CN101703932B - Method for preparing Pd and Pt loaded mesoporous manganese oxide for catalytically eliminating VOCs - Google Patents
Method for preparing Pd and Pt loaded mesoporous manganese oxide for catalytically eliminating VOCs Download PDFInfo
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- CN101703932B CN101703932B CN2009102362773A CN200910236277A CN101703932B CN 101703932 B CN101703932 B CN 101703932B CN 2009102362773 A CN2009102362773 A CN 2009102362773A CN 200910236277 A CN200910236277 A CN 200910236277A CN 101703932 B CN101703932 B CN 101703932B
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Abstract
The invention relates to a method for preparing Pd and Pt loaded mesoporous manganese oxide for catalytically eliminating VOCs, which belongs to the field of catalysts. The invention provides a method for preparing a mesoporous manganese oxide carrier and a method for preparing a catalyst of noble metals Pt and Pd loaded thereby, which are used for catalytically eliminating VOCs gas at a low temperature. The mesoporous manganese oxide carrier is prepared by a sol-gel method and the noble metals Pt and Pd are loaded by an improved wet dipping method. The prepared catalyst has a high catalytic combustion activity for benzene and CO at the lower temperature. The method has the advantages of low power consumption, simple operation, mild reaction condition, capacity of reducing secondary pollution and continuously working, and the like.
Description
Technical field
The present invention relates to the preparation of the simple mesoporous manganese oxide carrier of a kind of cheapness, and carried noble metal Pt and Pd Preparation of catalysts method, and be used for low-temperature catalyzed elimination VOCs gas.
Background technology
Mesopore oxide material is the modal mesoporous material of a class, also is a most widely used class material.Mesopore oxide material is through years of researches, characteristics that it is unique and superior performance are understood by people gradually, its application has been not limited only to fields such as traditional catalysis, absorption, but becomes the multifunctional material of crossing over light, electricity, magnetic, nanometer engineering, bioengineering, medicine and other fields.
Volatile organic matter (Volatile organic compounds (VOCs)) is the major pollutants of urban atmosphere, is mainly derived from motor vehicle exhaust emission, industrial production and energy use.VOCs is poisonous mostly, can induce an illness with carcinogenic, even teratogenesis.VOCs pollutes one of the five big factors that are detrimental to health that have been listed in the world.Formation based on the photochemical fog of ozone mainly is by the leading chemical reaction process of VOCs.Therefore, the key issue that control and the improvement of atmosphere VOCs is environmental protection.
Benzene is the material of difficult conversion in all VOCs gases, and is being indoor and outdoor one of the widest material that distributes, and therefore, the present invention is that the catalysis that probe is studied VOCs is eliminated with benzene.It is less research to be eliminated in the catalysis of benzene both at home and abroad at present, and the reaction temperature that benzene is eliminated in complete catalysis is higher.For example: " The effect of mass transfer on the catalyticcombustion of benzene and methane over palladium catalysts supported on porousmaterials " (Catal.Today that the research of Korea S Gon SeoO seminar is delivered, 83 (2003) 131-139) in the paper, in air speed is 60,000h-1, the concentration of benzene is 10, (air speed is lower than of the present invention 80 during 000ppm, 000h-1, benzene concentration is higher than 1000ppm of the present invention), use the FAU zeolite, MCM-41 and KIT-1 Pt-supported catalyst carry out catalyst combustion reaction to benzene, and its complete catalysis is eliminated the temperature of benzene mostly more than 300 ℃.
This project implementation obtain state natural sciences fund (numbering: 20777005), Beijing's natural science fund (numbering: 8082008) and the outstanding personnel of Beijing organization department fund (number: the 20071D0501500210) subsidy of project funds is the research contents of these projects.
Summary of the invention
The preparation method who the purpose of this invention is to provide the low-temperature catalyzed elimination of Pd and Pt loaded mesoporous manganese oxide VOCs gas.
