CN103191743B - 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 PDFInfo
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- CN103191743B CN103191743B CN201310137366.9A CN201310137366A CN103191743B CN 103191743 B CN103191743 B CN 103191743B CN 201310137366 A CN201310137366 A CN 201310137366A CN 103191743 B CN103191743 B CN 103191743B
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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
Technical field
The present invention relates to a kind of benzene homologues catalyst for catalytic combustion, be specifically related to a kind of Co base supported catalyst for benzene in air system thing catalytic removal and preparation method thereof.
Background technology
Volatile organic matter (Volatile Organic Compounds-VOCs) waste gas causes one of air-polluting main matter, even under lower concentration, serious harm can be caused to environment and the mankind, in these VOCs, the harm of benzene homologues (e.g., benzene, benzene homologues, two benzene homologues etc.) is more outstanding.Benzene homologues is mainly derived from industrial waste gas, be iron and steel manufacture, semiconductor components and devices production, petrochemical industry, pharmacy, printing, shoemaking, the industry such as to spray paint discharge modal pollutant.Because benzene homologues has volatile feature, the multiplex benzene homologues of house decorative material, two benzene homologues replace purified petroleum benzin as the solvent of the materials such as various glue, paint, coating or diluent, and therefore, interior decoration is also important benzene homologues source.WHO is defined as strong carcinogen benzene, has mutagenesis, teratogenesis and carcinogenic " three cause " harm, caused the great attention of countries in the world to human body.Processing method for benzene homologues can be divided into two large classes usually: a class is non-destructive technique and absorption method; One class is destructive technology, namely make benzene homologues 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 the common technique such as direct burning, catalytic combustion, biodegradation, plasma oxidation, photocatalytic oxidation.Wherein, catalytic combustion can process the benzene homologues gas of low concentration under far below direct ignition temperature condition, has the advantages that purification efficiency is high, non-secondary pollution, energy consumption are low, is one of the most effective processing method of process benzene homologues application.
At present, benzene homologues catalyst for catalytic combustion used mainly contains noble metal catalyst and catalyst of transition metal oxide.Noble metal catalyst mainly comprises containing Pt, Pd, Ru and Au etc., due to high, selective good, the long service life of activity, high temperature resistant and have the advantages such as good antitoxin performance, causes the great interest of researcher.Although noble metal catalyst has lot of advantages, due to its expensive and limit noble metal catalyst benzene homologues eliminate in application.Therefore, cheap in recent years catalyst of transition metal oxide causes the broad interest of people.Research for catalyst of transition metal oxide finds, the composite oxide catalysts with spinelle and perovskite structure shows good benzene homologues catalytic combustion activity and stability, and price exists very large advantage, and easily obtain, therefore have broad application prospects.But to studied non-precious metal catalyst, exist subject matter be the clearance of benzene homologues still (< 90 %) on the low side, reaction temperature high (> 300 DEG C), which also limits application non-precious metal catalyst being used for benzene in air system thing catalytic removal.Carry out further and non-precious metal catalyst is used for benzene in air system thing catalytic removal, develop the catalyst with high low temperature active and atmospheric environment protection is had great importance.
Summary of the invention
In view of this, the invention provides a kind of Co base supported catalyst for benzene in air system thing catalytic removal and preparation method thereof, this catalyst is with low cost and have good low temperature benzene homologues catalytic combustion activity.
The invention discloses a kind of Co base supported catalyst for benzene in air system thing catalytic removal, this catalyst comprises active component Co
3o
4and carrier active carbon.
Further, in described catalyst, Co
3o
4be 1 ~ 3:7 ~ 9 with the weight ratio of active carbon.
Further, in described catalyst, Co
3o
4be 2:8 with the weight ratio of active carbon.
The invention also discloses the preparation method of the above-mentioned Co base supported catalyst for benzene in air system thing catalytic removal, comprise the following steps:
1) by Co
3o
4amount take cobalt salt being fully dissolved in distilled water, then get active carbon and impregnated in gained cobalt salt solution, then evaporate to dryness moisture content dry process, obtained siccative;
2) calcination steps 1 in Muffle furnace) obtained siccative, obtained described catalyst.
Further, in described step 1), cobalt salt is cobalt nitrate, and active carbon is 20 ~ 80 object activated carbon granules, and active carbon impregnated in cobalt nitrate solution, in 70 DEG C of evaporate to dryness moisture content under continuous stirring condition, then at 100 DEG C freeze-day with constant temperature 10 ~ 24 h, obtained siccative.
Further, described step 2) in, the design parameter of roasting is: siccative is warming up to 300 ~ 400 DEG C with the heating rate of 10 DEG C/min in Muffle furnace, then constant temperature calcining 2 ~ 4 h at 300 ~ 400 DEG C.
