CN114768814A - Preparation method of catalyst for catalytic combustion of VOCs and product thereof - Google Patents
Preparation method of catalyst for catalytic combustion of VOCs and product thereof Download PDFInfo
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- CN114768814A CN114768814A CN202210432968.6A CN202210432968A CN114768814A CN 114768814 A CN114768814 A CN 114768814A CN 202210432968 A CN202210432968 A CN 202210432968A CN 114768814 A CN114768814 A CN 114768814A
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- 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
- B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/83—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with rare earths or actinides
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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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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F23—COMBUSTION APPARATUS; COMBUSTION PROCESSES
- F23G—CREMATION FURNACES; CONSUMING WASTE PRODUCTS BY COMBUSTION
- F23G2209/00—Specific waste
- F23G2209/14—Gaseous waste or fumes
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Abstract
The invention discloses a preparation method of a catalyst for catalytic combustion of VOCs and a product thereof. According to the catalyst, gallium oxide is prepared by a hydrothermal method, then substances such as a copper source, a cerium source, urea, polyvinylpyrrolidone and the like are added, a hydrothermal reaction is carried out again to obtain the copper and cerium co-modified gallium oxide catalyst, the crystal form of the catalyst can be remarkably improved by two-step hydrothermal reaction, the improvement of the specific surface area of the catalyst is promoted, the catalytic combustion performance of gallium oxide can be remarkably improved by the modification of copper and cerium, and the purification of VOCs is effectively improved, so that the catalyst is an ideal material for treating VOCs.
Description
Technical Field
The invention relates to the field of VOCs treatment, in particular to a preparation method of a catalyst for catalytic combustion of VOCs and a product thereof.
Background
Volatile Organic Compounds (VOCs) refer to organic compounds with saturated vapor pressure of more than 70Pa at normal temperature and boiling point of below 260 ℃ at normal pressure, and include alkanes, aromatic hydrocarbons, olefins, alcohols, aldehydes, ketones, halogenated hydrocarbons and the like, and common emission sources in daily life include building materials, decoration materials, adhesives of furniture, kitchen fumes, motor vehicle exhaust emission and the like; the common main sources in the industrial aspect are chemical industry and petrochemical industry waste gas, cleaning agents in the electronic industry, printing industry, production and use of paint and coating, waste gas discharged in industrial processes such as power plant boiler tail gas and the like, most VOCs are toxic and smelly, and some VOCs are carcinogenic and cause great harm to human health; the VOCs can also perform photochemical reaction with nitrogen oxides in the atmosphere under the action of sunlight to generate photochemical smog with higher toxicity. In recent years, the method has become one of the main atmospheric pollutants in China, so that the purification treatment technology of the VOCs has become a research hotspot problem in the field of environmental catalysis.
The main methods for treating the VOCs comprise adsorption methods, catalytic methods and other means, wherein the catalytic methods comprise catalytic combustion methods, the catalytic combustion methods can treat low-concentration VOCs gas at a temperature far lower than the direct combustion temperature, and the method has the characteristics of high purification efficiency, no secondary pollution and low energy consumption, and is one of the most effective treatment methods for treating the VOCs in commerce. Su et al in CuO-CeO2Pd/CuO-CeO is prepared for the precursor2-Y2O3The catalyst has good catalytic combustion activity and thermal stability of toluene and ethyl acetate, and the key of the activity is carrier CuO-CeO2The solid solution structure of (1); tidahy et al found 0.5% Pd/NaFAU and 5% Cu/ZrO2The catalyst has good toluene catalytic combustion potential, the activity of the Pd-based catalyst is related to the carrier, and the activity of the Cu-based catalyst is related to the fluidity of oxygen. Avgouropoulos et Al Pt/Al2O3A small amount of basic substance (K, Na) was added to the catalyst to neutralize the acid active site and reduce the formation of diethyl ether and ethylene, and potassium (n (K)/n (Al) 0.1) was added to the catalyst to make Pt/Al catalyst2O3The complete conversion temperature of the ethanol is reduced from 280 ℃ to 220 ℃. From the above, although the catalyst using the noble metal as a carrier has excellent catalytic combustion performance, the noble metal is expensive and has a relatively simple performance. Therefore, it is necessary to develop a new catalytic combustion catalyst, which has excellent catalytic performance on the basis of reducing the production cost, and is still a problem to be solved urgently at present.
Disclosure of Invention
The technical problem to be solved by the present invention is to provide a preparation method of a catalyst for catalytic combustion of VOCs and a product thereof, aiming at the defects in the prior art. According to the catalyst, gallium oxide is prepared by a hydrothermal method, then substances such as a copper source, a cerium source, urea, polyvinylpyrrolidone and the like are added, a hydrothermal reaction is carried out again to obtain the copper and cerium co-modified gallium oxide catalyst, the crystal form of the catalyst can be remarkably improved by two-step hydrothermal reaction, the improvement of the specific surface area of the catalyst is promoted, the catalytic combustion performance of gallium oxide can be remarkably improved by the modification of copper and cerium, and the purification of VOCs is effectively improved, so that the catalyst is an ideal material for treating VOCs.
