CN110975870A - Preparation method and application of copper-cobalt composite oxide catalyst - Google Patents
Preparation method and application of copper-cobalt composite oxide catalyst Download PDFInfo
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- 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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- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
- B01D53/86—Catalytic processes
- B01D53/8668—Removing organic compounds not provided for in B01D53/8603 - B01D53/8665
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- 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
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- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
- B01J37/082—Decomposition and pyrolysis
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- 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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- B01D2257/708—Volatile organic compounds V.O.C.'s
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F23—COMBUSTION APPARATUS; COMBUSTION PROCESSES
- F23G—CREMATION FURNACES; CONSUMING WASTE PRODUCTS BY COMBUSTION
- F23G2202/00—Combustion
- F23G2202/60—Combustion in a catalytic combustion chamber
Abstract
The invention discloses a preparation method and application of a copper-cobalt composite oxide catalyst, and belongs to the technical field of composite catalyst preparation. The preparation method comprises the following steps: mixing copper salt, cobalt salt and a complexing agent, and grinding into dry materials; roasting the dry material, wherein the roasting condition is that the temperature is increased to 300-550 ℃ at the temperature increase rate of 10 ℃/min, then roasting at the constant temperature of 300-550 ℃ for 1-2 h, and after the roasting is finished, taking out the roasted dry material after the temperature is reduced to the normal temperature to obtain the finished product; the copper salt, the cobalt salt and the complexing agent are 1:2: 0-5 in molar ratio, and the complexing agent is oxalic acid. The copper-cobalt composite oxide catalyst prepared by the method shows good catalytic combustion activity of low-temperature toluene volatile organic compounds. The method prepares the copper-cobalt composite oxide catalyst by a grinding method, has simple preparation process, mild and easily-controlled conditions, safety, environmental protection and good repeatability, and has great industrial application value.
Description
Technical Field
The invention belongs to the technical field of composite catalyst preparation, and particularly relates to a preparation method and application of a copper-cobalt composite oxide catalyst.
Background
The atmospheric environment is closely related to human survival, and atmospheric pollution seriously threatens human survival. Volatile Organic Compounds (VOCs) are important components of air pollution, the VOCs are various in types and complex in components, and not only seriously harm human health, but also greatly affect the environment, and toluene Volatile Organic Compounds (VOCs) are one of the VOCs and are widely concerned due to the great harmfulness to human health and environment.
Toluene is used as an additive and an important chemical raw material, is widely applied to industries such as petrochemical industry, dye, medicine, pesticide, explosive, spice and the like, and volatile organic compounds such as toluene and the like are easily generated in discharged waste gas in the production process of the industries. In addition, toluene is widely used as a solvent for solvents or diluents of raw materials such as glue, paint, coating and the like for interior decoration, and due to the characteristic of volatility, interior decoration materials also become one of main sources of toluene waste gas. The toluene volatile organic compound has strong irritation to human skin and respiratory mucosa, and strong toxicity to liver and central nervous system. Volatile organic compounds such as toluene have 'three-cause' hazards of causing mutation, teratogenesis and carcinogenesis to human bodies, and the toluene is listed as a strong carcinogen by the international health organization. The quality standard of the atmospheric pollutants of the toluene is established in many countries of the world, and the World Health Organization (WHO) regulates the daily average contact concentration limit of the toluene in the atmosphere to be 8.21 mu g/m3According to the indoor air quality standard of 2002 in China, the concentration of toluene in indoor air is required to be less than or equal to 0.2mg/m3. In addition, toluene is closely related to the formation of atmospheric photochemical smog and aerosol, and forms fine Particulate Matter (PM)2.5) And ozone (O)3) Important precursor of (a).
At present, the technology for removing the toluene volatile organic compounds mainly comprises three major types, namely a physical method, a chemical method and a biological method. The physical method mainly comprises absorption method, adsorption method, membrane separation method, condensation method and other technologies. The chemical method mainly comprises the technologies of a thermal burning method, catalytic combustion, a plasma oxidation method, a photocatalytic degradation method and the like. The biological method mainly comprises a biological filtration method, a biological trickling filtration method and a biological washing method. Compared with other treatment technologies, the catalytic combustion technology has the advantages of low energy consumption, high pollutant removal rate, recoverable energy, no secondary pollution and the like, and is more widely concerned in the VOCs removal technology. Scholars at home and abroad make a lot of relevant researches and reports, and the key of the catalytic combustion technology is the synthesis and design of catalyst materials.
