CN105268440A - Graphene loaded cobaltous oxide catalyst and preparation method thereof - Google Patents
Graphene loaded cobaltous oxide catalyst and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a graphene loaded cobaltous oxide catalyst and a preparation method thereof. The preparation method comprises the steps that a cobaltous acetate aqueous solution and a graphene oxide aqueous solution are prepared firstly, after mixing is conducted, magnetic stirring is conducted, and a mixed solution A is obtained; ammonia water is dropwise added into the mixed solution A, magnetic stirring is conducted, and a mixed solution B is obtained; the mixed solution B is filled into a high-pressure reaction kettle with a polytetrafluoroethylene lining, a hydrothermal reaction is conducted for 10-14 h at 160-190 DEG C, and a mixture is obtained; after speed centrifugal separation is conducted on the obtained mixture, supernatant liquor is removed, residual solid matter is transferred to a drying oven after being washed, drying is conducted for 8 h at 60 DEG C, and the graphene loaded cobaltous oxide catalyst is prepared. The prepared catalyst can be applied to catalyzing of carbon monoxide low-temperature oxidation, the carbon monoxide can be completely oxidized into carbon dioxide at 100 DEG C, and the carbon monoxide can be completely converted into the carbon dioxide for at least 3000 min at 100 DEG C.
Description
Technical field
The present invention relates to a kind of catalyst, specifically a kind of graphene-supported cobalt oxide catalyst and preparation method thereof.
Background technology
Carbon monoxide is a kind of major pollutants in air, mainly from vehicle exhaust and industrial processes.Human body can damage central nervous system after sucking, and causes great harm to the health of the mankind.The catalytic oxidative desulfurization of carbon monoxide is the approach effectively controlling its discharge.In the catalyst of catalytic CO oxidation, the catalytic activity of noble metal is higher, but noble metal is expensive, less and generally keep away the defects such as unavoidable sulfur poisoning at occurring in nature content, limit the extensive use in its industry.Significantly work so exploitation base metal all replaces or partly replace the catalyst of noble metal to be one.
Graphene is the two dimensional crystal of monoatomic thickness, is considered to the basic structural unit of fullerene, CNT and graphite.Graphene has the character of high-specific surface area, outstanding heat conductivility and a series of excellence such as mechanical property, outstanding electronic transmission performance, make its research as catalyst carrier cause the extensive concern of scientific worker, graphene-based composite has excellent performance in light degradation, capacitor etc.A lot of research shows, transition metals cobalt has similar even higher than the catalytic CO low-temperature oxidation performance of noble metal, but the easy inactivation of cobalt species of simple component.
Summary of the invention
The present invention seeks to the deficiency for solving the problems of the technologies described above, a kind of graphene-supported cobalt oxide catalyst and preparation method thereof is provided, in the preparation method adopted prepared graphene-supported cobalt oxide catalyst simple to operate, cobalt oxide particle is uniformly dispersed at graphenic surface, particle size is homogeneous, this catalyst is the mesoporous material of aperture 3.1-5.8 nanometer, and specific area is up to 210cm
3/ g; Can be used for the low-temperature oxidation of catalytic CO.
A preparation method for graphene-supported cobalt oxide catalyst, comprises the following steps:
Under step one, normal temperature, be the ratio of 1:20-21 according to mass ratio, get cobalt acetate and distilled water; Join in distilled water by got cobalt acetate, magnetic agitation makes it dissolve completely, the obtained cobalt acetate aqueous solution, for subsequent use;
Step 2, according to mass fraction be 1.12% graphene oxide water solution in the mass ratio of cobalt oxide prepared in Graphene and above-mentioned steps one be the ratio of 1:4-2:3, get the graphene oxide water solution that mass fraction is 1.12%; Got graphene oxide water solution to be joined in above-mentioned steps one get in the distilled water of distilled water 3.7-4.6 volume, be placed in the ultrasonic 60-120 minute of ultrasound reactor of power 168W, the graphene oxide water solution after obtained dilution, for subsequent use;
Step 3, the prepared cobalt acetate aqueous solution and dilution rear oxidation graphene aqueous solution are mixed, magnetic agitation 20-25 minute, obtains mixed solution A; In gained mixed solution A, dropwise add its volume 0.09-0.11 mass fraction is doubly the ammoniacal liquor of 28%, and magnetic agitation 115-120 minute, obtains mixed solution B, for subsequent use;
Step 4, step 3 gained mixed solution B is incorporated with in teflon-lined autoclave, mixed solution B accounts for the 60%-70% of reactor volume, hydro-thermal reaction 10-14h at 160-190 DEG C, naturally cools to room temperature after reaction terminates, obtains mixture;
Step 5, by the mixture of gained after step 4 reaction with the rotating speed centrifugation of 3500r/min after 5-10 minute, remove supernatant liquor, remaining solid material first adopts distilled water to wash 3-5 time, 1 time is washed again with ethanol, transfer in baking oven, 60 DEG C of dry 8h, do not need calcining, namely prepare graphene-supported cobalt oxide catalyst.
