CN103191743A - Co-based supported catalyst for catalytic removal of benzene-series compounds in air and preparation method thereof - Google Patents

Co-based supported catalyst for catalytic removal of benzene-series compounds in air and preparation method thereof Download PDF

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CN103191743A
CN103191743A CN2013101373669A CN201310137366A CN103191743A CN 103191743 A CN103191743 A CN 103191743A CN 2013101373669 A CN2013101373669 A CN 2013101373669A CN 201310137366 A CN201310137366 A CN 201310137366A CN 103191743 A CN103191743 A CN 103191743A
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CN103191743B (en
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谢红梅
周桂林
赵聪
张海霞
何小玲
唐祖兰
宋如意
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Chongqing Technology and Business University
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Abstract

The invention discloses a Co-based supported catalyst for catalytic removal of benzene-series compounds in air and a preparation method thereof. The catalyst comprises an active component, namely Co3O4 and a carrier, namely activated carbon. The preparation method of the catalyst comprises the following steps of: 1) weighing a cobalt salt according to the amount of the Co3O4, fully dissolving in distilled water, further taking the activated carbon, soaking in an obtained cobalt salt solution, further distilling water to dryness, and performing drying treatment to prepare a dry material; and 2) roasting the dry material prepared in the step 1) in a Muffle furnace to prepare the catalyst. According to the catalyst disclosed by the invention, the activated carbon is taken as the carrier, and the oxide of non-precious metal cobalt, namely the Co3O4 is taken as the active component, so that the cost of the catalyst is greatly reduced; and furthermore, the catalyst disclosed by the invention shows good activity in catalyzing the combustion of the benzene-series compounds at a high reaction airspeed (66000mL.g<-1>-1.h<-1>) and within a low and narrow reaction temperature range.

