CN114515586B - Catalyst for purifying volatile organic compounds and preparation method thereof - Google Patents
Catalyst for purifying volatile organic compounds and preparation method thereof Download PDFInfo
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- 239000003054 catalyst Substances 0.000 title claims abstract description 89
- 238000002360 preparation method Methods 0.000 title claims abstract description 31
- 239000012855 volatile organic compound Substances 0.000 title claims abstract description 24
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims abstract description 107
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 39
- KLFRPGNCEJNEKU-FDGPNNRMSA-L (z)-4-oxopent-2-en-2-olate;platinum(2+) Chemical compound [Pt+2].C\C([O-])=C\C(C)=O.C\C([O-])=C\C(C)=O KLFRPGNCEJNEKU-FDGPNNRMSA-L 0.000 claims abstract description 32
- 238000011068 loading method Methods 0.000 claims abstract description 27
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Substances [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims abstract description 23
- SHWZFQPXYGHRKT-FDGPNNRMSA-N (z)-4-hydroxypent-3-en-2-one;nickel Chemical compound [Ni].C\C(O)=C\C(C)=O.C\C(O)=C\C(C)=O SHWZFQPXYGHRKT-FDGPNNRMSA-N 0.000 claims abstract description 22
- LZKLAOYSENRNKR-LNTINUHCSA-N iron;(z)-4-oxoniumylidenepent-2-en-2-olate Chemical compound [Fe].C\C(O)=C\C(C)=O.C\C(O)=C\C(C)=O.C\C(O)=C\C(C)=O LZKLAOYSENRNKR-LNTINUHCSA-N 0.000 claims abstract description 19
- 239000012752 auxiliary agent Substances 0.000 claims abstract description 7
- 239000000126 substance Substances 0.000 claims abstract description 3
- 239000012298 atmosphere Substances 0.000 claims description 27
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 claims description 22
- 238000005303 weighing Methods 0.000 claims description 20
- 229910000366 copper(II) sulfate Inorganic materials 0.000 claims description 16
- 238000005470 impregnation Methods 0.000 claims description 14
- 238000002791 soaking Methods 0.000 claims description 14
- 238000001035 drying Methods 0.000 claims description 12
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 12
- 238000010438 heat treatment Methods 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 10
- 239000010949 copper Substances 0.000 claims description 6
- 229910000365 copper sulfate Inorganic materials 0.000 claims description 6
- 238000007598 dipping method Methods 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 238000004090 dissolution Methods 0.000 claims description 4
- 239000002904 solvent Substances 0.000 claims description 4
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 3
- 229910052742 iron Inorganic materials 0.000 claims 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 abstract description 21
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 abstract description 21
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 abstract description 21
- 230000009257 reactivity Effects 0.000 abstract description 10
- 239000000843 powder Substances 0.000 abstract 1
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 79
- 229910010271 silicon carbide Inorganic materials 0.000 description 77
- 238000011056 performance test Methods 0.000 description 15
- CDVAIHNNWWJFJW-UHFFFAOYSA-N 3,5-diethoxycarbonyl-1,4-dihydrocollidine Chemical compound CCOC(=O)C1=C(C)NC(C)=C(C(=O)OCC)C1C CDVAIHNNWWJFJW-UHFFFAOYSA-N 0.000 description 11
- 230000000052 comparative effect Effects 0.000 description 10
- 230000003197 catalytic effect Effects 0.000 description 9
- 229910000510 noble metal Inorganic materials 0.000 description 7
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 6
- 238000000034 method Methods 0.000 description 6
- 238000006243 chemical reaction Methods 0.000 description 5
- 230000000694 effects Effects 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000007084 catalytic combustion reaction Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- SZVJSHCCFOBDDC-UHFFFAOYSA-N ferrosoferric oxide Chemical compound O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- -1 pharmacy Substances 0.000 description 2
- POILWHVDKZOXJZ-ARJAWSKDSA-M (z)-4-oxopent-2-en-2-olate Chemical compound C\C([O-])=C\C(C)=O POILWHVDKZOXJZ-ARJAWSKDSA-M 0.000 description 1
- 206010028980 Neoplasm Diseases 0.000 description 1
- 230000010718 Oxidation Activity Effects 0.000 description 1
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- MCMNRKCIXSYSNV-UHFFFAOYSA-N ZrO2 Inorganic materials O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 1
