cobalt-based spinel catalyst. As can be seen from FIG. 3, CuCo obtained by introducing cobalt atoms2O4，NiCo2O4And ZnCo2O4Compared with CuO, NiO and ZnO, the performance of the catalyst is greatly improved. Probably due to CuCo2O4，NiCo2O4And ZnCo2O4The spherical small spines of the three catalysts have more active sites, and can adsorb more active oxygen species. However, the three composite catalysts compare to Co3O4In other words, CuCo2O4Exhibit higher catalytic activity, while NiCo2O4And Co3O4Equivalent activity, ZnCo2O4Exhibit a specific Co ratio3O4Significantly reduced catalytic performance. The reason for this is probably that the synergistic effect between Cu and Co promotes the catalyst performance to be obviously higher than that of CuO and Co3O4And the introduction of Zn makes ZnCo2O4The appearance is changed to cause structural damage, so that the catalytic performance of the catalyst is better than that of Co3O4Low.
FIG. 4 shows N of each cobalt-based spinel catalyst2Adsorption and desorption yeastAnd (6) line drawing. As can be seen from FIG. 4, the adsorption-desorption curves of all the catalysts are IV-type isotherms, which indicates that they have mesoporous structures.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the technical solutions of the present invention will be described in detail below. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. All other embodiments, which can be derived by a person skilled in the art from the examples given herein without any inventive step, are within the scope of the present invention.
Comparative example 1
Weighing 8.7315g Co (NO)3)3·6H2O is dissolved in 500ml of deionized water to form a solution A, NH with a concentration of 0.06 mol/L4HCO3(4.74g) is dissolved in 500ml of deionized water to form a solution B with the concentration of 0.12 mol/L, the two solutions are quickly mixed and stirred for 0.5h, then the solution B is aged for 6h in a 30 ℃ water bath, the aged solution B is washed by the deionized water for a plurality of times, the dried solution B is dried for 12h in a 60 ℃ oven, then the sample is placed in a tube furnace for roasting for 3h at the temperature of 300 ℃, and the temperature rising rate is 5 ℃/min to obtain a sample Co3O4. The XRD pattern is shown in figure 1, and the SEM pattern is shown in figure 2 for Co3O4The catalytic activity of toluene is shown in FIG. 3.
Comparative example 2
Weighing 7.248g Cu (NO)3)2·3H2O is dissolved in 500ml of deionized water to form a solution C, NH with a concentration of 0.06 mol/L4HCO3(4.74g) is dissolved in 500ml of deionized water to form a solution D with the concentration of 0.12 mol/L. the two solutions are quickly mixed and stirred for 0.5h, then are aged for 6h in a 30 ℃ water bath, after the aging is finished, the two solutions are washed by the deionized water for a plurality of times, are dried for 12h in an oven at the temperature of 60 ℃, and then are put in a tube furnace to be roasted for 3h at the temperature of 300 ℃ with the temperature rise rate of 5 ℃/min to obtain a sample CuO catalyst, wherein the toluene catalytic activity diagram of the catalyst is shown in figure 3.
Comparative example 3
8.7243g of Ni (NO) were weighed out3)2·6H2O is dissolved in 500ml of deionized water to form a solution C, NH with a concentration of 0.06 mol/L4HCO3(4.74g) in 500ml deionized water to form a solution D with the concentration of 0.12 mol/L. the two solutions are rapidly mixed and stirred for 0.5h, then are aged for 6h in a 30 ℃ water bath, after the aging is completed, the two solutions are washed by deionized water for a plurality of times, are dried for 12h in an oven at the temperature of 60 ℃, and then the sample is placed in a tube furnace to be roasted for 3h at the temperature of 300 ℃ and the temperature rise rate is 5 ℃/min to obtain a sample NiO catalyst, wherein the toluene catalytic activity of the catalyst is shown in figure 3.
Comparative example 4
Weighing 8.9247g Zn (NO)3)2·6H2O is dissolved in 500ml of deionized water to form a solution C, NH with a concentration of 0.06 mol/L4HCO3(4.74g) is dissolved in 500ml of deionized water to form a solution D with the concentration of 0.12 mol/L. the two solutions are quickly mixed and stirred for 0.5h, then are aged for 6h in a 30 ℃ water bath, after the aging is finished, the two solutions are washed by the deionized water for a plurality of times, are dried for 12h in an oven at the temperature of 60 ℃, and then the sample is placed in a tube furnace to be roasted for 3h at the temperature of 300 ℃ with the temperature rising rate of 5 ℃/min to obtain a sample ZnO catalyst, and the toluene catalytic activity graph of the catalyst is shown in figure 3.
Comparative example 5:
weighing 5.821g Co (NO)3)3·6H2O、2.9081g Ni(NO3)2·6H2Dissolving weighed sample in 500ml deionized water to form solution A with the concentration of 0.06 mol/L and 4.74g NH4HCO3Dissolving the two solutions in 500ml of deionized water to form a solution B with the concentration of 0.12 mol/L, quickly mixing and stirring the two solutions for 0.5h, then aging the solution in a water bath kettle at 30 ℃ for 6h, washing the aged solution for a plurality of times by using the deionized water after the aging is finished, drying the dried solution in an oven at 60 ℃ for 12h, putting the sample in a tubular furnace for roasting at 300 ℃ for 3h, and obtaining NiCo with the heating rate of 5 ℃/min2O4. The XRD pattern is shown in FIG. 1, and the SEM pattern is NiCo in FIG. 22O4The catalytic activity of toluene is shown in FIG. 3.