Description

Being used for benzene in air is Co base supported catalyst of thing catalysis elimination and preparation method thereof
Technical field
The present invention relates to a kind of benzene series thing catalyst for catalytic combustion, being specifically related to a kind of is Co base supported catalyst of eliminating of thing catalysis and preparation method thereof for benzene in air.
Background technology
(Volatile Organic Compounds-VOCs) waste gas is to cause one of air-polluting main matter to volatile organic matter, even under lower concentration, can both cause serious harm to environment and the mankind, benzene series thing among these VOCs (as, benzene, benzene series thing, two benzene series things etc.) harm more outstanding.The benzene series owner will derive from industrial waste gas, the modal pollutant of industry discharging such as be iron and steel manufacturing, semiconductor components and devices production, petrochemical industry, pharmacy, printing, shoemaking, spray paint.Because the benzene series thing has volatile characteristics, how house decorative material replaces purified petroleum benzin as solvent or the diluent of materials such as various glue, paint, coating with benzene series thing, two benzene series things, and therefore, interior decoration also is important benzene series thing source.WHO is defined as strong carcinogen to benzene, and human body is had mutagenesis, teratogenesis and carcinogenic " three cause " harm, has caused the great attention of countries in the world.Processing method for the benzene series thing can be divided into two big classes usually: a class is that non-destructive technology is absorption method; One class is destructive technology, namely make the benzene series thing be converted into the inorganic matter that carbon dioxide, water and hydrogen chloride etc. are nontoxic or toxicity is little by chemistry or biological technology, these class methods comprise common technique such as direct burning, catalytic combustion, biodegradation, plasma oxidation, photocatalytic oxidation.Wherein, catalytic combustion can be handled the benzene series thing gas of low concentration under far below direct ignition temperature condition, has purification efficiency height, non-secondary pollution, characteristic of low energy consumption, is to handle the benzene series thing to use one of the most effective processing method.
At present, used benzene series thing catalyst for catalytic combustion mainly contains noble metal catalyst and catalyst of transition metal oxide.Noble metal catalyst mainly comprises and contains Pt, Pd, Ru and Au etc., because active high, selective good, long service life, high temperature resistant and have good advantages such as antitoxin performance has caused researcher's very big interest.Though noble metal catalyst has lot of advantages, limited the application of noble metal catalyst in the benzene series thing is eliminated owing to it is expensive.Therefore, cheap catalyst of transition metal oxide has caused people's extensive interest in recent years.For discovering of catalyst of transition metal oxide, composite oxide catalysts with spinelle and perovskite structure shows good benzene series thing catalytic combustion activity and stability, and have very big advantage on the price, and obtain easily, therefore have broad application prospects.But to the non-precious metal catalyst of studying, the subject matter of existence is the clearance still (＜90 %) on the low side of benzene series thing, 300 ℃ of reaction temperature height (〉), this has also limited, and non-precious metal catalyst is used for benzene in air is the application that thing catalysis is eliminated.Further carrying out non-precious metal catalyst is that thing catalysis is eliminated for benzene in air, develops the catalyst with high low temperature active atmospheric environment protection is had great importance.
Summary of the invention
In view of this, the invention provides a kind of is Co base supported catalyst of eliminating of thing catalysis and preparation method thereof for benzene in air, and this catalyst is with low cost and have a good low temperature benzene series thing catalytic combustion activity.
The invention discloses a kind of is the Co base supported catalyst that thing catalysis is eliminated for benzene in air, and this catalyst comprises active component Co 3O 4And carrier active carbon.
Further, in the described catalyst, Co 3O 4With the weight ratio of active carbon be 1 ~ 3:7 ~ 9.
Further, in the described catalyst, Co 3O 4With the weight ratio of active carbon be 2:8.
The invention also discloses above-mentioned is the preparation method of the Co base supported catalyst of thing catalysis elimination for benzene in air, may further comprise the steps:
1) presses Co 3O 4Amount take by weighing cobalt salt and fully being dissolved in the distilled water, get active carbon again and impregnated in the gained cobalt salt solution, evaporate to dryness moisture content and dry the processing make siccative again;
2) calcination steps 1 in Muffle furnace) siccative that makes makes described catalyst.
Further, in the described step 1), cobalt salt is cobalt nitrate, and active carbon is 20 ~ 80 purpose activated carbon granules, and active carbon impregnated in the cobalt nitrate solution, in 70 ℃ of evaporate to dryness moisture content, in 100 ℃ of following freeze-day with constant temperature 10 ~ 24 h, makes siccative again under the continuous stirring condition.
Further, described step 2) in, the concrete parameter of roasting is: siccative heating rate with 10 ℃/min in Muffle furnace is warming up to 300 ~ 400 ℃, then at 300 ~ 400 ℃ of following constant temperature calcining 2 ~ 4 h.
Further, described step 2) in, sintering temperature is 350 ℃.
Beneficial effect of the present invention is:
1) catalyst of the present invention is carrier with the active carbon, with the oxide Co of base metal cobalt 3O 4Be active component, reduced the catalyst cost significantly;
