CN106111154A - Quaternary compound oxide type catalyst for the VOCs that degrades and preparation method thereof - Google Patents
Quaternary compound oxide type catalyst for the VOCs that degrades and preparation method thereof Download PDFInfo
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- CN106111154A CN106111154A CN201610453755.6A CN201610453755A CN106111154A CN 106111154 A CN106111154 A CN 106111154A CN 201610453755 A CN201610453755 A CN 201610453755A CN 106111154 A CN106111154 A CN 106111154A
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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
- B01J23/76—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
- B01J23/84—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 arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/889—Manganese, technetium or rhenium
- B01J23/8892—Manganese
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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
- B01J23/002—Mixed oxides other than spinels, e.g. perovskite
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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
- B01J2523/00—Constitutive chemical elements of heterogeneous catalysts
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Abstract
The present invention relates to chemical catalyst and technology of preparing thereof, it is desirable to provide for the quaternary compound oxide type catalyst and preparation method thereof of the VOCs that degrades.This catalyst is the Cu Mn Ce Zr cordierite metal composite oxide type integral catalyzer prepared by load method；The load capacity of the active component of this catalyst is 5% 25%, including: as the oxide of transition metal copper and the oxide of manganese of main active component, and as the oxide of rare-earth element cerium of auxiliary agent and the oxide of transition metal zirconium；Wherein, cordierite: the mass ratio of Cu: Mn: Ce: Zr is 100%: (0.5% 7%): (2% 15%): (0.5% 5%): (0.5% 5%).The catalyst that the present invention prepares can be degraded multiple VOCs, and activity is high, and initiation temperature is low；This catalyst is integral catalyzer, and mechanical strength is high, and the life-span is long.Owing to using transition metal, with low cost, prospects for commercial application is good.
Description
Technical field
The invention belongs to chemical catalyst and preparing technical field thereof, be specifically related to a kind of rare earth gold for the VOCs that degrades
Belong to transition metal based quaternary catalytic combustion catalyst of modification and preparation method thereof.
Background technology
In recent years, along with synthetic leather, automobile, the fast development of the color industry such as steel and motor vehicles manufacture, create a large amount of
VOCs (VOC).Water body, soil and air are not only polluted by VOCs, and owing to its discharge is to haze
Formation contribution rate is high, is detrimental to health, and causes and pays close attention to widely.By the Ministry of Finance, National Development and Reform Commission, Environmental Protection Department
Combine " volatile organic matter Pollution Charges Site way " execution from 1 day October in 2015, the China pair formulating and printing and distributing
The emission control of VOCs is very urgent.
At present, the precious metal catalyst combustion catalyst commonly used in the Production by Catalytic Combustion Process of conventional processs VOCs have Pt, Pd,
Au, Rh etc..Patent CN102513130A discloses a kind of integral combustion catalyst for platinum-based honeycomb iron-chrome-aluminiuwire wire mesh, about
Under the lower temperature of 180 DEG C, toluene conversion can be made to reach more than 90%.But its preparation process need to use PdCl2Process
Iron-chrome-aluminium wire mesh, adds the cost of this noble metal catalyst.For reducing cost, and overcome asking of noble metal catalyst easy-sintering
Topic, transition metal based catalysts is gradually widely studied.
The present invention is prepared for that a kind of low cost for the VOCs that degrades, high activity, initiation temperature be low, the rare earth gold of life-span length
Belong to the transition metal base Cu-Mn-Ce-Zr compound oxide type catalyst for catalytic combustion modified.
Summary of the invention
The technical problem to be solved in the present invention is, overcomes deficiency of the prior art, it is provided that a kind of for degrading VOCs's
Quaternary compound oxide type catalyst and preparation method thereof.
For solving technical problem, the solution of the present invention is:
Thering is provided a kind of quaternary compound oxide type catalyst for the VOCs that degrades, this catalyst is to be prepared by load method
Cu-Mn-Ce-Zr-cordierite metal composite oxide type integral catalyzer；The load capacity of the active component of this catalyst is
5%-25%, including: as the oxide of transition metal copper and the oxide of manganese of main active component, and as auxiliary agent
The oxide of rare-earth element cerium and the oxide of transition metal zirconium；Wherein, cordierite: the mass ratio of Cu: Mn: Ce: Zr is 100%
: (0.5%-7%): (2%-15%): (0.5%-5%): (0.5%-5%).