Catalyst of the present invention, and under high-speed (80,000h
-1), low concentration benzene (1000ppm) is had higher low-temperature catalyzed elimination activity: 1) Pt loaded mesoporous manganese oxide catalyst is completely oxidized to CO with benzene in the time of 190～200 ℃
2And H
2O is completely oxidized to CO with CO in the time of 80～90 ℃
22) Pd loaded mesoporous manganese oxide catalyst is completely oxidized to CO at 290 ℃ with benzene
2And H
2O is completely oxidized to CO with CO in the time of 57-70 ℃
2
The preparation of mesoporous manganese oxide provided by the invention is to be used for catalyst carrier, and Pt and Pd make by load carriers.With maleic acid and potassium permanganate is raw material, uses sol-gel (sol-gel) legal system to be equipped with the mesoporous manganese oxide carrier, wet infusion process supporting Pt, Pd catalyst.Concrete preparation is achieved through the following technical solutions:
Above-mentioned Preparation of catalysts method provided by the present invention comprises the steps:
(1) preparation of mesoporous manganese oxide
With mol ratio 1～4: 1 KMnO
4With the maleic acid wiring solution-forming, adding KOH adjusting pH is 7～10, and temperature remains on 30 ℃～60 ℃, stirs after 10～30 minutes, leaves standstill 15～30 hours.Outwell supernatant, suction filtration, ethanol washing at room temperature, the dark brown gelinite that obtains vacuumizes this gelinite dry 15～24 hours at 80 ℃～120 ℃ then, gets black solid.With ethanolic solution this solid was soaked 15～24 hours, suction filtration, distilled water washing vacuumize drying at 80 ℃～120 ℃, obtain the black powdery solid.In the air stream of 20～40ml/min, 200 ℃～400 ℃ roastings of powdery solid were obtained mesoporous manganese oxide in 2～5 hours.
(2) preparation of wet infusion process Pd and Pt loaded mesoporous manganese oxide
Get above-mentioned mesoporous manganese oxide and add the 0.1～0.4M Pd (NO that configures
3)
2In the solution, form suspension, wherein Mn: the mol ratio of Pd element is 15～40: 1, and in above-mentioned suspension, adding nitric acid adjusting pH is 6～9, and stirring at room 10～24 hours adds 0.2～0.7M NaBH then
4Solution continues to stir 4～7 hours, and ultrasonic wave was handled 15～30 minutes.Above-mentioned solution room temperature backspin is changeed evaporation got black solid in 8～16 hours.This solid washs several times with distilled water and ethanol respectively, then 80～120 ℃ of vacuum drying 18～24 hours, promptly makes the catalyst of Pd loaded mesoporous manganese oxide after the drying.
Get above-mentioned mesoporous manganese oxide and add the 0.1～0.5M H that configures
2PtCl
6In the solution, form suspension, wherein Mn: the mol ratio of Pt element is 15～40: 1, and in above-mentioned suspension, adding nitric acid adjusting pH is 6～9, and stirring at room 10～24 hours adds 0.2～0.7M NaBH then
4Solution continues to stir 4～7 hours, and ultrasonic wave was handled 15～30 minutes.Above-mentioned solution room temperature backspin is changeed evaporation got black solid in 8～16 hours.This solid washs respectively several times with distilled water and acetone, uses AgNO
3Solution detects no Cl
-Ion gets final product.In 80～120 ℃ of vacuum 18～24 hours, promptly make the catalyst of Pt loaded mesoporous manganese oxide after the drying.
The present invention does not need additional any fuel, directly utilizes O in the air
2Be oxidant, energy consumption is low, easy and simple to handle, reaction condition is gentle, can reduce advantages such as secondary pollution and continuous operation but have.
Description of drawings
Fig. 1 is the XRD figure of the Pd loaded mesoporous manganese oxide catalyst of the embodiment of the invention 1 and 2 preparations
Fig. 2 is the XRD figure of the Pt loaded mesoporous manganese oxide catalyst of the embodiment of the invention 3 and 4 preparations
Fig. 3 is the Pd of the embodiment of the invention 1 to 4 preparation and the N of Pt loaded mesoporous manganese oxide catalyst
2Absorption/desorption isothermal curve figure
Fig. 4 is the Pd of the embodiment of the invention 1 to 4 preparation and the graph of pore diameter distribution of Pt loaded mesoporous manganese oxide catalyst
Fig. 5 is the Pd of the embodiment of the invention 1 to 4 preparation and the benzene catalytic oxidation curve map of Pt loaded mesoporous manganese oxide catalyst
Fig. 6 is the Pd of the embodiment of the invention 1 to 4 preparation and the CO catalytic oxidation curve map of Pt loaded mesoporous manganese oxide catalyst
The specific embodiment
Used potassium permanganate, maleic acid, sodium borohydride, the NaOH of preparation catalyst is that the Beijing Chemical Plant produces, and analyzes pure.Pd (NO
3)
22H
2O and H
2PtCl
66H
2O is that Shanghai new peak chemical reagent Co., Ltd produces, and analyzes pure.