The invention adopts the following technical scheme:
a preparation method of a catalyst for catalytic combustion of VOCs comprises the following steps:
(1) adding a gallium salt and a regulator into a mixed solution of ethanol and water, magnetically stirring at room temperature, uniformly mixing, pouring into a hydrothermal reaction kettle, reacting at 180-200 ℃ for 12-24 hours, filtering the obtained suspension after the reaction kettle is cooled, washing with ethanol, centrifuging, filtering for 3 times, drying at 80-120 ℃ for 12-14 hours, and calcining at 300-500 ℃ for 10-40 hours to obtain gallium oxide;
(2) adding gallium oxide into a mixture containing copper salt, cerium salt, urea, polyvinylpyrrolidone, ethanol and deionized water, stirring, uniformly stirring, adding into a hydrothermal reaction kettle, reacting for 10-20 hours at 100-140 ℃, filtering the obtained suspension after the reaction kettle is cooled after the reaction is finished, washing with ethanol, centrifuging, filtering for 3 times, drying for 12-24 hours at 80-100 ℃, and calcining for 4-6 hours at 400-500 ℃ to obtain a gallium oxide catalyst jointly modified by copper and cerium, wherein the mass fraction of copper relative to gallium oxide is 2-4 wt%; the mass fraction of cerium relative to gallium oxide is 2-4 wt%.
Preferably, in step (1), the regulator is sodium acetate, sodium dodecylbenzenesulfonate or trisodium citrate.
Preferably, in step (1), the gallium salt is gallium nitrate, gallium acetate or gallium chloride.
Preferably, in the step (1), the molar ratio of the gallium salt to the regulator is 1: 0.2 to 0.4; the volume ratio of the ethanol to the water is 1: 1.
Preferably, in the step (1), the stirring speed is 300-400 rpm, and the stirring time is 0.5-1 h.
Preferably, in the step (2), the copper salt is copper nitrate, copper chloride or copper acetate; the cerium salt is cerium nitrate, cerium chloride or cerium acetate.
Preferably, in step (2), the ratio of urea, polyvinylpyrrolidone, ethanol and water is: 1-3 g: 3-5 g: 50-60 mL: 50-60 mL.
Preferably, in the step (2), the stirring speed is 300-400 rpm, and the stirring time is 1-2 hours.
According to another technical scheme, the catalyst for catalytic combustion of VOCs prepared by the preparation method is a gallium oxide catalyst jointly modified by copper and cerium, wherein the mass fraction of copper relative to gallium oxide is 2-4 wt%; the mass fraction of cerium relative to gallium oxide is 2-4 wt%.
According to another technical scheme, the catalyst for catalytic combustion of VOCs is used for catalytic combustion of VOCs based on the application of the catalyst for catalytic combustion of VOCs, and the VOCs comprises acetone, chlorobenzene and toluene.
The preparation method of the catalyst for catalytic combustion of VOCs and the product thereof provided by the invention have the following technical effects:
(1) the copper and cerium co-modified gallium oxide catalyst prepared by two-step hydrothermal method can well promote crystal formation, increases catalytic active sites, and further promotes the improvement of catalytic performance due to the fact that copper and cerium are doped into crystal lattices of gallium oxide.
(2) The T is reduced by the common modification of copper and cerium and the synergistic action of copper and cerium50(T50Representing 50% conversion) and T90(T90The conversion rate reaches 90%), the corresponding reaction temperature effectively improves the purification capacity of the catalyst.
(3) The adoption of the regulator can obviously improve the crystal form of gallium oxide, improve the active site of the catalyst and promote the obvious improvement of the catalytic performance.
(4) The preparation method is simple and easy to control, and the prepared product has excellent performance and is beneficial to industrial production.
In conclusion, the catalyst for catalytic combustion of VOCs prepared by the invention has excellent catalytic performance and good purification capacity for VOCs, and is an ideal material for purifying VOCs.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are some embodiments of the present invention, but not all embodiments. The components of the embodiments of the present invention generally shown may be arranged and designed in a wide variety of different configurations. Thus, the following detailed description of the embodiments of the present invention is not intended to limit the scope of the invention as claimed, but is merely representative of selected embodiments of the invention. All other embodiments, which can be obtained by a person skilled in the art without inventive step based on the embodiments of the present invention, are within the scope of protection of the present invention.