- 238000007792 addition Methods 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 201000011510 cancer Diseases 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- XTVVROIMIGLXTD-UHFFFAOYSA-N copper(II) nitrate Chemical compound [Cu+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XTVVROIMIGLXTD-UHFFFAOYSA-N 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 201000010099 disease Diseases 0.000 description 1
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 239000000975 dye Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000010985 leather Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- JKQOBWVOAYFWKG-UHFFFAOYSA-N molybdenum trioxide Inorganic materials O=[Mo](=O)=O JKQOBWVOAYFWKG-UHFFFAOYSA-N 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000001699 photocatalysis Effects 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 230000000087 stabilizing effect Effects 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/20—Carbon compounds
- B01J27/22—Carbides
- B01J27/224—Silicon carbide
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- 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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- 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
- B01D53/8678—Removing components of undefined structure
- B01D53/8687—Organic components
-
- 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
- B01J35/613—10-100 m2/g
-
- 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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/02—Impregnation, coating or precipitation
- B01J37/0201—Impregnation
- B01J37/0205—Impregnation in several steps
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2257/00—Components to be removed
- B01D2257/70—Organic compounds not provided for in groups B01D2257/00 - B01D2257/602
- B01D2257/708—Volatile organic compounds V.O.C.'s
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/20—Air quality improvement or preservation, e.g. vehicle emission control or emission reduction by using catalytic converters
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- Chemical & Material Sciences (AREA)
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- Chemical Kinetics & Catalysis (AREA)
- Environmental & Geological Engineering (AREA)
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- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Biomedical Technology (AREA)
- Analytical Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Catalysts (AREA)
Abstract
The invention discloses a catalyst for purifying volatile organic compounds and a preparation method thereof, wherein the catalyst consists of a carrier, active components and auxiliary agents, and the carrier is CuSO 4/SiC; the active component is Pt; the auxiliary agents are Fe 3O4 and NiO. The CuSO 4/SiC carrier is prepared by loading CuSO 4 with SiC powder, and the loading amount of the CuSO 4 is 1wt% of the mass of the SiC. The active components Pt, the auxiliary agents Fe 3O4 and NiO are prepared by impregnating nickel acetylacetonate, platinum acetylacetonate and iron acetylacetonate in sequence, wherein the loading amount of NiO, pt, fe 3O4 is 0.1-0.4wt%, 0.1wt% and 0.2wt% of CuSO 4/SiC carrier by simple substance; the catalyst of the invention can be carried out in a low temperature range, and has high reactivity to toluene, ethyl acetate, acetone and ethanol.
Description
Technical Field
The invention belongs to the technical field of environmental protection, relates to a catalyst and a preparation method thereof, and particularly relates to a catalyst for purifying volatile organic compounds and a preparation method thereof.
Background
Volatile Organic Compounds (VOCs) are a common type of atmospheric pollutants that are highly toxic to humans and can cause cancer and other serious diseases. Volatile organic compounds relate to petrochemical industry, dyes, pharmacy, plastics, leather and other industries. VOCs also cause an increase in atmospheric ozone concentration and photochemical pollution, and it is important to strictly control the emission of VOCs.
Currently, methods for removing Volatile Organic Compounds (VOCs) include adsorption, photocatalytic, direct incineration, catalytic combustion, and the like. The catalytic oxidation technology is widely researched and applied because of the characteristics of low energy consumption, simple operation, high purification efficiency and the like. Noble metal catalysts are typical catalysts for catalytic combustion of VOCs. However, since noble metal resources are scarce and expensive, reducing the noble metal content has been a concern in the industry.