In prepared graphene-supported cobalt oxide catalyst, Graphene and cobalt oxide mass ratio are 1:4-2:3, are preferably 3:7; This graphene-supported cobalt oxide catalyst is the mesoporous material of aperture 3.1-5.8 nanometer, and specific area is 210cm
3/ g.This catalyst can be applicable in catalytic CO low-temperature oxidation, can be carbon dioxide by carbon monoxide complete oxidation at 100 DEG C, and there is the stability of higher catalytic CO oxidation, at least can maintain carbon monoxide and be converted into carbon dioxide completely 3000 minutes at 100 DEG C.
Beneficial effect is:
1, the invention provides a kind of preparation method of graphene-supported cobalt oxide catalyst, the method have simple to operate, mild condition is easily controlled, with low cost, the feature that do not need high-temperature calcination.The structure utilizing Graphene special and excellent electronic transmission performance, in conjunction with the high catalytic CO low-temperature oxidation activity of cobalt oxide, simple method is adopted to prepare catalytic CO low-temperature oxidation excellent performance, nano-graphene load cobalt oxide catalyst that stability is high.
2, in the catalyst prepared by the present invention, cobalt oxide particle disperses at two-dimentional Sheet Graphite alkene surface uniform, and particle size is homogeneous, and this catalyst is the mesoporous material of aperture 3.1-5.8 nanometer, and specific area is up to 210cm
3/ g, has high activity in catalytic CO low-temperature oxidation, and 100 DEG C by carbon monoxide complete oxidation, and can have higher stability, keep carbon monoxide to be converted into carbon dioxide completely more than 3000 minutes under the reaction temperature of 100 DEG C.
Accompanying drawing explanation
The X-ray diffracting spectrum of the different Graphene prepared by Fig. 1, the present invention and the graphene-supported cobalt oxide catalyst of cobalt oxide mass ratio;
The transmission electron microscope photo of graphene-supported cobalt oxide catalyst prepared by Fig. 2, embodiment 2 and SEAD photo;
The nitrogen adsorption desorption isotherm of graphene-supported cobalt oxide catalyst prepared by Fig. 3, embodiment 2 and embodiment 3;
The pore size distribution curve of graphene-supported cobalt oxide catalyst prepared by Fig. 4, embodiment 2 and embodiment 3;
The catalyst CO low temperature oxidation performance curve of Fig. 5, Graphene and different Graphene content;
Graphene-supported cobalt oxide catalyst catalytic CO low-temperature oxidation stability curve prepared by Fig. 6, embodiment 2.
Detailed description of the invention
A kind of graphene-supported cobalt oxide catalyst and preparation method thereof, the preparation method adopted is simple to operate, in prepared graphene-supported cobalt oxide catalyst, cobalt oxide particle is uniformly dispersed at graphenic surface, particle size is homogeneous, this catalyst is the mesoporous material of aperture 3.1-5.8 nanometer, and specific area is up to 210cm
3/ g; Can be used for the low-temperature oxidation of catalytic CO.