Further, described step 2) in, sintering temperature is 350 DEG C.
Beneficial effect of the present invention is:
1) catalyst of the present invention take active carbon as carrier, with the oxide Co of base metal cobalt
3o
4for active component, considerably reduce catalyst cost;
2) catalyst of the present invention is at high reaction velocity (66,000 mLg
– 1h
– 1), show good benzene homologues catalytic combustion activity in low and wide range of reaction temperature; 200 DEG C time, toluene removal rate can reach more than 99.7%, effectively toluene concentration in air can be dropped to 30 below ppm, and 250 DEG C time, dimethylbenzene clearance can reach 98 more than %, effectively xylene concentration in air can be dropped to 200 below ppm;
3) cobalt salt is carried on active carbon by wet infusion process by the present invention, and then obtained containing Co by high-temperature roasting
3o
4catalyst, the method technique is simple, and mild condition is easily controlled, reproducible.
Accompanying drawing explanation
In order to make the object, technical solutions and advantages of the present invention clearly, below in conjunction with accompanying drawing, the present invention is described in further detail, wherein:
Fig. 1 is the XRD spectra of the catalyst of embodiment 1 ~ 5;
Fig. 2 is the XRD spectra of the catalyst of embodiment 1,6,7.
Detailed description of the invention
Hereinafter with reference to accompanying drawing, the preferred embodiments of the present invention are described in detail.
embodiment 1
The catalyst of the present embodiment comprises active component Co
3o
4and carrier active carbon, Co
3o
4be 2:8 with the weight ratio of active carbon.
The preparation method of the catalyst of the present embodiment, comprises the following steps:
1) by Co
3o
4amount take cobalt nitrate being fully dissolved in distilled water, getting 20 ~ 80 object activated carbon granules again impregnated in gained cobalt nitrate solution, in 70 DEG C of evaporate to dryness moisture content under continuous stirring condition, at 100 DEG C, freeze-day with constant temperature 24 h(is the crystallization water removed in raw material in the object of 100 DEG C of freeze-day with constant temperature again, drying time is that 10 ~ 24h all can realize goal of the invention herein), obtained siccative;
2) siccative that step 1) is obtained is warming up to 350 DEG C with the heating rate of 10 DEG C/min, then constant temperature calcining 2h at 350 DEG C in Muffle furnace, obtained described catalyst.
embodiment 2
The catalyst of the present embodiment comprises active component Co
3o
4and carrier active carbon, Co
3o
4be 1:9 with the weight ratio of active carbon.
The preparation method of the catalyst of the present embodiment is identical with embodiment 1.
embodiment 3
The catalyst of the present embodiment comprises active component Co
3o
4and carrier active carbon, Co
3o
4be 1.5:8.5 with the weight ratio of active carbon.
The preparation method of the catalyst of the present embodiment is identical with embodiment 1.
embodiment 4
The catalyst of the present embodiment comprises active component Co
3o
4and carrier active carbon, Co
3o
4be 2.5:7.5 with the weight ratio of active carbon.
The preparation method of the catalyst of the present embodiment is identical with embodiment 1.
embodiment 5
The catalyst of the present embodiment comprises active component Co
3o
4and carrier active carbon, Co
3o
4be 3:7 with the weight ratio of active carbon.
The preparation method of the catalyst of the present embodiment is identical with embodiment 1.
embodiment 6
The catalyst of the present embodiment comprises active component Co
3o
4and carrier active carbon, Co
3o
4be 2:8 with the weight ratio of active carbon.
In the preparation method of the catalyst of the present embodiment, except step 2) sintering temperature be except 300 DEG C, all the other conditions are identical with embodiment 1.
embodiment 7
The catalyst of the present embodiment comprises active component Co
3o
4and carrier active carbon, Co
3o
4be 2:8 with the weight ratio of active carbon.
In the preparation method of the catalyst of the present embodiment, except step 2) sintering temperature be except 400 DEG C, 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 method of the catalyst of comparative example 1, comprises the following steps:
1) by Co
3o
4amount take cobalt nitrate being fully dissolved in distilled water, then get mesopore SiO
2impregnated in gained cobalt nitrate solution, in 70 DEG C of evaporate to dryness moisture content under continuous stirring condition, then at 100 DEG C freeze-day with constant temperature 24 h, obtained siccative;
2) siccative that step 1) is obtained is warming up to 350 DEG C with the heating rate of 10 DEG C/min, then constant temperature calcining 2h at 350 DEG C in Muffle furnace, obtained described catalyst.