Patent CN202010797156.2 discloses a catalyst for eliminating volatile organic compounds, which is composed of a carrier, an active component and a cocatalyst, wherein the catalyst is a Pt/Ag 2O-MoO3/Al2(SO4)2-VOSO4-ZrO2 catalyst, and the catalyst has high catalytic activity, but the noble metal Pt reaches 0.5wt% and the Ag content is 1wt%, and the catalyst preparation is complex.
Disclosure of Invention
The invention aims to solve the defects of high noble metal Pt content and complex preparation of the existing catalyst and provide a catalyst for purifying volatile organic matters, which has low noble metal Pt content, high reaction activity and stable performance, and a preparation method thereof.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
The invention provides a catalyst for purifying volatile organic compounds, which comprises a carrier, active components and an auxiliary agent, wherein the carrier is CuSO 4/SiC, the active components are Pt, and the auxiliary agent is Fe 3O4 and NiO.
In the invention, cuSO 4 is added into SiC to ensure the existence of sulfate radical in the catalyst, so as to change the surface acidity of the catalyst, and the performance of the catalyst is improved by improving the surface acidity, and the SiC material is selected to be favorable for stabilizing the sulfate radical. The metal acetylacetonate compound (nickel acetylacetonate (Ni (C 5H7O2)2), platinum (II) acetylacetonate) (Pt (C 5H7O2)2 and iron acetylacetonate (Fe (C 5H7O2)3)) is selected to improve the performance of the catalyst by enabling the catalyst to have smaller particles or amorphous states on the one hand, and further to enable part of acetylacetonate or part of acetone to be carbonized during the roasting process of the N 2 atmosphere so as to be beneficial to the generation of small particle oxides or metals, and the stepwise impregnation is carried out so as to enable the distribution form of Fe 3O4 Pt-NiO to be changed to improve the performance of the catalyst.
As a preferred embodiment of the present invention, the specific surface area of SiC in the carrier is 50-60m 2/g.
As a preferred scheme of the invention, the loading amounts of NiO, pt and Fe3O4 are respectively 0.1-0.4wt% (calculated as Ni), 0.1wt% and 0.2wt% (calculated as Fe) of CuSO 4/SiC carrier in terms of simple substance.
The invention also provides a preparation method of the catalyst, which comprises the following steps:
1) Preparation of the carrier: weighing corresponding copper sulfate, adding water for dissolution, adding SiC for impregnation, drying and roasting to obtain a CuSO 4/SiC carrier;
2) Preparation of the catalyst: weighing corresponding nickel acetylacetonate, platinum acetylacetonate and iron acetylacetonate, respectively adding the nickel acetylacetonate, the platinum acetylacetonate and the iron acetylacetonate into solvents to prepare solutions, and immersing CuSO 4/SiC carriers in the solutions; heating under stirring, volatilizing the solvent, and roasting under N 2 atmosphere; finally roasting in air atmosphere to obtain the Fe 3O4-Pt-NiO/CuSO4/SiC catalyst.
In step 1), corresponding copper sulfate is weighed according to the weight percentage of Cu being 1wt% of SiC, the water used for dissolving the copper sulfate is 15-30mL, and the SiC dipping time is 0.5-1.5h.
As a preferable scheme of the invention, in the step 1), the drying temperature is 110-130 ℃, the drying time is 4.5-5.5h, the roasting temperature is 480-550 ℃, and the roasting time is 4.5-5.5h.
In the step 2), nickel acetylacetonate is weighed according to the proportion of 0.1-0.4wt% of the Ni load of CuSO 4/SiC carrier, platinum acetylacetonate is weighed according to the proportion of 0.1wt% of the Pt load of CuSO 4/SiC carrier, and iron acetylacetonate is weighed according to the proportion of 0.2wt% of the Fe load, and the platinum acetylacetonate solution, the platinum acetylacetonate solution and the iron acetylacetonate solution are respectively dissolved in acetone to obtain the nickel acetylacetonate solution, the platinum acetylacetonate solution and the iron acetylacetonate solution.