The catalysts currently used in catalyst combustion technology are mainly of two types, noble metal catalysts and transition metal catalysts. Noble metals such as Pt, Pd, Ru and Au catalyst are of great research interest for researchers due to the advantages of high activity and selectivity, long service life and the like. However, the noble metal catalyst has the defects of high price, scarce resources, easy poisoning and the like, and further development and application of the noble metal catalyst in the field of catalytic combustion are limited. Researches show that the transition metal catalyst has low cost, rich resources and good catalytic activity, thereby arousing great interest of researchers, and particularly the multi-component transition metal composite oxide catalyst shows excellent catalytic activity, stability and antitoxic performance and has wide market application prospect.
Transition metal oxides are widely applied to various fields as an important functional material, and in the field of catalysis, multicomponent transition metal composite oxides are used as catalysts, and have better catalytic performance than single-component transition metal oxides. The metal oxide component prepared by the conventional method has the defects of low active component content, compact structure and the like, which greatly influences the performance of the catalytic performance of the catalyst. Therefore, the preparation of a catalyst having high reactivity by an appropriate method is also one of important research subjects in the field of catalytic combustion research. The preparation of the multi-component composite oxide catalyst and the research on the catalytic combustion performance of the toluene volatile organic compound are developed, so that the method has important scientific reference and application values for the preparation and application of the transition metal oxide, and has important significance for the fields of catalytic combustion of the toluene volatile organic compound, atmospheric environment protection and the like.
Disclosure of Invention
In view of the above, the present invention aims to provide a preparation method and an application of a copper-cobalt composite oxide catalyst.
In order to achieve the above purpose, the inventor of the present invention has made a long-term study and a large number of practices to obtain the technical scheme of the present invention as follows:
1. a preparation method of a copper-cobalt composite oxide catalyst comprises the following steps:
s1, mixing copper salt, cobalt salt and a complexing agent, and grinding into a dry material;
s2, roasting the dry material in the S1, wherein the roasting condition is that the temperature is increased to 300-550 ℃ at the temperature increase rate of 10 ℃/min, then roasting at the constant temperature of 300-550 ℃ for 1-2 h, and after the roasting is finished, taking out the roasted material after the temperature is reduced to the normal temperature to obtain the product;
the copper salt, the cobalt salt and the complexing agent are 1:2: 0-5 in molar ratio, and the complexing agent is oxalic acid.
Preferably, the copper salt is copper nitrate, copper sulfate or copper chloride.
Preferably, the cobalt salt is cobalt nitrate, cobalt sulfate or cobalt chloride.
Preferably, the copper salt, the cobalt salt and the complexing agent are in a molar ratio of 1:2: 3.
Preferably, in the S2, the constant-temperature roasting temperature is 450 ℃ and the time is 2 h.
2. The copper-cobalt composite oxide catalyst prepared by the preparation method.
3. The application of the copper-cobalt composite oxide catalyst in degrading volatile organic compounds.
The invention has the beneficial effects that:
1) the copper-cobalt composite oxide catalyst prepared by the method uses non-noble metal Co3O4And CuO composite oxide is used as an active component, so that the cost of the catalyst is greatly reduced;
2) the crystal phase of the copper-cobalt composite oxide catalyst prepared by the method is a spinel phase, and is catalyzed by toluene volatile organic compound reactant moleculesThe chemical combustion reaction provides the active ingredient at a high reaction space velocity (66,000 mL. h)-1·g-1) Low reaction temperature (C)<The catalytic combustion activity of toluene volatile organic compounds is good at 260 ℃, and the catalytic combustion activity of toluene volatile organic compounds at low temperature is good;
3) the copper-cobalt composite oxide catalyst prepared by the method has a mesoporous structure, can provide a larger reaction interface for the adsorption and activation of reactant molecules, also provides superior conditions for the diffusion and migration of the reactant and product molecules in the catalyst, and lays a foundation for the good low-temperature catalytic activity of the catalyst;
4) the copper-cobalt composite oxide catalyst prepared by copper salt, cobalt salt and oxalic acid through a grinding method has the advantages of simple preparation process, mild and easily-controlled conditions, safety, environmental protection and good repeatability, and has great industrial application value.