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 method of the catalyst of comparative example 2, comprises the following steps:
1) by Co
3o
4amount take cobalt nitrate being fully dissolved in distilled water, then get Al
2o
3impregnated in gained cobalt nitrate solution, in 70 DEG C of evaporate to dryness moisture content under continuous stirring condition, then at 100 DEG C freeze-day with constant temperature 24 h, obtained siccative;
2) siccative that step 1) is obtained is warming up to 350 DEG C with the heating rate of 10 DEG C/min, then constant temperature calcining 2h at 350 DEG C in Muffle furnace, obtained described catalyst.
The catalyst of embodiment 1 ~ 7 is used for the catalytic removal experiment of toluene in air, carries out the activity rating of catalyst; The activity rating of catalyst is carry out in the miniature tubular fixed-bed reactor of 8 mm at ambient pressure in internal diameter, and thermocouple is built in reactor, and reaction temperature is controlled by ü GU-708P type temperature programming controller, and microreactor is placed in tube furnace; Toluene waste gas by volume percentage comprises: toluene 1.0 % and air 99.0 %; Concrete operation step is: measure 50 mg catalyst and load in the reaction tube of miniature tubular fixed-bed reactor, be warmed up to reaction temperature, pass into the toluene waste gas of described composition, in this reaction temperature and 66, and 000 mLh
-1g
-1under reaction gas space velocities, constant temperature eliminates toluene (air mass flow is controlled by flowmeter), by residual toluene content in the GC-1026 type gas-chromatography on-line checkingi tail gas of band hydrogen flame detector, testing conditions is: detector temperature 220 DEG C, injector temperature 180 DEG C, and post case temperature perseverance is 150 DEG C.
The toluene removal rate result that the catalytic removal of above-mentioned toluene tests the catalyst of the embodiment 1 ~ 7 obtained is as shown in table 1:
As can be seen from above-mentioned toluene removal rate result, the catalyst of embodiment 1 ~ 7 is at high reaction velocity (66,000 mLg
– 1h
– 1), to show good toluene catalytic combustion in low and wide range of reaction temperature active; Wherein, (sintering temperature is 350 DEG C to the catalyst of most preferably embodiment 1, Co
3o
4be 2:8 with the weight ratio of active carbon), this catalyst toluene removal rate 200 DEG C time can reach more than 99.7%, effectively toluene concentration in air can be dropped to 30 below ppm.
The catalyst of embodiment 1 is used for the catalytic removal experiment of dimethylbenzene in air, xylene waste gas by volume percentage comprises: dimethylbenzene 1.0 % and air 99.0 %, all the other experiment conditions are tested identical with the catalytic removal of toluene.The dimethylbenzene clearance result that the catalytic removal of dimethylbenzene tests the catalyst of the embodiment 1 obtained is as shown in table 2:
Catalyst dimethylbenzene clearance 250 DEG C time of embodiment 1 can reach 98 more than %, effectively xylene concentration in air can be dropped to 200 below ppm.
The catalyst of embodiment 1 is used for the catalytic removal experiment of benzene in air, benzene exhaust air by volume percentage comprises: benzene 1.0 % and air 99.0 %, all the other experiment conditions are tested identical with the catalytic removal of toluene.The benzene clearance result that the catalytic removal of benzene tests the catalyst of the embodiment 1 obtained is as shown in table 3:
The catalyst of comparative example 1 ~ 2 is used for the catalytic removal experiment of toluene in air, the toluene removal rate result of the catalyst of the comparative example 1 ~ 2 obtained is as shown in table 4:
By the toluene removal rate of the catalyst of embodiment in table 11 compared with the toluene removal rate of the catalyst of comparative example in table 41 ~ 2, can find out, 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 X-ray diffraction detection, and the XRD spectra obtained is Fig. 1; X-ray powder diffraction experiment is carried out on Philips X ' Pert Pro MPD X-ray diffraction instrument, experimental condition: Cu K α is radiographic source, λ=1.5418, tube voltage 40 kV, tube current 40 mA, scan frequency 1 °/min, sweep limits 20-80 °.
As shown in Figure 1, the XRD of the catalyst of embodiment 1 ~ 5 spectrum is the XRD diffraction maximum that high strength has appearred in 36.6 °, 42.6 °, 62.0 °, 74.4 ° and 78.5 ° of places at the angle of diffraction 2 θ respectively, by Co
3o
4the information that provides of standard P DF card known, Co
3o
4-PDF-43-1004:36.5 ° { 111}, 42.4 ° { 200}, 61.5 ° { 220}, 73.7 ° { 311} and 77.6 ° { namely 222} shows the XRD angle of diffraction and the Co of the catalyst of embodiment 1 ~ 5
3o
4closely similar, show mainly to define Co in the catalyst of embodiment 1 ~ 5
3o
4thing phase, and in this XRD spectra, there is no thing phase (e.g., CoO, Co of other cobalt
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 20%, the Co of embodiment 2
3o
4load capacity is 10%, the Co of embodiment 3
3o
4load capacity is 15%, the Co of embodiment 4
3o
4load capacity is 25%, the Co of embodiment 5
3o
4load capacity is 30%), contrast is known further, under identical sintering temperature condition, different Co
3o
4the intensity of load capacity on XRD diffraction maximum creates impact, with Co
3o
4the increase of load capacity, peak intensity is more and more stronger, and peak shape becomes more and more sharp-pointed.