As a preferred embodiment of the present invention, in step 2), the impregnation sequence of the CuSO 4/SiC support is nickel acetylacetonate solution, platinum acetylacetonate solution, and iron acetylacetonate solution.
As a preferable scheme of the invention, the dipping time of the CuSO 4/SiC carrier in the nickel acetylacetonate solution is 0.5-1.2h, the dipping time of the platinum acetylacetonate solution is 0.5-1.2h, and the dipping time of the iron acetylacetonate solution is 1.5-2.5h.
As a preferable scheme of the invention, in the step 2), the roasting temperature is 480-550 ℃ and the roasting time is 4.5-5.5h under the atmosphere of N 2; the roasting temperature is 380-420 ℃ and the roasting time is 4.5-5.5h under the air atmosphere.
Compared with the prior art, the invention has the following beneficial effects:
1) The catalyst can be carried out in a low temperature range, and has high reactivity to toluene, ethyl acetate, acetone and ethanol;
2) The noble metal Pt content in the catalyst is low, and the catalyst performance is improved;
3) The preparation method of the catalyst has simple steps.
Drawings
FIG. 1 is an XRD pattern of the catalyst prepared in example 2 of the present invention, in which several diffraction peaks other than those of SiC were not attributed, and diffraction peaks associated with Fe 3O4、Pt、NiO、CuSO4 were not seen, indicating that Fe 3O4、Pt、NiO、CuSO4 particles were too small to be in an amorphous state.
Detailed Description
The technical solutions of the embodiments of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
The present embodiment provides a method for preparing a catalyst for purifying volatile organic compounds, comprising:
(1) Preparation of CuSO 4/SiC Carrier
Taking high specific surface area SiC as a carrier (specific surface area is 60m 2/g), weighing 0.7813g of copper sulfate (CuSO 4·5H2 O) according to the weight percent of Cu accounting for 1wt% of SiC, adding water for dissolution, then adding 20g of silicon carbide (SiC) carrier for soaking for 1 hour, then drying for 5 hours at 120 ℃, and finally roasting for 4 hours at 500 ℃ to obtain the CuSO 4/SiC carrier.
(2) Preparation of Fe 3O4-Pt-NiO/CuSO4/SiC catalyst
0.0438G of nickel acetylacetonate was weighed out and dissolved in 10mL of acetone solution at a Ni loading of 0.1wt% of CuSO 4/SiC support, and 10g of CuSO 4/SiC support was added to impregnate for 1 hour, which was referred to as A. Then weighing 0.0202g of platinum (II) acetylacetonate to be dissolved in 5mL of acetone solution according to the Pt load of 0.1wt% of CuSO 4/SiC carrier, adding the platinum (II) acetylacetonate acetone solution into the impregnating solution A for impregnation, and drying at 120 ℃ under the atmosphere of N 2 to obtain a sample B. According to the Fe loading amount of 0.2wt% of CuSO 4/SiC carrier, weighing 0.1261g of ferric acetylacetonate, dissolving in 5mL of acetone solution, adding the ferric acetylacetonate acetone solution into the sample B, and soaking for 2 hours. The acetone solution was volatilized by heating to 90℃with stirring, and then calcined at 500℃for 4 hours under an atmosphere of N 2. And then roasting for 4 hours at 400 ℃ in the air atmosphere to obtain the Fe 3O4-Pt-NiO/CuSO4/SiC catalyst.
(3) Catalyst Performance test
The catalyst performance evaluation is carried out in a reaction tube with the inner diameter of 8mm, the airspeed of 20000h -1, the measurement temperature is the temperature of gas entering the catalyst bed, and the reactants are toluene, ethyl acetate, acetone and ethanol respectively. The activity of the catalyst is expressed by the lowest reaction temperature T 99 at which the organic matter conversion rate reaches 99%, and the reactivity of the catalyst to toluene, ethyl acetate, acetone and ethanol is shown in Table 1.