Drawings
FIG. 1 is an X-ray diffraction (XRD) pattern of a copper-cobalt composite oxide catalyst obtained in example 2;
FIG. 2 shows N in the copper-cobalt composite oxide catalyst obtained in example 22-adsorption desorption isotherm diagram;
FIG. 3 is a scanning electron micrograph of a copper-cobalt composite oxide prepared according to example 2;
FIG. 4 shows H of the copper-cobalt composite oxide catalyst prepared in example 22Temperature programming reduction curve diagram;
fig. 5 is an XRD pattern of the copper cobalt composite oxide catalyst prepared in example 3.
Detailed Description
The present invention is further illustrated by the following specific examples so that those skilled in the art can better understand the present invention and can practice it, but the examples are not intended to limit the present invention.
Example 1
The preparation method of the copper-cobalt composite oxide catalyst of the embodiment comprises the following steps:
s1, adding copper nitrate: cobalt nitrate: mixing oxalic acid with the molar ratio of 1:2:3, and grinding into dry materials;
s2, roasting the dry material in the S1 under the roasting condition that the temperature is increased to 450 ℃ at the heating rate of 10 ℃/min, then roasting at the constant temperature of 450 ℃ for 2 hours, and after the roasting is finished, taking out the roasted dry material after the temperature is reduced to the normal temperature to obtain the catalyst.
Example 2
This example investigates the effect of oxalic acid ratio on catalyst performance. In this example, except that copper nitrate: cobalt nitrate: the molar ratio of oxalic acid was changed to 1:2:0, 1:2:1 and 1:2:5, and the rest was the same as in example 1.
The prepared copper-cobalt composite oxide catalysts were respectively labeled with oxalic acid content as Cu-Co-0, Cu-Co-1 and Cu-Co-5, and the copper-cobalt composite oxide catalyst prepared in example 1 was labeled as Cu-Co-3.
The copper-cobalt composite oxide catalysts of examples 1 and 2 were used for catalytic combustion of toluene, and the activity of the catalysts was evaluated. The activity evaluation of the catalyst is carried out in a mini-tubular fixed bed reactor with an inner diameter of 8mm under normal pressure, a thermocouple is arranged in the reactor, and the reaction temperature is controlled by
And (4) controlling by a-708P type programmed temperature controller, and placing the microreactor in a tubular furnace. The toluene waste gas comprises the following components in percentage by volume: toluene 1.0% and air 99.0%; the specific operation steps are as follows:
50mg of the catalysts obtained in example 1 and example 2 were weighed out, respectively, and charged into a reaction tube of a microtube type fixed bed reactor, and heated to a reaction temperature, and a toluene off-gas of the above composition was introduced at the reaction temperature and 66,000 mL. h-1·g-1Toluene is eliminated at constant temperature under the condition of airspeed of reaction gas (the air flow is controlled by a flowmeter), the content of residual toluene in tail gas is detected on line by GC-7900 II type gas chromatography with a hydrogen flame detector, and the detection conditions are as follows: the temperature of the detector is 120 ℃, the temperature of the sample inlet is 433K, and the temperature of the column box is constantly 433K.
The conversion rate results of the copper-cobalt composite oxide catalyst obtained in the catalyst activity evaluation experiment on the catalytic combustion of toluene volatile organic compounds are shown in table 1:
TABLE 1 influence of oxalic acid content on catalytic toluene Combustion Performance of the catalyst
As can be seen from the analysis in table 1, under the same reaction temperature conditions, copper nitrate: cobalt nitrate: the oxalic acid proportion is 1:2:3, the Cu-Co-3 catalyst has the best conversion effect on the catalytic combustion of the toluene volatile organic compounds. Under the condition of the same oxalic acid content, the conversion rate of the copper-cobalt composite oxide catalyst to toluene volatile organic compound catalytic combustion is increased along with the increase of the temperature. Thus, the addition amount of oxalic acid and the temperature of catalytic combustion both influence the catalytic performance of the copper-cobalt composite oxide catalyst.