The present invention will be further described by embodiment below:
(1) with mol ratio is 1: 1 KMnO
4With the maleic acid wiring solution-forming, adding KOH adjusting pH is 7, and temperature remains on 30 ℃, stirs after 10 minutes, leaves standstill 15 hours.Outwell supernatant, suction filtration, ethanol washing at room temperature, the dark brown gelinite that obtains vacuumizes this gelinite dry 15 hours at 80 ℃ then, gets black solid.With ethanolic solution this solid was soaked 15 hours, suction filtration, distilled water washing vacuumize drying at 80 ℃, obtain the black powdery solid.In the air stream of 20ml/min, 200 ℃ of roastings of powdery solid were obtained mesoporous manganese oxide in 2 hours.
Get above-mentioned mesoporous manganese oxide and put into the H that configures
2PtCl
6(press Mn: Pt mol ratio 40: 1), suspension was stirring at room 10 hours, and it is 6 that nitric acid is regulated pH, adds 0.2M NaBH then in the solution
4Solution continues to stir 10 hours; Ultrasonic wave was handled 15 minutes, above-mentioned solution room temperature backspin is changeed evaporation got black solid in 8 hours.This solid washs respectively several times with distilled water and acetone, up to using AgNO
3Solution detects no Cl
-Ion 80 ℃ of vacuum drying 18 hours, promptly makes the catalyst of Pt loaded mesoporous manganese oxide.
(2) catalyst activity evaluation.The concentration of benzene is 1000ppm, and air speed is 80,000h
-1Gas-chromatography TCD detection reaction tail gas CO
2And CO, FID detects the content of benzene and other organic species.The temperature that benzene is eliminated in the complete catalysis of the embodiment of the invention 1 obtained catalyst is 190 ℃, when temperature in 150 ℃～190 ℃ scope, benzene conversion ratio straight line raises until reaching 100%, eliminates in the reaction in the catalysis of benzene, benzene changes into CO fully
2And H
2O; CO 50% changes into CO
2Temperature be 60 ℃, CO changes into CO fully
2Temperature be 80 ℃.
Embodiment 2
(1) with mol ratio is 4: 1 KMnO
4With the maleic acid wiring solution-forming, adding KOH adjusting pH is 10, and temperature remains on 60 ℃, stirs after 30 minutes, leaves standstill 30 hours.Outwell supernatant, suction filtration, ethanol washing at room temperature, the dark brown gelinite that obtains vacuumizes this gelinite dry 24 hours at 120 ℃ then, gets black solid.With ethanolic solution this solid was soaked 24 hours, suction filtration, distilled water washing vacuumize drying at 120 ℃, obtain the black powdery solid.In the air stream of 40ml/min, 400 ℃ of roastings of powdery solid were obtained mesoporous manganese oxide in 5 hours.
Get above-mentioned mesoporous manganese oxide and put into the H that configures
2PtCl
6(press Mn: Pt mol ratio 15: 1), suspension was stirring at room 24 hours, and it is 9 that nitric acid is regulated pH, adds 0.7M NaBH then in the solution
4Solution continues to stir 7 hours; Ultrasonic wave was handled 30 minutes, above-mentioned solution room temperature backspin is changeed evaporation got black solid in 16 hours.This solid washs respectively several times with distilled water and acetone, up to using AgNO
3Solution detects no Cl
-Ion 120 ℃ of vacuum drying 24 hours, promptly makes the catalyst of Pt loaded mesoporous manganese oxide.
(2) catalyst activity evaluation.The concentration of benzene is 1000ppm, and air speed is 80,000h
-1Gas-chromatography TCD detection reaction tail gas CO
2And CO, FID detects the content of benzene and other organic species.The temperature that benzene is eliminated in the complete catalysis of the embodiment of the invention 2 obtained catalyst is 200 ℃, when temperature in 150 ℃～200 ℃ scope, benzene conversion ratio straight line raises until reaching 100%, eliminates in the reaction in the catalysis of benzene, benzene changes into CO fully
2And H
2O; CO 50% changes into CO
2Temperature be 63 ℃, CO changes into CO fully
2Temperature be 90 ℃.