Comparative example 6
Weighing 5.821g Co (NO)3)3·6H2O、2.9749g Zn(NO3)2·6H2Dissolving weighed sample in 500ml deionized water to form solution A with the concentration of 0.06 mol/L and 4.74g NH4HCO3Dissolving the two solutions in 500ml of deionized water to form a solution B with the concentration of 0.12 mol/L, quickly mixing and stirring the two solutions for 0.5h, then aging the solution B in a water bath kettle at 30 ℃ for 6h, washing the aged solution B for a plurality of times by using the deionized water, drying the aged solution B in an oven at 60 ℃ for 12h, then putting the sample in a tubular furnace for roasting at 300 ℃ for 3h, wherein the heating rate is 5 ℃/min to obtain a sample ZnCo2O4. The XRD pattern is shown in figure 1, and the SEM pattern is ZnCo in figure 22O4The catalytic activity of toluene is shown in FIG. 3.
Example 1:
weighing 5.821g Co (NO)3)3·6H2O、2.416g Cu(NO3)2·3H2O was dissolved in 500ml of deionized water to give solution A having a concentration of 0.06 mol/L, 4.74g NH4HCO3Dissolving the two solutions in 500ml of deionized water to form a solution B with the concentration of 0.12 mol/L, quickly mixing and stirring the two solutions for 0.5h, then aging the solution B in a water bath kettle at 30 ℃ for 6h, washing the aged solution B for a plurality of times by using the deionized water, drying the aged solution B in an oven at 60 ℃ for 12h, putting the sample in a tubular furnace for roasting at 300 ℃ for 3h, and heating the sample at the rate of 5 ℃/min to obtain a sample CuCo2O4. The XRD pattern is shown in figure 1, and the SEM pattern is CuCo in figure 22O4The catalytic activity of toluene is shown in FIG. 3.
Quantitative catalysts obtained in various proportions and examples are weighed and mixed with quartz sand (40-70 meshes), and toluene is used as a probe molecule to perform catalyst performance tests. Controlling the concentration of toluene to be 1000ppm and the reaction space velocity to be 10000h-1The temperature at which the conversion of toluene is 90% (by T) is determined experimentally90Representative) is shown in the following table:
| examples | T90/℃ |
| Example 1 | 229 |
| Comparative example 1 | 249 |
| Comparative example 2 | 260 |
| Comparative example 3 | 300 |
| Comparative example 4 | - |
| Comparative example 5 | 249 |
| Comparative example 6 | 279 |
From the comparison of the above results, it can be found that CuCo2O4The catalyst shows the most excellent catalytic performance, the addition of Cu atoms greatly improves the catalytic performance of the catalyst, the addition of Ni elements has no obvious improvement on the catalytic performance, and the addition of Zn elements inhibits the catalytic performance of the catalyst. In addition, it was found that, in combination with the catalytic performance and the specific surface area of the catalyst, the specific surface area is not the most critical factor affecting the performance of the catalyst.
The above description is only for the specific embodiments of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art can easily conceive of the changes or substitutions within the technical scope of the present invention, and the present invention shall be covered thereby. Therefore, the protection scope of the present invention shall be subject to the protection scope of the appended claims.
Claims (5)
1. A rapid preparation method of a cobalt spinel catalyst is characterized by comprising the following steps:
mixing cobalt nitrate and copper salt, dissolving the mixture in deionized water to form a solution A, and dissolving ammonium bicarbonate in the deionized water to form a solution B; then mixing the two solutions, stirring uniformly, and aging for 6h at 30 ℃; washing with deionized water, drying at 60 ℃, and calcining at 300 ℃ for 3h to obtain the cobalt spinel catalyst.
2. The method for rapidly preparing a cobalt-based spinel catalyst according to claim 1, wherein the amount ratio of the copper salt to the cobalt nitrate in the solution A is 1: 2.
3. The method of claim 1 or 2, wherein the amount of ammonium bicarbonate in the solution B is 2 times of the total amount of copper salt and cobalt nitrate.
4. The method for rapidly preparing a cobalt-based spinel catalyst according to claim 1 or 2, wherein the total concentration of the cobalt nitrate and the copper salt in the solution A is 0.06 mol/L.
5. The method for rapidly preparing a cobalt-based spinel catalyst according to claim 1 or 2, wherein the concentration of ammonium bicarbonate in the solution B is 0.12 mol/L.
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| CN114574807A (en) * | 2022-02-28 | 2022-06-03 | 广东鼎泰高科技术股份有限公司 | Plasma transmission device |
| CN114984959A (en) * | 2022-06-07 | 2022-09-02 | 福州大学 | Catalyst for catalytic combustion of copper-cobalt spinel by using methane and preparation method thereof |
| CN116003125A (en) * | 2022-12-06 | 2023-04-25 | 重庆文理学院 | Preparation method of zirconia ceramic material for automobile exhaust sensor |
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