The copper-cobalt composite oxide catalysts obtained in example 1 and example 2 were each subjected to X-ray diffraction analysis. X-ray diffraction analysis was performed using a Rigaku D/Max-2500/PC X-ray diffractometer, Japan; cu KαIs a radiation source and is provided with a radiation source,
ni filtering, tube pressure of 40kV, tube flow of 200mA, and scan rate of 5°Min, the scanning interval is 20-80°The scanning step length is 0.02°. The results are shown in FIG. 1.
As can be seen from the analysis in FIG. 1, the Co composite oxide catalysts obtained in examples 1 and 2 are both Co3O4And mainly CuO oxide, and the crystal phase of the catalyst is not changed along with the increase of the proportion of oxalic acid.
The copper-cobalt composite oxide catalysts obtained in examples 1 and 2 were subjected to N2Adsorption-desorption analysis. N is a radical of2The adsorption-desorption isotherm curves were determined by means of a TriStarII model 3020 (Mike, USA) fully automatic analyzer at-196 ℃. The samples were degassed for 6h at 250 ℃ pre-treatment before testing. The specific surface area of the sample was calculated using the Brunauer-Emmett-Teller (BET) equation. The results are shown in FIG. 2.
As can be seen from the analysis in FIG. 2, the method was carried outThe copper-cobalt composite oxide catalysts prepared in examples 1 and 2 both have type IV characteristic adsorption isotherms and H1 hysteresis loops (IUPAC), which indicate that the samples have mesoporous structures, and the existence of the mesoporous structures lays a foundation for high catalytic activity of the catalysts. The specific surface areas of the Cu-Co-0, Cu-Co-1, Cu-Co-3 and Cu-Co-5 catalysts can be calculated by a BET equation and are respectively as follows: 0.86, 5.87, 21.69 and 5.21m2(ii) in terms of/g. According to the BET calculation result, the Cu-Co-3 catalyst has the largest specific surface area, can provide a larger reaction interface for the adsorption and activation of reactant molecules, also provides superior conditions for the diffusion and migration of the reactant and product molecules in the catalyst, and lays a foundation for the good low-temperature catalytic activity of the catalyst.
The copper-cobalt composite oxide catalysts obtained in examples 1 and 2 were analyzed by scanning electron microscopy. The scanning electron microscope analysis was carried out on a scanning electron microscope of SU1510 type (Hitachi, Japan) at an acceleration voltage of 15 kV. The results are shown in FIG. 3.
As can be seen from the analysis in fig. 3, the copper-cobalt composite oxide catalysts prepared in examples 1 and 2 have a large amount of mesoporous structures on the surface, wherein the surface structure of the Cu-Co-3 catalyst is the most bulky, which indicates that the Cu-Co-3 surface has more pore structures and is relatively uniformly distributed, which is consistent with the BET test result, and provides excellent reaction conditions for the diffusion and reaction of reactant molecules.
Fresh samples of the copper cobalt composite oxide catalysts prepared in examples 1 and 2 were both subjected to H2And (5) performing temperature programming reduction test. With H2H content of 5%2the-Ar mixed gas is reducing gas, and the content of H is 5 vol% at 25mL/min2Raising the temperature from room temperature to a set temperature at a speed of 10 ℃/min in the mixed atmosphere of/Ar, and recording the hydrogen consumption of the sample to obtain H2-a TPR map. The results are shown in FIG. 4.
From the analysis in fig. 4, it can be seen that the copper-cobalt composite oxide catalysts can provide active substances for the catalytic oxidation reaction of toluene at low temperature, wherein the temperature of the reduction peak position of the Cu-Co-3 catalyst is the lowest, which indicates that the Cu-Co-3 catalyst has the best low-temperature reducibility, and can provide more active substances for the catalytic combustion reaction of toluene at low temperature. Therefore, the copper-cobalt composite oxide catalyst prepared by the simple grinding method has high low-temperature reducible property, so that the catalytic oxidation of toluene under the low-temperature condition is promoted.