Embodiment 3
(1) with mol ratio is 1: 1 KMnO
4With the maleic acid wiring solution-forming, adding KOH adjusting pH is 7, and temperature remains on 30 ℃, stirs after 10 minutes, leaves standstill 15 hours.Outwell supernatant, suction filtration, ethanol washing at room temperature, the dark brown gelinite that obtains vacuumizes this gelinite dry 15 hours at 80 ℃ then, gets black solid.With ethanolic solution this solid was soaked 15 hours, suction filtration, distilled water washing vacuumize drying at 80 ℃, obtain the black powdery solid.In the air stream of 20ml/min, 200 ℃ of roastings of powdery solid were obtained mesoporous manganese oxide in 2 hours.
Get above-mentioned mesoporous manganese oxide and put into the Pd (NO that configures
3)
2(press Mn: Pd mol ratio 40: 1), suspension was stirring at room 10 hours, and it is 6 that nitric acid is regulated pH, adds 0.2M NaBH then in the solution
4Solution continues to stir 4 hours, and ultrasonic wave was handled 15 minutes.Above-mentioned solution room temperature backspin is changeed evaporation got black solid in 8 hours.This solid washs several times with distilled water and ethanol respectively, then 80 ℃ of vacuum drying 18 hours, promptly makes the catalyst of Pd loaded mesoporous manganese oxide after the drying.
(2) catalyst activity evaluation.The concentration of benzene is 1000ppm, and air speed is 80,000h
-1Gas-chromatography TCD detection reaction tail gas CO
2And CO, FID detects the content of benzene and other organic species.The temperature that the embodiment of the invention 3 obtained catalysts are eliminated 50% benzene is 216 ℃, and the temperature of catalysis elimination benzene is 290 ℃ fully, eliminates in the reaction in the catalysis of benzene, and benzene changes into CO fully
2And H
2O; CO50% changes into CO
2Temperature is 25 ℃ of room temperatures, and CO changes into CO fully
2Temperature be 57 ℃.
Embodiment 4
(1) with mol ratio is 4: 1 KMnO
4With the maleic acid wiring solution-forming, adding KOH adjusting pH is 10, and temperature remains on 60 ℃, stirs after 30 minutes, leaves standstill 30 hours.Outwell supernatant, suction filtration, ethanol washing at room temperature, the dark brown gelinite that obtains vacuumizes this gelinite dry 24 hours at 120 ℃ then, gets black solid.With ethanolic solution this solid was soaked 24 hours, suction filtration, distilled water washing vacuumize drying at 120 ℃, obtain the black powdery solid.In the air stream of 40ml/min, 400 ℃ of roastings of powdery solid were obtained mesoporous manganese oxide in 5 hours.
Get above-mentioned mesoporous manganese oxide and put into the Pd (NO that configures
3)
2(press Mn: Pd mol ratio 15: 1), suspension was stirring at room 24 hours, and it is 9 that nitric acid is regulated pH, adds 0.7M NaBH then in the solution
4Solution continues to stir 7 hours, and ultrasonic wave was handled 30 minutes.Above-mentioned solution room temperature backspin is changeed evaporation got black solid in 16 hours.This solid washs several times with distilled water and ethanol respectively, then 120 ℃ of vacuum drying 24 hours, promptly makes the catalyst of Pd loaded mesoporous manganese oxide after the drying.
(2) catalyst activity evaluation.The concentration of benzene is 1000ppm, and air speed is 80,000h
-1Gas-chromatography TCD detection reaction tail gas CO
2And CO, FID detects the content of benzene and other organic species.The temperature that the embodiment of the invention 4 obtained catalysts are eliminated 50% benzene is 245 ℃, and the temperature of catalysis elimination benzene is 290 ℃ fully, eliminates in the reaction in the catalysis of benzene, and benzene changes into CO fully
2And H
2O; CO50% changes into CO
2Temperature is 35 ℃ of room temperatures, and CO changes into CO fully
2Temperature be 70 ℃.