The catalyst of embodiment 1,6,7 is carried out X-ray diffraction detection, and the XRD spectra obtained is Fig. 2; The catalyst of embodiment 1,6,7 is only that (sintering temperature of embodiment 1 is 350 DEG C to sintering temperature difference, the sintering temperature of embodiment 6 is 300 DEG C, the sintering temperature of embodiment 7 is 400 DEG C), as shown in Figure 2, the intensity of sintering temperature on XRD diffraction maximum creates impact, along with the rising of sintering temperature, Co
3o
4diffraction peak intensity grow, peak shape becomes more and more sharp-pointed, Co in interpret sample
3o
4grain size becomes large, and crystallinity improves.In XRD spectrum, significantly new thing phase peak is not detected, and the change not having dominant phase is described, still with Co in the process of sintering temperature change in catalyst
3o
4exist.
What finally illustrate is, above embodiment is only in order to illustrate technical scheme of the present invention and unrestricted, although by referring to the preferred embodiments of the present invention, invention has been described, but those of ordinary skill in the art is to be understood that, various change can be made to it in the form and details, and not depart from the spirit and scope of the present invention that appended claims limits.
Claims (4)
1., for a Co base supported catalyst for benzene homologues catalytic removal multiple in air, it is characterized in that: this catalyst is by active component Co
3o
4with carrier active carbon composition, Co
3o
4be 1 ~ 3:7 ~ 9 with the weight ratio of active carbon, synthesis step is as follows:
1) by Co
3o
4amount take cobalt nitrate being fully dissolved in distilled water, then get 20 ~ 80 object active carbons and impregnated in gained cobalt nitrate solution, in 70 DEG C of evaporate to dryness moisture content under continuous stirring condition, then at 100 DEG C freeze-day with constant temperature 10 ~ 24 h, obtained siccative;
2) siccative is warming up to 300 ~ 400 DEG C with the heating rate of 10 DEG C/min in Muffle furnace, then constant temperature calcining 2 ~ 4 h at 300 ~ 400 DEG C, obtained described catalyst.
2. the Co base supported catalyst for benzene homologues catalytic removal multiple in air according to claim 1, is characterized in that: in described catalyst, Co
3o
4be 2:8 with the weight ratio of active carbon.
3. the preparation method of the Co base supported catalyst for benzene homologues catalytic removal multiple in air described in claim 1 to 2 any one, is characterized in that: comprise the following steps:
1) by Co
3o
4amount take cobalt nitrate being fully dissolved in distilled water, then get 20 ~ 80 object active carbons and impregnated in gained cobalt nitrate solution, in 70 DEG C of evaporate to dryness moisture content under continuous stirring condition, then at 100 DEG C freeze-day with constant temperature 10 ~ 24 h, obtained siccative;
2) siccative is warming up to 300 ~ 400 DEG C with the heating rate of 10 DEG C/min in Muffle furnace, then constant temperature calcining 2 ~ 4 h at 300 ~ 400 DEG C, obtained described catalyst.
4. the preparation method of the Co base supported catalyst for benzene homologues catalytic removal multiple in air according to claim 3, is characterized in that: described step 2) in, sintering temperature is 350 DEG C.
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| CN104383878B (en) * | 2014-11-19 | 2016-04-27 | 上海纳米技术及应用国家工程研究中心有限公司 | Monoblock type trace carbon hydrogen compound normal temperature scavenging material and preparation method thereof |
| CN106582651B (en) * | 2017-01-10 | 2019-07-23 | 武汉大学 | A kind of preparation method of the nanometer cobalt catalyst of porous carrier load |
| 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 |
| 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 |
| 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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| CN102000576A (en) * | 2010-11-30 | 2011-04-06 | 复旦大学 | Catalyst for toluene exhaust gas catalytic combustion and preparation method thereof |
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| CN1792438A (en) * | 2005-12-21 | 2006-06-28 | 中国科学院山西煤炭化学研究所 | Catalyst for treating benzene series organic waste-gas or waste-water by using low temp. and dry method, prepn. method and application thereof |
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