Example 3
This example investigates the effect of calcination temperature on catalyst performance. In this example, the same procedure as in example 1 was repeated except that the baking temperatures were changed to 300 ℃, 350 ℃ and 550 ℃. The prepared copper-cobalt composite oxide catalysts were respectively labeled 300-Cu-Co, 350-Cu-Co and 550-Cu-Co at reaction temperatures, and the copper-cobalt composite oxide catalyst prepared in example 1 was labeled 450-Cu-Co.
The catalysts were used for catalytic combustion of toluene, and the activity of the catalysts was evaluated in the same manner as in example 2. The results of the catalyst activity evaluation experiments on the conversion of the copper-cobalt composite oxide catalyst by catalytic combustion of toluene are shown in table 2:
TABLE 2 influence of calcination temperature on catalytic toluene Combustion Performance of the catalyst
From the analysis in table 2, it can be seen that the obtained copper-cobalt composite oxide catalyst has the best conversion effect on the toluene volatile organic compound catalytic combustion at the calcination temperature of 450 ℃, and the toluene conversion rate can reach 95.9% at the reaction temperature of 260 ℃. Thus, it was confirmed that the calcination temperature had an influence on the catalytic performance of the copper-cobalt composite oxide.
The copper-cobalt composite oxide catalysts obtained in example 3 were each subjected to X-ray diffraction analysis. The detection conditions were the same as in example 2. The results are shown in FIG. 5.
As can be seen from the analysis in FIG. 5, the Co/Cu composite oxide catalysts obtained in example 3 all use Co3O4And mainly CuO oxide, and the crystal phase of the catalyst is not changed with the increase of the roasting temperature, but the crystallinity of the catalyst is increased.
The above-mentioned embodiments are merely preferred embodiments for fully illustrating the present invention, and the scope of the present invention is not limited thereto. The equivalent substitution or change made by the technical personnel in the technical field on the basis of the invention is all within the protection scope of the invention. The protection scope of the invention is subject to the claims.
Claims (7)
1. The preparation method of the copper-cobalt composite oxide catalyst is characterized by comprising the following steps of:
s1, mixing copper salt, cobalt salt and a complexing agent, and grinding into a dry material;
s2, roasting the dry material in the S1, wherein the roasting condition is that the temperature is increased to 300-550 ℃ at the temperature increase rate of 10 ℃/min, then roasting at the constant temperature of 300-550 ℃ for 1-2 hours, and after the roasting is finished, taking out the roasted material after the temperature is reduced to the normal temperature to obtain the product;
the copper salt, the cobalt salt and the complexing agent are 1:2: 0-5 in molar ratio, and the complexing agent is oxalic acid.
2. The method of claim 1, wherein the copper salt is copper nitrate, copper sulfate or copper chloride.
3. The method for preparing a copper-cobalt composite oxide catalyst according to claim 1, wherein the cobalt salt is cobalt nitrate, cobalt sulfate or cobalt chloride.
4. The method according to claim 1, wherein the copper salt, the cobalt salt and the complexing agent are in a molar ratio of 1:2: 3.
5. The method for preparing the copper-cobalt composite oxide catalyst according to claim 1, wherein the baking temperature at constant temperature in S2 is 450 ℃ and the baking time is 2 h.
6. A copper-cobalt composite oxide catalyst produced by the production method according to any one of claims 1 to 5.
7. Use of the copper cobalt composite oxide catalyst of claim 6 in the degradation of volatile organic compounds.
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Cited By (4)
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| CN112264027A (en) * | 2020-10-27 | 2021-01-26 | 南京工业大学 | Copper-cobalt-cerium composite oxide catalytic combustion catalyst and preparation method and application thereof |
| CN113617373A (en) * | 2021-08-06 | 2021-11-09 | 大连海事大学 | Catalyst for removing volatile organic compounds and preparation method thereof |
| CN114029082A (en) * | 2021-12-01 | 2022-02-11 | 南京晓庄学院 | Synthesis method and application of novel high-activity magnetic nanoparticles |
| CN114870854A (en) * | 2022-05-05 | 2022-08-09 | 复旦大学 | Manganese-cobalt composite oxide catalyst and preparation method and application thereof |
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