A preparation method for graphene-supported cobalt oxide catalyst, comprises the following steps:
Under step one, normal temperature, be the ratio of 1:20-21 according to mass ratio, get cobalt acetate and distilled water; Join in distilled water by got cobalt acetate, magnetic agitation makes it dissolve completely, the obtained cobalt acetate aqueous solution, for subsequent use;
Step 2, according to mass fraction be 1.12% graphene oxide water solution in the mass ratio of cobalt oxide prepared in Graphene and above-mentioned steps one be the ratio of 1:4-2:3, get the graphene oxide water solution that mass fraction is 1.12%; Got graphene oxide water solution to be joined in above-mentioned steps one get in the distilled water of distilled water 3.7-4.6 volume, be placed in the ultrasonic 60-120 minute of ultrasound reactor of power 168W, the graphene oxide water solution after obtained dilution, for subsequent use;
Step 3, the prepared cobalt acetate aqueous solution and dilution rear oxidation graphene aqueous solution are mixed, magnetic agitation 20-25 minute, obtains mixed solution A; In gained mixed solution A, dropwise add its volume 0.09-0.11 mass fraction is doubly the ammoniacal liquor of 28%, and magnetic agitation 115-120 minute, obtains mixed solution B, for subsequent use;
Step 4, step 3 gained mixed solution B is incorporated with in teflon-lined autoclave, mixed solution B accounts for the 60%-70% of reactor volume, hydro-thermal reaction 10-14h at 160-190 DEG C, naturally cools to room temperature after reaction terminates, obtains mixture;
Step 5, by the mixture of gained after step 4 reaction with the rotating speed centrifugation of 3500r/min after 5-10 minute, remove supernatant liquor, remaining solid material first adopts distilled water to wash 3-5 time, 1 time is washed again with ethanol, transfer in baking oven, 60 DEG C of dry 8h, do not need calcining, namely prepare graphene-supported cobalt oxide catalyst.
In prepared graphene-supported cobalt oxide catalyst, Graphene and cobalt oxide mass ratio are 1:4-2:3, are preferably 3:7; This graphene-supported cobalt oxide catalyst is the mesoporous material of aperture 3.1-5.8 nanometer, and specific area is 210cm
3/ g.This catalyst can be applicable in catalytic CO low-temperature oxidation, can be carbon dioxide by carbon monoxide complete oxidation at 100 DEG C, and there is the stability of higher catalytic CO oxidation, at least can maintain carbon monoxide and be converted into carbon dioxide completely 3000 minutes at 100 DEG C.
embodiment 1
Under normal temperature, get 2.49 grams of cobalt acetates and be dissolved in 50 ml distilled waters, magnetic agitation makes it dissolve completely, the obtained cobalt acetate aqueous solution I, for subsequent use.The ratio being 1:4 according to the mass ratio of Graphene in catalyst and cobalt oxide gets graphene oxide water solution, adds 230 ml distilled waters, ultrasonic 20 minutes, obtained graphene oxide water solution II, for subsequent use; Wherein, described graphene oxide utilizes the Hummers method improved to prepare graphite oxide, and then through ultrasonic process 60 minutes, obtained mass percentage is the graphene oxide water solution of 1.12%.Solution I and solution II are mixed, magnetic agitation 20 minutes, dropwise adding 26 milliliters of mass percentage is the ammoniacal liquor of 28%, magnetic agitation 120 minutes.Be incorporated with by mixed solution in teflon-lined autoclave, at 180 DEG C, hydro-thermal reaction 12 hours, naturally cools to room temperature; By gained mixture with the rotating speed centrifugation 5-10 minute of 3500r/min, remove supernatant liquor, by remaining solid material distilled water washing 3-5 time, ethanol washs 1 time, precipitation is transferred in baking oven, 60 DEG C of dry 8h.Acquisition Graphene and cobalt oxide mass ratio are the graphene-supported cobalt oxide catalyst of 1:4.
The method that the Hummers method of described improvement prepares graphite oxide is: get 66 milliliters of concentrated sulfuric acids and join in the three-neck flask of 500 milliliters, slowly add 1.5 grams of graphite, 1.5 grams of sodium nitrate, control temperature less than 4 DEG C reaction 90 minutes; Be warming up to 35 DEG C of reactions 30 minutes; Dropwise add distilled water 132 milliliters, control temperature 70 DEG C reaction 15 minutes; Dropwise add hydrogen peroxide and become glassy yellow to solution, centrifugation, salt acid elution, distilled water washing.