Claims (1)
1. be used for the preparation method of the Pd and the Pt loaded mesoporous manganese oxide of catalysis of removing VOCs, it is characterized in that preparation process is:
(1) preparation of mesoporous manganese oxide
With mol ratio 1～4: 1 KMnO
4With the maleic acid wiring solution-forming, adding KOH adjusting pH is 7～10, and temperature remains on 30 ℃～60 ℃, stirs after 10～30 minutes, leaves standstill 15～30 hours; Outwell supernatant, suction filtration, ethanol washing at room temperature, the dark brown gelinite that obtains vacuumizes this gelinite dry 15～24 hours at 80 ℃～120 ℃ then, gets black solid; With ethanolic solution this solid was soaked 15～24 hours, suction filtration, distilled water washing vacuumize drying at 80 ℃～120 ℃, obtain the black powdery solid; In the air stream of 20～40ml/min, 200 ℃～400 ℃ roastings of powdery solid were obtained mesoporous manganese oxide in 2～5 hours;
(2) preparation of wet infusion process Pd and Pt loaded mesoporous manganese oxide
Get above-mentioned mesoporous manganese oxide and add the 0.1～0.4M Pd (NO that configures
3)
2In the solution, form suspension, wherein Mn: the mol ratio of Pd element is 15～40: 1, in above-mentioned suspension, and stirring at room 10～24 hours, adding nitric acid adjusting pH is 6～9; Add 0.2～0.7M NaBH then
4Solution continues to stir 4～7 hours, and ultrasonic wave was handled 15～30 minutes; Above-mentioned solution room temperature backspin is changeed evaporation got black solid in 8～16 hours; This solid washs several times with distilled water and ethanol respectively, then 80～120 ℃ of vacuum drying 18～24 hours, promptly makes the catalyst of Pd loaded mesoporous manganese oxide after the drying;
Perhaps get above-mentioned mesoporous manganese oxide and add the 0.1～0.5M H that configures
2PtCl
6In the solution, form suspension, wherein Mn: the mol ratio of Pt element is 15～40: 1, in above-mentioned suspension, and stirring at room 10～24 hours, adding nitric acid adjusting pH is 6～9; Add 0.2～0.7M NaBH then
4Solution continues to stir 4～7 hours, and ultrasonic wave was handled 15～30 minutes; Above-mentioned solution room temperature backspin is changeed evaporation got black solid in 8～16 hours; This solid washs respectively several times with distilled water and acetone, uses AgNO
3Solution detects no Cl
-Ion gets final product; 80～120 ℃ of vacuum drying 18～24 hours, promptly make the catalyst of Pt loaded mesoporous manganese oxide after the drying.
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Families Citing this family (9)
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| CN101927179A (en) * | 2010-07-09 | 2010-12-29 | 北京工业大学 | OMS-2 catalyst used in elimination of benzene series at low temperature and preparation and application |
| CN101912784B (en) * | 2010-08-13 | 2012-08-29 | 北京工业大学 | Preparation method and application of mesoporous Co3O4/ Beta-MnO2 or NiO/ Beta-MnO2 catalysts |
| CN101905159B (en) * | 2010-08-13 | 2011-12-21 | 北京工业大学 | Preparation method and application of Au and Ag loaded mesoporous beta-MnO2 catalyst |
| CN104174411B (en) * | 2014-07-07 | 2016-06-29 | 中国科学院过程工程研究所 | A kind of method improving VOCs catalyst oxidation activity |
| CN107816730B (en) * | 2016-09-14 | 2019-03-26 | 中国石油化工股份有限公司 | A kind of device and method of catalysis burning removing VOC |
| CN109012659B (en) * | 2018-07-19 | 2022-04-29 | 天津大学 | Preparation method of noble metal-loaded activated carbon fiber monatomic catalyst for normal-temperature catalytic degradation of VOCs (volatile organic chemicals) |
| CN109569645B (en) * | 2018-12-23 | 2022-02-08 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation of cobalt-manganese composite oxide/carbon catalyst for propane treatment, product and application |
| CN111282579B (en) * | 2020-03-20 | 2023-01-20 | 北京工业大学 | Preparation method and application of neodymium-samarium-doped NiO/MgO compound supported platinum catalyst |
| CN112076760A (en) * | 2020-09-19 | 2020-12-15 | 河南省百艾堂科技有限公司 | Supported noble metal catalyst for moxa smoke purification treatment during moxibustion |
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| US6906208B2 (en) * | 1999-09-07 | 2005-06-14 | Abb Lummus Global Inc. | Mesoporous material and use thereof for the selective oxidation of organic compounds |
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