2) catalyst of the present invention is at high reaction velocity (66,000 mLg – 1H – 1), show good benzene series thing catalytic combustion activity in the low and wide range of reaction temperature; The toluene clearance can reach more than 99.7% in the time of 200 ℃, can effectively toluene concentration in the air be dropped to below 30 ppm, and the dimethylbenzene clearance can reach more than 98 % in the time of 250 ℃, can effectively xylene concentration in the air be dropped to below 200 ppm;
3) the present invention is carried on cobalt salt on the active carbon by wet infusion process, and then makes by high-temperature roasting and to contain Co 3O 4Catalyst, this method technology is simple, mild condition is easily controlled, good reproducibility.
Description of drawings
In order to make the purpose, technical solutions and advantages of the present invention clearer, the present invention is described in further detail below in conjunction with accompanying drawing, wherein:
Fig. 1 is the XRD spectra of the catalyst of embodiment 1 ~ 5;
Fig. 2 is the XRD spectra of embodiment 1,6,7 catalyst.
The specific embodiment
Hereinafter with reference to accompanying drawing, the preferred embodiments of the present invention are described in detail.
Embodiment 1
The catalyst of present embodiment comprises active component Co 3O 4And carrier active carbon, Co 3O 4With the weight ratio of active carbon be 2:8.
The Preparation of catalysts method of present embodiment may further comprise the steps:
1) presses Co 3O 4Amount take by weighing cobalt nitrate and fully be dissolved in the distilled water, getting 20 ~ 80 purpose activated carbon granules again impregnated in the gained cobalt nitrate solution, constantly under the stirring condition in 70 ℃ of evaporate to dryness moisture content, be to remove the crystallization water in the raw material in 100 ℃ of following freeze-day with constant temperature 24 h(in the purpose of 100 ℃ of freeze-day with constant temperature again, be that 10 ~ 24h all can realize goal of the invention drying time herein), make siccative;
2) siccative heating rate with 10 ℃/min in Muffle furnace of making of step 1) is warming up to 350 ℃, at 350 ℃ of following constant temperature calcining 2h, makes described catalyst then.
Embodiment 2
The catalyst of present embodiment comprises active component Co 3O 4And carrier active carbon, Co 3O 4With the weight ratio of active carbon be 1:9.
The Preparation of catalysts method of present embodiment is identical with embodiment 1.
Embodiment 3
The catalyst of present embodiment comprises active component Co 3O 4And carrier active carbon, Co 3O 4With the weight ratio of active carbon be 1.5:8.5.
The Preparation of catalysts method of present embodiment is identical with embodiment 1.
Embodiment 4
The catalyst of present embodiment comprises active component Co 3O 4And carrier active carbon, Co 3O 4With the weight ratio of active carbon be 2.5:7.5.
The Preparation of catalysts method of present embodiment is identical with embodiment 1.
Embodiment 5
The catalyst of present embodiment comprises active component Co 3O 4And carrier active carbon, Co 3O 4With the weight ratio of active carbon be 3:7.
The Preparation of catalysts method of present embodiment is identical with embodiment 1.
Embodiment 6
The catalyst of present embodiment comprises active component Co 3O 4And carrier active carbon, Co 3O 4With the weight ratio of active carbon be 2:8.
In the Preparation of catalysts method of present embodiment, except step 2) sintering temperature be 300 ℃, all the other conditions are identical with embodiment 1.
Embodiment 7
The catalyst of present embodiment comprises active component Co 3O 4And carrier active carbon, Co 3O 4With the weight ratio of active carbon be 2:8.
In the Preparation of catalysts method of present embodiment, except step 2) sintering temperature be 400 ℃, all the other conditions are identical with embodiment 1.
Comparative example 1
The catalyst of comparative example 1 comprises active component Co 3O 4With carrier mesopore SiO 2, Co 3O 4With SiO 2Weight ratio be 2:8.
The Preparation of catalysts method of comparative example 1 may further comprise the steps:
1) presses Co 3O 4Amount take by weighing cobalt nitrate and fully being dissolved in the distilled water, get mesopore SiO again 2Impregnated in the gained cobalt nitrate solution, in 70 ℃ of evaporate to dryness moisture content, in 100 ℃ of following freeze-day with constant temperature 24 h, make siccative again under the continuous stirring condition;
2) siccative heating rate with 10 ℃/min in Muffle furnace of making of step 1) is warming up to 350 ℃, at 350 ℃ of following constant temperature calcining 2h, makes described catalyst then.
Comparative example 2
The catalyst of comparative example 2 comprises active component Co 3O 4With carrier A l 2O 3, Co 3O 4With Al 2O 3Weight ratio be 2:8.
The Preparation of catalysts method of comparative example 2 may further comprise the steps:
1) presses Co 3O 4Amount take by weighing cobalt nitrate and fully being dissolved in the distilled water, get Al again 2O 3Impregnated in the gained cobalt nitrate solution, in 70 ℃ of evaporate to dryness moisture content, in 100 ℃ of following freeze-day with constant temperature 24 h, make siccative again under the continuous stirring condition;
2) siccative heating rate with 10 ℃/min in Muffle furnace of making of step 1) is warming up to 350 ℃, at 350 ℃ of following constant temperature calcining 2h, makes described catalyst then.
The catalyst of embodiment 1 ~ 7 is eliminated experiment for the catalysis of air toluene, carry out the activity of such catalysts evaluation; The activity of such catalysts evaluation is carried out in internal diameter is the miniature tubular fixed-bed reactor of 8 mm under normal pressure, and thermocouple is built in the reactor, and reaction temperature is by the control of ü GU-708P type temperature programming controller, and microreactor places tube furnace; Toluene waste gas by volume percentage comprises: toluene 1.0 % and air 99.0 %; The concrete operations step is: measure 50 mg catalyst and pack in the reaction tube of miniature tubular fixed-bed reactor, be warmed up to reaction temperature, feed the toluene waste gas of described composition, at this reaction temperature and 66,000 mLh -1G -1Constant temperature is eliminated toluene (air mass flow is controlled by flowmeter) under the reaction gas air speed condition, by residual toluene content in the online detection tail gas of GC-1026 type gas-chromatography of band hydrogen flame detector, testing conditions is: 220 ℃ of detector temperatures, and 180 ℃ of injector temperatures, post oven temperature, degree perseverance is 150 ℃.