embodiment 2
Under normal temperature, get 2.49 grams of cobalt acetates and be dissolved in 50 ml distilled waters, magnetic agitation makes it dissolve completely, the obtained cobalt acetate aqueous solution I, for subsequent use.The ratio being 3:7 according to the mass ratio of Graphene in catalyst and cobalt oxide gets graphene oxide water solution, adds 215 ml distilled waters, ultrasonic 20 minutes, obtained graphene oxide water solution II, for subsequent use; Wherein, described graphene oxide utilizes the Hummers method improved to prepare graphite oxide, and then through ultrasonic process 60 minutes, obtained mass percentage is the graphene oxide water solution of 1.12%.Solution I and solution II are mixed, magnetic agitation 20 minutes, dropwise adding 26 milliliters of mass percentage is the ammoniacal liquor of 28%, magnetic agitation 120 minutes.Be incorporated with by mixed solution in teflon-lined autoclave, at 180 DEG C, hydro-thermal reaction 12 hours, naturally cools to room temperature; By gained mixture with the rotating speed centrifugation 5-10 minute of 3500r/min, remove supernatant liquor, by remaining solid material distilled water washing 3-5 time, ethanol washs 1 time, precipitation is transferred in baking oven, 60 DEG C of dry 8h.Acquisition Graphene and cobalt oxide mass ratio are the graphene-supported cobalt oxide catalyst of 3:7.
embodiment 3
Under normal temperature, get 2.49 grams of cobalt acetates and be dissolved in 50 ml distilled waters, magnetic agitation makes it dissolve completely, the obtained cobalt acetate aqueous solution I, for subsequent use.The ratio being 2:3 according to the mass ratio of Graphene in catalyst and cobalt oxide gets graphene oxide water solution, adds 186 ml distilled waters, ultrasonic 20 minutes, obtained graphene oxide water solution II, for subsequent use; Wherein, described graphene oxide utilizes the Hummers method improved to prepare graphite oxide, and then through ultrasonic process 60 minutes, obtained mass percentage is the graphene oxide water solution of 1.12%.Solution I and solution II are mixed, magnetic agitation 20 minutes, dropwise adding 26 milliliters of mass percentage is the ammoniacal liquor of 28%, magnetic agitation 120 minutes.Be incorporated with by mixed solution in teflon-lined autoclave, at 180 DEG C, hydro-thermal reaction 12 hours, naturally cools to room temperature; By gained mixture with the rotating speed centrifugation 5-10 minute of 3500r/min, remove supernatant liquor, by remaining solid material distilled water washing 3-5 time, ethanol washs 1 time, precipitation is transferred in baking oven, 60 DEG C of dry 8h.Acquisition Graphene and cobalt oxide mass ratio are the graphene-supported cobalt oxide catalyst of 2:3.
test experience:
1, the graphene-supported cobalt oxide catalyst prepared by Example 1, embodiment 2 and embodiment 3 carries out X-ray powder diffraction (XRD) and detects, result as shown in Figure 1, show that the graphene oxide prepared successfully is reduced, in catalyst, all diffraction maximums all and Co
3o
4characteristic diffraction peak corresponding, illustrate and successfully prepared graphene-supported cobalt oxide catalyst.
2, the graphene-supported cobalt oxide catalyst prepared by Example 2 carries out transmission electron microscope feature, and result as shown in Figure 2, shows by Co in the graphene-supported cobalt oxide catalyst prepared by the method
3o
4nano particle diameter is homogeneous, be evenly distributed at graphenic surface; That choose that electronic diffraction proves load on Graphene again is Co
3o
4nano particle.
3, as shown in Figure 3, pore distribution curve as shown in Figure 4 for the nitrogen adsorption desorption isotherm of embodiment 2 and the graphene-supported cobalt oxide catalyst prepared by embodiment 3.Fig. 3 shows, the thermoisopleth of prepared graphene-supported cobalt oxide catalyst belongs to IV type thermoisopleth, shows that sample has typical meso-hole structure; Sample has complete H3 type hysteresis loop, shows that sample has slit-shaped apertures structure and exists.Fig. 4 shows, the most probable pore size of prepared graphene-supported cobalt oxide catalyst concentrates on 4 ran, distributes homogeneous.