Example 2
The present embodiment provides a method for preparing a catalyst for purifying volatile organic compounds, comprising:
(1) Preparation of CuSO 4/SiC support was the same as in example 1;
(2) Preparation of Fe 3O4-Pt-NiO/CuSO4/SiC catalyst
0.0875G of nickel acetylacetonate is weighed according to the Ni loading amount of 0.2wt% of CuSO 4/SiC carrier, dissolved in 10mL of acetone solution, and 10g of CuSO 4/SiC carrier is added for soaking for 1 hour, which is called A. Then weighing 0.0202g of platinum (II) acetylacetonate to be dissolved in 5mL of acetone solution according to the Pt load of 0.1wt% of CuSO 4/SiC carrier, adding the platinum (II) acetylacetonate acetone solution into the impregnating solution A for impregnation, and drying at 120 ℃ under the atmosphere of N 2 to obtain a sample B. According to the Fe loading amount of 0.2wt% of CuSO 4/SiC carrier, weighing 0.1261g of ferric acetylacetonate, dissolving in 5mL of acetone solution, adding the ferric acetylacetonate acetone solution into the sample B, and soaking for 2 hours. The acetone solution was volatilized by heating to 90℃with stirring, and then calcined at 500℃for 4 hours under an atmosphere of N 2. And then roasting for 4 hours at 400 ℃ in the air atmosphere to obtain the Fe 3O4-Pt-NiO/CuSO4/SiC catalyst.
(3) Catalyst Performance test
Catalyst performance test the same as in example 1 and catalytic reactivity is shown in table 1.
Example 3
The present embodiment provides a method for preparing a catalyst for purifying volatile organic compounds, comprising:
(1) Preparation of CuSO 4/SiC support was the same as in example 1;
(2) Preparation of Fe 3O4-Pt-NiO/CuSO4/SiC catalyst
According to the Ni loading amount of 0.3wt% of CuSO 4/SiC carrier, weighing 0.1313g of nickel acetylacetonate, dissolving in 10mL of acetone solution, adding 10g of CuSO 4/SiC carrier, and soaking for 1 hour, namely A. Then weighing 0.0202g of platinum (II) acetylacetonate to be dissolved in 5mL of acetone solution according to the Pt load of 0.1wt% of CuSO 4/SiC carrier, adding the platinum (II) acetylacetonate acetone solution into the impregnating solution A for impregnation, and drying at 120 ℃ under the atmosphere of N 2 to obtain a sample B. According to the Fe loading amount of 0.2wt% of CuSO 4/SiC carrier, weighing 0.1261g of ferric acetylacetonate, dissolving in 5mL of acetone solution, adding the ferric acetylacetonate acetone solution into the sample B, and soaking for 2 hours. The acetone solution was volatilized by heating to 90℃with stirring, and then calcined at 500℃for 4 hours under an atmosphere of N 2. And then roasting for 4 hours at 400 ℃ in the air atmosphere to obtain the Fe 3O4-Pt-NiO/CuSO4/SiC catalyst.
(3) Catalyst Performance test
Catalyst performance test the same as in example 1 and catalytic reactivity is shown in table 1.
Example 4
The present embodiment provides a method for preparing a catalyst for purifying volatile organic compounds, comprising:
(1) Preparation of CuSO 4/SiC support was the same as in example 1;
(2) Preparation of Fe 3O4-Pt-NiO/CuSO4/SiC catalyst
According to the Ni loading amount of 0.4wt% of CuSO 4/SiC carrier, weighing 0.1751g of nickel acetylacetonate, dissolving in 10mL of acetone solution, adding 10g of CuSO 4/SiC carrier, and soaking for 1 hour, namely A. Then weighing 0.0202g of platinum (II) acetylacetonate to be dissolved in 5mL of acetone solution according to the Pt load of 0.1wt% of CuSO 4/SiC carrier, adding the platinum (II) acetylacetonate acetone solution into the impregnating solution A for impregnation, and drying at 120 ℃ under the atmosphere of N 2 to obtain a sample B. According to the Fe loading amount of 0.2wt% of CuSO 4/SiC carrier, weighing 0.1261g of ferric acetylacetonate, dissolving in 5mL of acetone solution, adding the ferric acetylacetonate acetone solution into the sample B, and soaking for 2 hours. The acetone solution was volatilized by heating to 90℃with stirring, and then calcined at 500℃for 4 hours under an atmosphere of N 2. And then roasting for 4 hours at 400 ℃ in the air atmosphere to obtain the Fe 3O4-Pt-NiO/CuSO4/SiC catalyst.