The toluene clearance result of the catalyst of the embodiment 1 ~ 7 that the catalysis elimination experiment of above-mentioned toluene obtains is as shown in table 1:
Figure 2013101373669100002DEST_PATH_IMAGE002
From above-mentioned toluene clearance result as can be seen, the catalyst of embodiment 1 ~ 7 is at high reaction velocity (66,000 mLg – 1H – 1), show good toluene catalytically combustion activity in the low and wide range of reaction temperature; Wherein, most preferably the catalyst of embodiment 1 (sintering temperature is 350 ℃, Co 3O 4With the weight ratio of active carbon be 2:8), this catalyst toluene clearance in the time of 200 ℃ can reach more than 99.7%, can effectively toluene concentration in the air be dropped to below 30 ppm.
The catalyst of embodiment 1 is eliminated experiment for the catalysis of air dimethylbenzene, and dimethylbenzene waste gas by volume percentage comprises: dimethylbenzene 1.0 % and air 99.0 %, all the other experiment conditions are identical with the catalysis elimination experiment of toluene.The dimethylbenzene clearance result of the catalyst of the embodiment 1 that the catalysis elimination experiment of dimethylbenzene obtains is as shown in table 2:
Figure 2013101373669100002DEST_PATH_IMAGE004
The catalyst of embodiment 1 dimethylbenzene clearance in the time of 250 ℃ can reach more than 98 %, can effectively xylene concentration in the air be dropped to below 200 ppm.
The catalyst of embodiment 1 is eliminated experiment for the catalysis of benzene in air, and benzene exhaust air by volume percentage comprises: benzene 1.0 % and air 99.0 %, all the other experiment conditions are identical with the catalysis elimination experiment of toluene.The benzene clearance result of the catalyst of the embodiment 1 that the catalysis elimination experiment of benzene obtains is as shown in table 3:
Figure 2013101373669100002DEST_PATH_IMAGE006
The catalyst of comparative example 1 ~ 2 is eliminated experiment for the catalysis of air toluene, and the toluene clearance result of the catalyst of the comparative example 1 ~ 2 that obtains is as shown in table 4:
Figure 2013101373669100002DEST_PATH_IMAGE008
The toluene clearance of the catalyst of comparative example 1 ~ 2 in the toluene clearance of the catalyst of embodiment in the table 11 and the table 4 is compared, as can be seen, SiO 2, Al 2O 3Compare with these three kinds of carrier materials of active carbon, active carbon of the present invention is the excellent carrier material of catalyst system.
The catalyst of embodiment 1 ~ 5 is carried out the X-ray diffraction detection, and the XRD spectra that obtains is Fig. 1; The X-ray powder diffraction experiment is carried out experimental condition at Philips X ' Pert Pro MPD X-ray diffraction instrument: Cu K α is radiographic source, λ=1.5418, tube voltage 40 kV, tube current 40 mA, 1 °/min of scan frequency, sweep limits 20-80 °.
As shown in Figure 1, the XRD of the catalyst of embodiment 1 ~ 5 spectrum is 36.6 °, 42.6 °, 62.0 °, 74.4 ° and 78.5 ° at the angle of diffraction 2 θ respectively and locates to have occurred high-intensity XRD diffraction maximum, by Co 3O 4The information that provides of standard P DF card as can be known, Co 3O 4-PDF-43-1004:36.5 ° { { { { { 222} namely shows the XRD angle of diffraction and the Co of the catalyst of embodiment 1 ~ 5 for 311} and 77.6 ° for 220}, 73.7 ° for 200}, 61.5 ° for 111}, 42.4 ° 3O 4Closely similar, show in the catalyst of embodiment 1 ~ 5 mainly to have formed Co 3O 4Thing phase, and in this XRD spectra, do not have other cobalt the thing phase (as, CoO, Co 2O 3Deng) be detected.The sintering temperature of the catalyst of embodiment 1 ~ 5 is identical, and Co 3O 4Load capacity difference (the Co of embodiment 1 3O 4Load capacity is the Co of 20%, embodiment 2 3O 4Load capacity is the Co of 10%, embodiment 3 3O 4Load capacity is the Co of 15%, embodiment 4 3O 4Load capacity is the Co of 25%, embodiment 5 3O 4Load capacity is 30%), further contrast as can be known, under the identical sintering temperature condition, different Co 3O 4Load capacity has produced influence to the intensity of XRD diffraction maximum, with Co 3O 4The increase of load capacity, peak intensity is more and more stronger, and it is more and more sharp-pointed that peak shape becomes.
Embodiment 1,6,7 catalyst are carried out X-ray diffraction detect, the XRD spectra that obtains is Fig. 2; Embodiment 1,6,7 catalyst only are that (sintering temperature of embodiment 1 is 350 ℃ to the sintering temperature difference, the sintering temperature of embodiment 6 is 300 ℃, the sintering temperature of embodiment 7 is 400 ℃), as shown in Figure 2, sintering temperature has produced influence to the intensity of XRD diffraction maximum, along with the rising of sintering temperature, Co 3O 4Diffraction peak intensity grow, peak shape become more and more sharp-pointed, Co in the interpret sample 3O 4It is big that grain size becomes, and crystallinity improves.Significantly not new thing phase peak is detected in the XRD spectrum, the variation that does not have main thing phase in the process that sintering temperature changes in the catalyst is described, still with Co 3O 4Exist.
Explanation is at last, above embodiment is only unrestricted in order to technical scheme of the present invention to be described, although by invention has been described with reference to the preferred embodiments of the present invention, but those of ordinary skill in the art is to be understood that, can make various changes to it in the form and details, and not depart from the spirit and scope of the present invention that appended claims limits.