4, the graphene-supported cobalt oxide catalyst prepared by Example 1, embodiment 2 and embodiment 3 carries out catalytic CO low-temperature oxidation performance evaluation.0.4 gram of catalyst is loaded in reactor along pad one deck silica wool, raps reactor first down between reactor flat-temperature zone, make that catalyst surface is smooth, thickness is even.Before all catalytic performance tests, room temperature purges 30 minutes, and controlling reacting gas air speed is 11000mL/h/g; Reacting gas is made up of air and carbon monoxide, and carbon monoxide content accounts for 10% of reacting gas total flow; Then, at the temperature of room temperature to 160, choose each temperature spot and carry out continuous active testing; During test, after concrete reaction temperature stablizes 30 minutes, by six-way valve, product is imported on-line chromatographic analysis.Analysis result as shown in Figure 5 and Figure 6.Fig. 5 illustrates that Graphene is to Oxidation of Carbon Monoxide catalytically inactive in Range of measuring temp, in all composite catalysts, Graphene and cobalt oxide mass ratio are that the catalyst of 3:7 has the highest catalytic activity, and the complete oxidation that can realize carbon monoxide at 100 DEG C removes.Figure 6 shows that graphene-supported cobalt oxide catalyst prepared by embodiment 3 is to CO low temperature oxidation stability curve, at can finding out this catalyst 90-150 DEG C, catalytic effect is good, under the reaction temperature of 100 DEG C, effect is best, carbon monoxide can be kept to be converted into carbon dioxide completely more than 3000 minutes, to illustrate that it has higher stability.
Claims (8)
1. a preparation method for graphene-supported cobalt oxide catalyst, is characterized in that: comprise the following steps:
Under step one, normal temperature, be the ratio of 1:20-21 according to mass ratio, get cobalt acetate and distilled water; Join in distilled water by got cobalt acetate, magnetic agitation makes it dissolve completely, the obtained cobalt acetate aqueous solution, for subsequent use;
Step 2, according in Graphene in the mass fraction graphene oxide water solution that is 1.12% and above-mentioned steps one get cobalt oxide mass ratio be the ratio of 1:4-2:3, get the graphene oxide water solution that mass fraction is 1.12%; Got graphene oxide water solution to be joined in above-mentioned steps one get in the distilled water of distilled water 3.7-4.6 volume, be placed in the ultrasonic 60-120 minute of ultrasound reactor of power 168W, obtained dilution rear oxidation graphene aqueous solution, for subsequent use;
Step 3, the prepared cobalt acetate aqueous solution and dilution rear oxidation graphene aqueous solution are mixed, magnetic agitation 20-25 minute, obtains mixed solution A; In gained mixed solution A, dropwise add its volume 0.09-0.11 mass fraction is doubly the ammoniacal liquor of 28%, and magnetic agitation 115-120 minute, obtains mixed solution B, for subsequent use;
Step 4, step 3 gained mixed solution B is incorporated with in teflon-lined autoclave, mixed solution B accounts for the 60%-70% of reactor volume, hydro-thermal reaction 10-14h at 160-190 DEG C, naturally cools to room temperature after reaction terminates, obtains mixture;
Step 5, by the mixture of gained after step 4 reaction with the rotating speed centrifugation of 3500r/min after 5-10 minute, remove supernatant liquor, after remaining solid material washs, transfer in baking oven, 60 DEG C of dry 8h, namely prepare graphene-supported cobalt oxide catalyst.
2. the preparation method of graphene-supported cobalt oxide catalyst as claimed in claim 1, is characterized in that: the method that the material of remaining solid described in step 5 carries out washing is, first adopts distilled water washing 3-5 time, then washs 1 time with ethanol.
3. the preparation method of graphene-supported cobalt oxide catalyst as claimed in claim 1, is characterized in that:
In prepared graphene-supported cobalt oxide catalyst, Graphene and cobalt oxide mass ratio are 1:4-2:3.
4. the preparation method of graphene-supported cobalt oxide catalyst as claimed in claim 3, is characterized in that:
In prepared graphene-supported cobalt oxide catalyst, Graphene and cobalt oxide mass ratio are 3:7.
5. the preparation method of graphene-supported cobalt oxide catalyst as claimed in claim 1, is characterized in that: prepared graphene-supported cobalt oxide catalyst is the mesoporous material of aperture 3.1-5.8 nanometer, and specific area is 210cm
3/ g.
6., as the preparation method of claim 1-5 graphene-supported cobalt oxide catalyst as described in one of them, it is characterized in that: the prepared application of graphene-supported cobalt oxide catalyst in catalytic CO low-temperature oxidation.
7. the preparation method of graphene-supported cobalt oxide catalyst as claimed in claim 6, is characterized in that: the temperature of described catalytic CO low-temperature oxidation is 90-150 DEG C.
8. as right wants the preparation method of graphene-supported cobalt oxide catalyst as described in 7, it is characterized in that: the temperature of described catalytic CO low-temperature oxidation is 100 DEG C.
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