The invention further provides for the preparation method of the quaternary compound oxide type catalyst of degraded VOCs, including
Following steps:
(1) according to cordierite: the mass ratio of Cu: Mn: Ce: Zr is (0.5%-7%): (2%-15%): (0.5%-5%)
: (0.5%-5%), weigh the mantoquita of solubility, zirconates, cerium salt and manganese salt, add in deionized water, stirring and dissolving；
(2) take viscosifier and join in solution, obtain homogeneous viscous solution, be dried after being evenly applied on cordierite；
(3) at 300-750 DEG C, calcine 2-10h, prepare Cu-Mn-Ce-Zr-cordierite metal composite oxide type overall
Formula catalyst.
In the present invention, described mantoquita is one or more in copper sulfate, Schweinfurt green, copper nitrate or copper chloride；Described manganese
Salt is one or more in manganese acetate, manganese chloride, manganese sulfate or manganese nitrate；Described cerium salt is cerous sulfate, cerous nitrate, tri-chlorination
One or more in cerium, Cericammoniumsulfate or ammonium ceric nitrate；Described zirconates is zirconium oxychloride, zirconyl nitrate, zirconium nitrate or acetic acid
One or more in zirconium；Described viscosifier are one or more in carboxymethyl cellulose, carboxyethyl cellulose or acrylic acid.
In the present invention, in step (2), control mantoquita, zirconates, cerium salt and manganese salt addition, make copper in catalyst, zirconium,
The load capacity of the oxide of cerium and manganese is 5%-25%.
In the present invention, the consumption of described viscosifier is 0.02-0.1g/mL.
Compared with prior art, the invention have the advantage that
(1) catalyst that the present invention prepares can be degraded multiple VOCs, and activity is high, and initiation temperature is low；
(2) this catalyst is integral catalyzer, and mechanical strength is high, and the life-span is long.
(3) owing to using transition metal, with low cost, prospects for commercial application is good.
Accompanying drawing explanation
Fig. 1 is the preparation flow figure of catalyst.
Fig. 2 is that the catalyst SEM of embodiment 1 characterizes collection of illustrative plates.
Fig. 3 is the catalyst multiple VOCs degrading activity evaluation figure of embodiment 1-6.
Fig. 4 is the catalyst toluene life-span design sketch of embodiment 1.
Detailed description of the invention
Below in conjunction with the accompanying drawings with embodiment come the present invention is described in more detail, wherein part preparation condition only as
The explanation of typical case, is not limited to the present invention.
Embodiment 1:
(1) Cu (NO of 4.26g is weighed3)2·3H2Ce (the NO of O, 1.49g3)3·6H2Zr (the NO of O, 2.26g3)4·
5H2O, measures the Mn (NO of 11.47g3)2Solution (mass fraction is 50%), joins in 50mL deionized water, stirring and dissolving；
(2) take 1g acrylic acid and join gained solution in (1), obtain homogeneous viscous solution；
(3) gained viscous solution in (2) is evenly applied on cordierite, and is dried；
(4) gained cordierite carrier in (3) is calcined 3h at 700 DEG C, prepare Cu-Mn-Ce-Zr-cordierite composite oxygen
Compound type monoblock type catalyst for catalytic combustion.
After measured, the load capacity of prepared integral catalyzer is 25%.Wherein, Cu accounts for the 7% of cordierite quality, Mn
Accounting for the 11% of cordierite quality, Ce accounts for the 3% of cordierite quality, and Zr accounts for the 3% of cordierite quality.
The catalysis activity of catalyst, GHSV (volume space velocity: pass through unit in the unit interval is evaluated in tube furnace reactor
The gas flow of volume of catalyst bed)=30000h-1.Reactant concentration is that (wherein toluene vapor is by pure for toluene=1000ppm
Toluene solution bubbling produces, and is controlled its concentration by mass flow controller), reaction end gas utilizes gas chromatograph to carry out online
Analyze.Result shows, reaction temperature is 170 DEG C, 190 DEG C, 210 DEG C, 230 DEG C, 250 DEG C, 270 DEG C, 290 DEG C, 310 DEG C and 330
DEG C time, the degradation rate of toluene is respectively 3.5%, 8.6%, 38.0%, 86.0%, 99.2%, 99.8%, 99.9%, 99.9%
With 99.9%.