Claims (7)

1. one kind is used for the Co base supported catalyst that benzene in air is thing catalysis elimination, and it is characterized in that: this catalyst comprises active component Co 3O 4And carrier active carbon.
2. according to claim 1 is the Co base supported catalyst that thing catalysis is eliminated for benzene in air, it is characterized in that: in the described catalyst, and Co 3O 4With the weight ratio of active carbon be 1 ~ 3:7 ~ 9.
3. according to claim 2 is the Co base supported catalyst that thing catalysis is eliminated for benzene in air, it is characterized in that: in the described catalyst, and Co 3O 4With the weight ratio of active carbon be 2:8.
Claim 1 to 3 any one described be the preparation method of the Co base supported catalyst eliminated of thing catalysis for benzene in air, it is characterized in that: may further comprise the steps:
1) presses Co 3O 4Amount take by weighing cobalt salt and fully being dissolved in the distilled water, get active carbon again and impregnated in the gained cobalt salt solution, evaporate to dryness moisture content and dry the processing make siccative again;
2) calcination steps 1 in Muffle furnace) siccative that makes makes described catalyst.
5. according to claim 4 is the preparation method of the Co base supported catalyst of thing catalysis elimination for benzene in air, it is characterized in that: in the described step 1), cobalt salt is cobalt nitrate, active carbon is 20 ~ 80 purpose activated carbon granules, active carbon impregnated in the cobalt nitrate solution, in 70 ℃ of evaporate to dryness moisture content, in 100 ℃ of following freeze-day with constant temperature 10 ~ 24 h, make siccative again under the continuous stirring condition.
6. according to claim 4 is the preparation method of the Co base supported catalyst of thing catalysis elimination for benzene in air, it is characterized in that: described step 2), the concrete parameter of roasting is: siccative heating rate with 10 ℃/min in Muffle furnace is warming up to 300 ~ 400 ℃, then at 300 ~ 400 ℃ of following constant temperature calcining 2 ~ 4 h.
7. according to claim 6 is the preparation method of the Co base supported catalyst of thing catalysis elimination for benzene in air, and it is characterized in that: described step 2), sintering temperature is 350 ℃.
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CN112844402A (en) * 2021-01-20 2021-05-28 中国计量大学 Nano cobaltosic oxide supported catalyst for catalytic oxidation of VOCs in biomass boiler flue gas and preparation method thereof

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CN104383878A (en) * 2014-11-19 2015-03-04 上海纳米技术及应用国家工程研究中心有限公司 Overall normal-temperature trace hydrocarbon purification material and preparation method thereof
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CN110090643A (en) * 2019-05-28 2019-08-06 辽宁大学 A kind of composite material Bi of room temperature degradation gaseous pollutant2O3-Co3O4Preparation method and application
CN110090643B (en) * 2019-05-28 2021-06-01 辽宁大学 Composite material Bi for degrading gaseous pollutants at room temperature2O3-Co3O4Preparation method and application of
CN110975870A (en) * 2019-12-12 2020-04-10 重庆工商大学 Preparation method and application of copper-cobalt composite oxide catalyst
CN111330579A (en) * 2020-03-04 2020-06-26 辽宁大学 Mesoporous composite material Fe3O4-Co3O4Preparation method thereof and application thereof in degrading gaseous pollutants
CN111330579B (en) * 2020-03-04 2022-07-19 辽宁大学 Mesoporous composite material Fe3O4-Co3O4Preparation method thereof and application thereof in degrading gaseous pollutants
CN112844402A (en) * 2021-01-20 2021-05-28 中国计量大学 Nano cobaltosic oxide supported catalyst for catalytic oxidation of VOCs in biomass boiler flue gas and preparation method thereof
CN112844402B (en) * 2021-01-20 2022-10-25 中国计量大学 Nano cobaltosic oxide supported catalyst for catalytic oxidation of VOCs in biomass boiler flue gas and preparation method thereof

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