Example 1
A preparation method of a catalyst for catalytic combustion of VOCs is characterized by comprising the following steps: the method comprises the following steps:
(1) adding 5mmol of gallium nitrate and 1.5mmol of trisodium citrate into 100mL of mixed solution of ethanol and water, wherein the volume ratio of ethanol to water is 1:1, magnetically stirring at room temperature, the stirring speed is 350rpm, stirring time is 1h, uniformly mixing, pouring into a hydrothermal reaction kettle, reacting at 190 ℃ for 20h, filtering the obtained suspension after the reaction kettle is cooled after the reaction is finished, washing with ethanol, centrifuging, filtering for 3 times, drying at 100 ℃ for 13h, and calcining at 400 ℃ for 30h to obtain gallium oxide;
(2) adding gallium oxide into a mixture containing copper nitrate, cerium nitrate, 1g of urea, 4g of polyvinylpyrrolidone, 55mL of ethanol and 55mL of deionized water, stirring at the stirring speed of 350rpm for 1.5h, uniformly stirring, adding into a hydrothermal reaction kettle, reacting at 120 ℃ for 15h, filtering the obtained suspension after the reaction is finished and the reaction kettle is cooled, washing with ethanol, centrifuging and filtering for 3 times, drying at 90 ℃ for 18h, and calcining at 450 ℃ for 5h to obtain a gallium oxide catalyst jointly modified by copper and cerium, wherein the mass fraction of copper relative to gallium oxide is 3 wt%; the mass fraction of cerium with respect to gallium oxide was 3 wt%.
Example 2
A preparation method of a catalyst for catalytic combustion of VOCs comprises the following steps:
(1) adding 5mmol of gallium acetate and 2mmol of sodium acetate into 100mL of mixed solution of ethanol and water, wherein the volume ratio of the ethanol to the water is 1:1, magnetically stirring at room temperature, the stirring speed is 400rpm, the stirring time is 0.5h, uniformly mixing, pouring into a hydrothermal reaction kettle, then reacting at 200 ℃ for 12h, filtering the obtained suspension after the reaction kettle is cooled after the reaction is finished, washing with ethanol, centrifuging, filtering for 3 times, drying at 120 ℃ for 12h, and calcining at 500 ℃ for 10h to obtain gallium oxide;
(2) adding gallium oxide into a mixture containing copper chloride, cerium acetate, 3g of urea, 5g of polyvinylpyrrolidone, 60mL of ethanol and 60mL of deionized water, stirring at the stirring speed of 400rpm for 1h, uniformly stirring, adding the mixture into a hydrothermal reaction kettle, reacting at 140 ℃ for 10h, filtering the obtained suspension after the reaction kettle is cooled after the reaction is finished, washing with ethanol, centrifuging and filtering for 3 times, drying at 100 ℃ for 12h, and calcining at 500 ℃ for 4h to obtain a copper and cerium jointly modified gallium oxide catalyst, wherein the mass fraction of copper relative to gallium oxide is 4 wt%; the mass fraction of cerium with respect to gallium oxide was 2 wt%.
Example 3
A preparation method of a catalyst for catalytic combustion of VOCs comprises the following steps:
(1) adding 5mmol of gallium chloride and 1mmol of trisodium citrate into a mixed solution of 100mL of ethanol and water, wherein the volume ratio of the ethanol to the water is 1: 1; magnetic stirring is carried out at room temperature, the stirring speed is 300rpm, the stirring time is 1h, the mixture is uniformly mixed and poured into a hydrothermal reaction kettle, then the mixture reacts for 24h at 180 ℃, the obtained suspension is filtered after the reaction kettle is cooled, washed by ethanol, centrifuged and filtered for 3 times, then the obtained suspension is dried for 14h at 80 ℃, and then calcined for 40h at 300 ℃ to obtain gallium oxide;
(2) adding gallium oxide into a mixture containing copper acetate, cerium chloride, 1g of urea, 3g of polyvinylpyrrolidone, 50mL of ethanol and 50mL of deionized water, stirring at the stirring speed of 300rpm for 2h, uniformly stirring, adding the mixture into a hydrothermal reaction kettle, reacting at 100 ℃ for 20h, filtering the obtained suspension after the reaction kettle is cooled after the reaction is finished, washing with ethanol, centrifuging and filtering for 3 times, drying at 80 ℃ for 24h, and calcining at 400 ℃ for 6h to obtain a copper and cerium co-modified gallium oxide catalyst, wherein the mass fraction of copper relative to gallium oxide is 2 wt%; the mass fraction of cerium with respect to gallium oxide was 4 wt%.
Comparative example 1
The same procedure and conditions as in example 1 were followed without addition of trisodium citrate.
Comparative example 2
Only copper nitrate was added with a mass fraction of copper to gallium oxide of 6 wt%, and other steps and conditions were the same as in example 1.