(3) Catalyst Performance test
Catalyst performance test the same as in example 1 and catalytic reactivity is shown in table 1.
Comparative example 1
(1) Preparation of Fe 3O4 -Pt-NiO/SiC catalyst
0.0875G of nickel acetylacetonate was weighed out and dissolved in 10mL of acetone solution, and 10g of SiC carrier was added to impregnate for 1 hour, which was called A, according to Ni loading of 0.2wt% of the SiC carrier. Then, according to platinum (II) acetylacetonate with the Pt loading of 0.1wt%, and according to the Pt loading of 0.1wt% of the SiC carrier, 0.0202g of platinum (II) acetylacetonate is weighed and dissolved in 5mL of acetone solution, the platinum (II) acetylacetonate solution is added into the impregnating solution A for impregnation, and the sample B is obtained by drying at 120 ℃ under the atmosphere of N 2. Iron acetylacetonate 0.1261g was weighed and dissolved in 5mL of acetone solution, and the iron acetylacetonate acetone solution was added to the sample B and immersed for 2 hours, according to the Fe loading of 0.2wt% of the SiC carrier. The acetone solution was volatilized by heating to 90℃with stirring, and then calcined at 500℃for 4 hours under an atmosphere of N 2. And then roasting for 4 hours at 400 ℃ in the air atmosphere to obtain the Fe 3O4 -Pt-NiO/SiC catalyst.
(2) Catalyst Performance test
Catalyst performance test the same as in example 1 and catalytic reactivity is shown in table 1.
Comparative example 2
(1) Preparation of CuSO 4/SiC support was the same as in example 1;
(2) Preparation of Fe 3O4-Pt-NiO/CuSO4/SiC catalyst
Weighing 0.0875g of nickel acetylacetonate according to the Ni loading amount of 0.2wt% of CuSO 4/SiC carrier; weighing 0.0202g of platinum (II) acetylacetonate according to the Pt loading amount of 0.1wt% of CuSO 4/SiC carrier; weighing 0.1261g of ferric acetylacetonate according to the Fe loading amount of 0.2wt% of CuSO 4/SiC carrier; the above nickel acetylacetonate, platinum (II) acetylacetonate and iron acetylacetonate were mixed and dissolved in 20mL of an acetone solution, followed by immersing in 10g of CuSO 4/SiC carrier for 2 hours. The acetone solution was volatilized by heating to 90℃with stirring, and then calcined at 500℃for 4 hours under an atmosphere of N 2. And then roasting for 4 hours at 400 ℃ in the air atmosphere to obtain the Fe 3O4-Pt-NiO/CuSO4/SiC catalyst.
(3) Catalyst Performance test
Catalyst performance test the same as in example 1 and catalytic reactivity is shown in table 1.
Comparative example 3
(1) Preparation of CuO/SiC Carrier
0.5861G of copper nitrate (Cu (NO 3)2) is weighed according to the weight percentage of Cu accounting for 1wt% of SiC by taking SiC with high specific surface area as a carrier (specific surface area of 60m 2/g), 20ml of water is added for dissolution, then 20g of silicon carbide (SiC) carrier is added for soaking for 1 hour, then the carrier is baked for 5 hours at 120 ℃, and finally the CuO/SiC carrier is obtained after roasting for 4 hours at 500 ℃.