Embodiment 2:
(1) Cu (CH of 2.01g is weighed3COO)2·H2The Ce of O, 0.65g2(SO4)3·8H2Zr (the CH of O, 0.92g3COO)4
Mn (CH with 17.13g3COO)2·4H2O, joins in 50mL deionized water, stirring and dissolving；
(2) take 2g acrylic acid and join gained solution in (1), obtain homogeneous viscous solution；
(3) gained viscous solution in (2) is evenly applied on cordierite, and is dried；
(4) gained cordierite carrier in (3) is calcined 10h at 300 DEG C, prepare Cu-Mn-Ce-Zr-cordierite composite oxygen
Compound type monoblock type catalyst for catalytic combustion.
After measured, the load capacity of prepared integral catalyzer is 20%.Wherein, Cu accounts for the 2.5% of cordierite quality,
Mn accounts for the 15% of cordierite quality, and Ce accounts for the 1% of cordierite quality, and Zr accounts for the 1% of cordierite quality.
The catalysis activity of catalyst, GHSV=30000h is evaluated in tube furnace reactor-1.Reactant concentration is acetic acid second
Ester=1000ppm (wherein ethyl acetate steam is produced by pure ethyl acetate solution bubbling, and by mass flow controller control
Its concentration), reaction end gas utilizes gas chromatograph to carry out on-line analysis.Result shows, reaction temperature is 170 DEG C, 190 DEG C, 210
DEG C, 230 DEG C, 250 DEG C, 270 DEG C, 290 DEG C, 310 DEG C and when 330 DEG C, the degradation rate of ethyl acetate is respectively 11.0%,
20.8%, 79.2%, 92.7%, 95.8%, 96.4%, 97.7%, 98.4% and 99.4%.
Embodiment 3:
(1) CuSO of 4.19g is weighed4·5H22 (the NH of O, 5.09g4)2SO4·Ce(SO4)2·4H2The ZrO of O, 4.51g
(NO3)2MnSO with 4.89g4, join in 50mL deionized water, stirring and dissolving；
(2) take 3g hydroxymethyl cellulose and join gained solution in (1), obtain homogeneous viscous solution；
(3) gained viscous solution in (2) is evenly applied on cordierite, and is dried；
(4) gained cordierite carrier in (3) is calcined 5h at 500 DEG C, prepare Cu-Mn-Ce-Zr-cordierite composite oxygen
Compound type monoblock type catalyst for catalytic combustion.
After measured, the load capacity of prepared integral catalyzer is 17%.Wherein, Cu accounts for the 3% of cordierite quality, Mn
Accounting for the 5% of cordierite quality, Ce accounts for the 3% of cordierite quality, and Zr accounts for the 5% of cordierite quality.
The catalysis activity of catalyst, GHSV=30000h is evaluated in tube furnace reactor-1.Reactant concentration is normal hexane
(wherein normal hexane steam is produced=1000ppm by pure hexane solution bubbling, and it is dense to be controlled it by mass flow controller
Degree), reaction end gas utilizes gas chromatograph to carry out on-line analysis.Result shows, reaction temperature is 170 DEG C, 190 DEG C, 210 DEG C,
When 230 DEG C, 250 DEG C, 270 DEG C, 290 DEG C, 310 DEG C and 330 DEG C, the degradation rate of normal hexane is respectively 10.6%, 13.4%,
18.1%, 34.6%, 92.5%, 96.2%, 96.6%, 98.0% and 99.1%.
Embodiment 4:
(1) CuCl of 5.84g is weighed2·2H2The CeCl of O, 2.04g3·7H2The ZrOCl of O, 2.71g2·8H2O and 9.22g
MnCl2·4H2O, joins in 50mL deionized water, stirring and dissolving；
(2) take 5g hydroxyethyl cellulose and join gained solution in (1), obtain homogeneous viscous solution；
(3) gained viscous solution in (2) is evenly applied on cordierite, and is dried；
(4) gained cordierite carrier in (3) is calcined 8h at 400 DEG C, prepare Cu-Mn-Ce-Zr-cordierite composite oxygen
Compound type monoblock type catalyst for catalytic combustion.