Comparative example 3
Only cerium nitrate was added with a cerium mass fraction of 6 wt% with respect to gallium oxide, and the other steps and conditions were the same as in example 1.
Comparative example 4
The copper and cerium modifications were not performed and other steps and conditions were the same as in example 1.
Comparative example 5
The procedure and conditions were the same as in example 1, except that polyvinylpyrrolidone was not added.
The catalysts of examples 1-3 and comparative examples 1-5 were used to catalytically combust VOCs. The specific method comprises the following steps:
the catalytic combustion reaction of VOCs (acetone, chlorobenzene or toluene) is carried out on a fixed bed reactor, the inner diameter of a reaction tube is 10mm, and the loading amount of the catalyst is 150 mg. Using a gas chromatograph model SC-8000 equipped with a Flame Ionization Detector (FID)Performing on-line analysis on the concentrations of VOCs and organic matters before and after reaction, and simultaneously introducing reaction tail gas into SC-3000 type gas chromatograph equipped with Thermal Capture Detector (TCD) to detect CO and CO2And (4) concentration. The composition of the raw material gas in the reaction is 0.2 percent of VOCs (acetone, chlorobenzene or toluene) + air, the normal pressure and the space velocity (GHSV) of the flow regulation reaction of the raw material gas are 5000 mL/(h.g).
Specific test results are shown in table 1:
TABLE 1 test results of examples 1-3 and comparative examples 1-5
It can be found from the comparison between the above examples 1-3 and comparative examples 1-5 that the catalyst of the present application has excellent catalytic combustion performance, has good purification effect on VOCs, and improves the purification capability of the catalyst due to the synergistic effect of copper and cerium, so that the catalyst of the present application is an ideal material for purifying VOCs.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (10)
1. A preparation method of a catalyst for catalytic combustion of VOCs is characterized by comprising the following steps: the method comprises the following steps:
(1) adding a gallium salt and a regulator into a mixed solution of ethanol and water, magnetically stirring at room temperature, uniformly mixing, pouring into a hydrothermal reaction kettle, reacting at 180-200 ℃ for 12-24 hours, filtering the obtained suspension after the reaction kettle is cooled, washing with ethanol, centrifuging, filtering for 3 times, drying at 80-120 ℃ for 12-14 hours, and calcining at 300-500 ℃ for 10-40 hours to obtain gallium oxide;
(2) adding gallium oxide into a mixture containing copper salt, cerium salt, urea, polyvinylpyrrolidone, ethanol and deionized water, stirring, uniformly stirring, adding into a hydrothermal reaction kettle, reacting for 10-20 hours at 100-140 ℃, filtering the obtained suspension after the reaction kettle is cooled after the reaction is finished, washing with ethanol, centrifuging, filtering for 3 times, drying for 12-24 hours at 80-100 ℃, and calcining for 4-6 hours at 400-500 ℃ to obtain a gallium oxide catalyst jointly modified by copper and cerium, wherein the mass fraction of copper relative to gallium oxide is 2-4 wt%; the mass fraction of cerium relative to gallium oxide is 2-4 wt%.
2. The method of claim 1, wherein: in the step (1), the regulator is sodium acetate, sodium dodecyl benzene sulfonate or trisodium citrate.
3. The method of claim 1, wherein: in the step (1), the gallium salt is gallium nitrate, gallium acetate or gallium chloride.
4. The production method according to claim 1, characterized in that: in the step (1), the molar ratio of the gallium salt to the regulator is 1: 0.2 to 0.4; the volume ratio of the ethanol to the water is 1: 1.
5. The method of claim 1, wherein: in the step (1), the stirring speed is 300-400 rpm, and the stirring time is 0.5-1 h.
6. The production method according to claim 1, characterized in that: in the step (2), the copper salt is copper nitrate, copper chloride or copper acetate; the cerium salt is cerium nitrate, cerium chloride or cerium acetate.
7. The method of claim 1, wherein: in the step (2), the proportion of the urea, the polyvinylpyrrolidone, the ethanol and the water is as follows: 1-3 g: 3-5 g: 50-60 mL: 50-60 mL.
8. The production method according to claim 1, characterized in that: in the step (2), the stirring speed is 300-400 rpm, and the stirring time is 1-2 h.
9. The catalyst for catalyzing and combusting VOCs prepared by the preparation method according to any one of claims 1-8, wherein the catalyst for catalyzing and combusting VOCs is a gallium oxide catalyst modified by copper and cerium together, wherein the mass fraction of copper relative to gallium oxide is 2-4 wt%; the mass fraction of cerium relative to gallium oxide is 2-4 wt%.
10. Use of a catalyst for catalytic combustion of VOCs according to claim 9, wherein the catalyst for catalytic combustion of VOCs comprising acetone, chlorobenzene and toluene is used for catalytic combustion of VOCs.
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