(2) Preparation of Fe 3O4 -Pt-NiO/CuO/SiC catalyst
0.0875G of nickel acetylacetonate was weighed out and dissolved in 10mL of acetone solution, and 10g of CuO/SiC support was added thereto for 1 hour to impregnate the support, which was referred to as A, according to the Ni loading of 0.2wt% of the CuO/SiC support. Then, according to the Pt load of 0.1wt% of the CuO/SiC carrier, 0.0202g of platinum (II) acetylacetonate is weighed and dissolved in 5mL of acetone solution, the platinum (II) acetylacetonate acetone solution is added into the impregnating solution A for impregnation, and the sample B is obtained by drying at 120 ℃ under the atmosphere of N 2. Iron acetylacetonate 0.1261g was weighed and dissolved in 5mL of acetone solution, and the iron acetylacetonate acetone solution was added to the sample B and immersed for 2 hours, according to the Fe loading of 0.2wt% of the CuO/SiC carrier. The acetone solution was volatilized by heating to 90℃with stirring, and then calcined at 500℃for 4 hours under an atmosphere of N 2. And then roasting for 4 hours at 400 ℃ in the air atmosphere to obtain the Fe 3O4 -Pt-NiO/CuO/SiC catalyst.
(3) Catalyst Performance test
Catalyst performance test the same as in example 1 and catalytic reactivity is shown in table 1.
Comparative example 4
(1) Preparation of CuSO 4/SiC support was the same as in example 1;
(2) Preparation of Fe 3O4-Pt-NiO/CuSO4/SiC catalyst
0.0875G of nickel acetylacetonate is weighed according to the Ni loading amount of 0.2wt% of CuSO 4/SiC carrier, dissolved in 10mL of acetone solution, and 10g of CuSO 4/SiC carrier is added for soaking for 1 hour, which is called A. Then weighing 0.0202g of platinum (II) acetylacetonate to be dissolved in 5mL of acetone solution according to the Pt load of 0.1wt% of CuSO 4/SiC carrier, adding the platinum (II) acetylacetonate acetone solution into the impregnating solution A for impregnation, and drying at 120 ℃ under the atmosphere of N 2 to obtain a sample B. According to the Fe loading amount of 0.2wt% of CuSO 4/SiC carrier, weighing 0.1261g of ferric acetylacetonate, dissolving in 5mL of acetone solution, adding the ferric acetylacetonate acetone solution into the sample B, and soaking for 2 hours. Heating to 90 ℃ under stirring, volatilizing the acetone solution, and roasting for 4 hours at 400 ℃ in an air atmosphere to obtain the Fe 3O4-Pt-NiO/CuSO4/SiC catalyst.
(3) Catalyst Performance test
Catalyst performance test the same as in example 1 and catalytic reactivity is shown in table 1.
Table 1: examples 1-4 and comparative examples 1-3 catalysts T 99 temperature for reactions of toluene, ethyl acetate, acetone, ethanol
As can be seen from Table 1, the catalysts of examples 1-4 all exhibited very high benzene, toluene, ethyl acetate, ethanol oxidation activity. Wherein the catalyst of example 2 has the highest activity and the lowest temperature T 99 for benzene, toluene, ethyl acetate and ethanol, the most difficult to catalyze of these VOCs is the T 99 of 230 ℃. The catalysts of examples 1-4 all performed higher than the catalysts of comparative examples 1-3. The comparative example 1 catalyst lacks the CuSO 4 component compared to the example catalyst; the catalyst of comparative example 2 was prepared by co-impregnation of Fe 3O4 -Pt-NiO; comparative example 3 the catalyst replaced the CuSO 4 of the example with CuO; comparative example 4 the catalyst was calcined at 500 c for 4 hours in the absence of an atmosphere of N 2 during calcination. The catalyst composition and preparation method of the examples are shown to be advantageous for obtaining high performance catalysts.
While the invention has been described with respect to preferred embodiments thereof, it will be understood by those skilled in the art that various modifications and additions may be made without departing from the scope of the invention. Equivalent embodiments of the present invention will be apparent to those skilled in the art having the benefit of the teachings disclosed herein, when considered in the light of the foregoing disclosure, and without departing from the spirit and scope of the invention; meanwhile, any equivalent changes, modifications and evolution of the above embodiments according to the essential technology of the present invention still fall within the scope of the technical solution of the present invention.