After measured, the load capacity of prepared integral catalyzer is 5%.Wherein, Cu accounts for the 1.7% of cordierite quality,
Mn accounts for the 2% of cordierite quality, and Ce accounts for the 0.6% of cordierite quality, and Zr accounts for the 0.6% of cordierite quality.
The catalysis activity of catalyst, GHSV=30000h is evaluated in tube furnace reactor-1.Reactant concentration be toluene=
1000ppm, reaction end gas utilizes gas chromatograph to carry out on-line analysis.Result shows, reaction temperature is 170 DEG C, 190 DEG C, 210
DEG C, 230 DEG C, 250 DEG C, 270 DEG C, 290 DEG C, 310 DEG C and when 330 DEG C, the degradation rate of toluene is respectively 3.5%, 4.4%,
7.7%, 51.8%, 90.1%, 98.3%, 99.2%, 99.5% and 99.7%.
Embodiment 5:
(1) Cu (NO of 2.70g is weighed3)2·3H2(the NH of O, 6.96g4)2Ce(NO3)6, the Zr (NO of 0.84g3)4·5H2O
MnCl with 8.97g2·4H2O, joins in 50mL deionized water, stirring and dissolving in the lump；
(2) take 1.5g hydroxyethyl cellulose and join gained solution in (1), obtain homogeneous viscous solution；
(3) gained viscous solution in (2) is evenly applied on cordierite, and is dried；
(4) gained cordierite carrier in (3) is calcined 4h at 600 DEG C, prepare Cu-Mn-Ce-Zr-cordierite composite oxygen
Compound type monoblock type catalyst for catalytic combustion.
After measured, the load capacity of prepared integral catalyzer is 15%.Wherein, Cu accounts for the 2% of cordierite quality, Mn
Accounting for the 7% of cordierite quality, Ce accounts for the 5% of cordierite quality, and Zr accounts for the 0.5% of cordierite quality.
The catalysis activity of catalyst, GHSV=30000h is evaluated in tube furnace reactor-1.Reactant concentration be toluene=
1000ppm, reaction end gas utilizes gas chromatograph to carry out on-line analysis.Result shows, reaction temperature is 170 DEG C, 190 DEG C, 210
DEG C, 230 DEG C, 250 DEG C, 270 DEG C, 290 DEG C, 310 DEG C and when 330 DEG C, the degradation rate of toluene is respectively 5.1%, 6.2%,
12.8%, 57.8%, 94.8%, 99.3%, 99.7%, 99.9% and 99.9%.
Embodiment 6:
(1) CuSO of 1.26g is weighed4·5H2Ce (the NO of O, 0.99g3)3·6H2Zr (the NO of O, 7.53g3)4·5H2O and
10.55g MnSO4, join in 50mL deionized water, stirring and dissolving；
(2) take 4g carboxymethyl cellulose and join gained solution in (1), obtain homogeneous viscous solution；
(3) gained viscous solution in (2) is evenly applied on cordierite, and is dried；
(4) gained cordierite carrier in (3) is calcined 2h at 750 DEG C, prepare Cu-Mn-Ce-Zr-cordierite composite oxygen
Compound type monoblock type catalyst for catalytic combustion.
After measured, the load capacity of prepared integral catalyzer is 10%.Wherein, Cu accounts for the 0.5% of cordierite quality,
Mn accounts for the 6% of cordierite quality, and Ce accounts for the 0.5% of cordierite quality, and Zr accounts for the 2.5% of cordierite quality.
The catalysis activity of catalyst, GHSV=30000h is evaluated in tube furnace reactor-1.Reactant concentration be toluene=
1000ppm, reaction end gas utilizes gas chromatograph to carry out on-line analysis.Result shows, reaction temperature is 170 DEG C, 190 DEG C, 210
DEG C, 230 DEG C, 250 DEG C, 270 DEG C, 290 DEG C, 310 DEG C and when 330 DEG C, the degradation rate of toluene is respectively 3.1%, 3.4%,
10.9%, 51.2%, 95.0%, 98.9%, 99.6%, 99.9% and 99.9%.
Claims (5)
1. the quaternary compound oxide type catalyst for the VOCs that degrades, it is characterised in that this catalyst is by load
Cu-Mn-Ce-Zr-cordierite metal composite oxide type integral catalyzer prepared by method；Bearing of the active component of this catalyst
Carrying capacity is 5%-25%, including: as the oxide of transition metal copper and the oxide of manganese of main active component, and conduct
The oxide of the rare-earth element cerium of auxiliary agent and the oxide of transition metal zirconium；Wherein, cordierite: the mass ratio of Cu: Mn: Ce: Zr
It is 100%: (0.5%-7%): (2%-15%): (0.5%-5%): (0.5%-5%).
2. the preparation method for the quaternary compound oxide type catalyst of the VOCs that degrades, it is characterised in that include following
Step:
(1) it is (0.5%-7%) according to the mass ratio of Cu: Mn: Ce: Zr: (2%-15%): (0.5%-5%): (0.5%-
5%), weigh the mantoquita of solubility, zirconates, cerium salt and manganese salt, add in deionized water, stirring and dissolving；
(2) take viscosifier and join in solution, obtain homogeneous viscous solution, be dried after being evenly applied on cordierite；
(3) at 300-750 DEG C, calcine 2-10h, prepare Cu-Mn-Ce-Zr-cordierite metal composite oxide type monoblock type and urge
Agent.
Method the most according to claim 2, it is characterised in that described mantoquita is copper sulfate, Schweinfurt green, copper nitrate or chlorination
One or more in copper；Described manganese salt is one or more in manganese acetate, manganese chloride, manganese sulfate or manganese nitrate；Described cerium
Salt is one or more in cerous sulfate, cerous nitrate, cerous chloride, Cericammoniumsulfate or ammonium ceric nitrate；Described zirconates is oxychlorination
One or more in zirconium, zirconyl nitrate, zirconium nitrate or acetic acid zirconium；Described viscosifier are carboxymethyl cellulose, carboxyethylcellulose
One or more in element or acrylic acid.
Method the most according to claim 2, it is characterised in that in step (2), controls mantoquita, zirconates, cerium salt and manganese salt
Addition, the load capacity making the oxide of copper in catalyst, zirconium, cerium and manganese is 5%-25%.
Method the most according to claim 2, it is characterised in that the consumption of described viscosifier is 0.02-0.1g/mL.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106693955A (en) * | 2016-12-22 | 2017-05-24 | 北京工业大学 | Double-metal integral type plasma catalyst as well as preparation method and application of double-metal integral type plasma catalyst |
| CN107754809A (en) * | 2017-10-23 | 2018-03-06 | 浙江工商大学 | The Cu Mn Zr composite catalysts and preparation method of degraded VOCs waste gas |
| CN108176397A (en) * | 2017-12-28 | 2018-06-19 | 大唐南京环保科技有限责任公司 | A kind of VOCs catalyst for catalytic combustion with anti-sulfur poisonous performance and preparation method thereof |
| CN110833833A (en) * | 2019-11-14 | 2020-02-25 | 西安凯立新材料股份有限公司 | Non-noble metal composite oxide honeycomb catalyst for catalytic combustion of low-carbon hydrocarbons |
| CN112588296A (en) * | 2020-12-23 | 2021-04-02 | 甄崇礼 | Catalyst for VOCs catalytic combustion and preparation method thereof |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106693955A (en) * | 2016-12-22 | 2017-05-24 | 北京工业大学 | Double-metal integral type plasma catalyst as well as preparation method and application of double-metal integral type plasma catalyst |
| CN107754809A (en) * | 2017-10-23 | 2018-03-06 | 浙江工商大学 | The Cu Mn Zr composite catalysts and preparation method of degraded VOCs waste gas |
| CN107754809B (en) * | 2017-10-23 | 2020-04-21 | 浙江工商大学 | Cu-Mn-Zr composite catalyst for degrading VOCs waste gas and preparation method thereof |
| CN108176397A (en) * | 2017-12-28 | 2018-06-19 | 大唐南京环保科技有限责任公司 | A kind of VOCs catalyst for catalytic combustion with anti-sulfur poisonous performance and preparation method thereof |
| CN110833833A (en) * | 2019-11-14 | 2020-02-25 | 西安凯立新材料股份有限公司 | Non-noble metal composite oxide honeycomb catalyst for catalytic combustion of low-carbon hydrocarbons |
| CN112588296A (en) * | 2020-12-23 | 2021-04-02 | 甄崇礼 | Catalyst for VOCs catalytic combustion and preparation method thereof |
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