Claims (4)
1. The catalyst for purifying the volatile organic compounds is characterized by comprising a carrier, an active component and an auxiliary agent, wherein the carrier is CuSO 4/SiC, the active component is Pt, the auxiliary agent is Fe 3O4 and NiO, and the loading amounts of NiO, pt and Fe 3O4 are respectively 0.1-0.4wt%, 0.1wt% and 0.2wt% of the CuSO 4/SiC carrier according to simple substance metering;
the preparation method of the catalyst for purifying volatile organic compounds comprises the following steps:
1) Preparation of the carrier: weighing corresponding copper sulfate according to the mass of Cu being 1wt% of SiC, adding water for dissolution, wherein the water consumption for dissolving the copper sulfate is 15-30mL, adding SiC for soaking, the SiC soaking time is 0.5-1.5h, the SiC soaking time is 110-130 ℃ for drying 4.5-5.5h, and the Cu is 480-550 ℃ for roasting 4.5-5.5h, so that a CuSO 4/SiC carrier is obtained;
2) Preparation of the catalyst: weighing corresponding nickel acetylacetonate, platinum acetylacetonate and iron acetylacetonate, respectively adding into solvents to prepare solutions, and dipping CuSO 4/SiC carrier in the solutions, wherein the dipping sequence of the CuSO 4/SiC carrier is nickel acetylacetonate solution, platinum acetylacetonate solution and iron acetylacetonate solution; heating under stirring, volatilizing solvent, and roasting at 480-550 ℃ for 4.5-5.5h under N 2 atmosphere; finally roasting for 4.5-5.5 hours at 380-420 ℃ in air atmosphere to obtain the Fe 3O4-Pt-NiO /CuSO4/SiC catalyst.
2. A catalyst for purifying volatile organic compounds according to claim 1, wherein the specific surface area of SiC in the carrier is 50-60m 2/g.
3. The catalyst for purifying volatile organic compounds according to claim 1, wherein in the step 2), nickel acetylacetonate is weighed according to 0.1 to 0.4wt% of a Ni loading amount of CuSO 4/SiC carrier, platinum acetylacetonate is weighed according to 0.1wt% of a Pt loading amount of CuSO 4/SiC carrier, and iron acetylacetonate is weighed according to 0.2wt% of a Fe loading amount, and is dissolved in acetone to obtain a nickel acetylacetonate solution, a platinum acetylacetonate solution and an iron acetylacetonate solution, respectively.
4. The catalyst for purifying volatile organic compounds according to claim 1, wherein the impregnation time of the CuSO 4/SiC support in the nickel acetylacetonate solution is 0.5 to 1.2 hours, the impregnation time in the platinum acetylacetonate solution is 0.5 to 1.2 hours, and the impregnation time in the iron acetylacetonate solution is 1.5 to 2.5 hours.
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| CN105478136A (en) * | 2015-12-24 | 2016-04-13 | 浙江大学 | Industrial organic waste gas catalytic degradation catalyst cooperated with low-temperature plasma, and preparation method and application of catalyst |
| CN109046345A (en) * | 2018-08-01 | 2018-12-21 | 中国科学院城市环境研究所 | A kind of loaded catalyst and its preparation method and application |
| CN110898834A (en) * | 2019-11-29 | 2020-03-24 | 金华铂锐催化科技有限公司 | Catalyst for eliminating volatile organic compounds and preparation method thereof |
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| CN105478136A (en) * | 2015-12-24 | 2016-04-13 | 浙江大学 | Industrial organic waste gas catalytic degradation catalyst cooperated with low-temperature plasma, and preparation method and application of catalyst |
| CN109046345A (en) * | 2018-08-01 | 2018-12-21 | 中国科学院城市环境研究所 | A kind of loaded catalyst and its preparation method and application |
| CN110898834A (en) * | 2019-11-29 | 2020-03-24 | 金华铂锐催化科技有限公司 | Catalyst for eliminating volatile organic compounds and preparation method thereof |
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