CN102319570A - The ternary compound oxides Catalysts and its preparation method of carbon monoxide oxidation - Google Patents
The ternary compound oxides Catalysts and its preparation method of carbon monoxide oxidation Download PDFInfo
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Abstract
The ternary compound oxides Catalysts and its preparation method of carbon monoxide oxidation relates to a kind of catalyst.A kind of ternary compound oxides Catalysts and its preparation method with carbon monoxide oxidation of active height and high mithridatism under the low temperature is provided.Catalyst consist of CuO-CeO-M, M is Co, Ni, Zn, Mg, at least a in the Zr metal oxide; The mol ratio of each component content of catalyst is CuO: CeO: M=20: 80: (0.1～20).Prepare the precursor solution of CuO, CeO and M metal oxide respectively, press the catalyst component proportioning and mix, get mixed liquor A; The preparation precipitant solution joins mixed liquor A in the precipitant solution after the heating, gets mixed liquid B; In mixed liquid B, add the surfactant reaction, get precipitated liquid; With precipitated liquid washing, filtration under diminished pressure, drying, roasting obtains the ternary compound oxides catalyst of carbon monoxide oxidation.
Description
Technical field
The present invention relates to a kind of catalyst, especially relate to a kind of ternary compound oxides Catalysts and its preparation method of carbon monoxide oxidation.
Background technology
As everyone knows, carbon monoxide is important industrial energy and raw material, also is one of important pollutant of many industrial environments and indoor environment.In the live and work environment; The existence of a small amount of carbon monoxide has had a strong impact on the healthy of the mankind; Smoking is to the pollution of room air, and engine discharge tail gas at work all will produce the carbon monoxide of poisoning human body, so the elimination of carbon monoxide is extremely important.In addition, mining, carbon monoxide protection military and civil and seal cavity are had very important protective action, the elimination of CO can be used for preventing that the existence owing to CO produces the electrode poisoning in the various fuel cells in the fuel cell.Traditional Au, Ag, Pd, noble metal catalysts such as Rh have good low-temperature catalyzed carbon monoxide oxidation activity, but since exist noble metal expensive, the occurring in nature reserves are few, defective such as poisonings very easily, so limited it and used widely.And catalyst of transition metal oxide such as copper, manganese, cobalt, iron, chromium etc. have potential superiority, and is low and insensitive to some catalyst poison (like chlorine etc.) like price.In recent years, more and more researchers turns to non-precious metal catalyst to notice, and these non-precious metal catalysts have shown good catalytic activity, can become the substitute of noble metal catalyst, therefore becomes the emphasis of researcher research.
Cerium oxide is a kind of oxide with fluorite structure; They have oxygen ions migrate usually and at high temperature CO are had the character of good catalytic oxidation activity; Copper is as co-catalyst, and ability and cerium oxide form copper cerium cooperative effect usually, thereby can significantly improve the catalytic performance of cerium oxide.Zhou Renxian etc. (referring to Chinese patent CN 200710156724.5) are complexing agent with the softex kw, and ethanol is the resulting copper cerium catalyst of solvent, and the conversion ratio of CO can reach 97.1% at 110 ℃.Jung employing coprecipitations such as (C.R.jung et al., Catal Today, 2004,93-95,183) prepares CuO-CeO
2Catalyst is discovered, has formed Cu-Ce-O solid solution in the catalyst, and the conversion ratio of CO is 99% in the time of 170 ℃.Liu etc. (Y.Liu et al., Appl.catalA, 1994, B4,167) have studied CuO-CeO
2The performance of removing CO by selective oxidation and auxiliary agent Zr, La, Pr find that to its Effect on Performance the adding of Zr, Pr has reduced CuO-CeO
2The performance of catalyst, La is then to CuO-CeO
2The performance of catalyst is influence not, and the CO conversion ratio reaches the highest (99%) in the time of 165 ℃.Wang etc. (J.B.Wang et al., Appl.catal.A, 2002,232,107) have studied the oxidation reaction performance of the CuO/CeO catalyst of doping oxidation shirt to CO, find that the CuO of body phase can be by CO and H
2Reduction generates metastable copper bunch, and the activity at it and metallic carrier interface has constituted the active sites of CO oxidation reaction, and the CO conversion ratio is 78% in the time of 120 ℃.Park etc. (J.W.Park et al., J.Hydrogen Energy, 2005,30,209) research shows that the adding of Co has improved CuO-CeO
2/ γ-Al
2O
3The catalytic performance of catalyst, at 210～225 ℃, the conversion ratio of CO can reach 99.9%.
Summary of the invention
The object of the present invention is to provide a kind of ternary compound oxides Catalysts and its preparation method with carbon monoxide oxidation of active height and high mithridatism under the low temperature.
The ternary compound oxides catalyst of said carbon monoxide oxidation consist of CuO-CeO-M, M is Co, Ni, Zn, Mg, at least a in the Zr metal oxide etc.; The mol ratio of each component content of catalyst is CuO: CeO: M=20: 80: (0.1～20).
The ternary compound oxides catalyst of said carbon monoxide oxidation the preparation method adopt the anti-coprecipitation that adds, concrete steps are following:
1) prepare the precursor solution of CuO, CeO and M metal oxide respectively, press the catalyst component proportioning and mix, mixed liquor A;
2) the preparation precipitant solution joins mixed liquor A in the precipitant solution after the heating, gets mixed liquid B;
3) in mixed liquid B, add the surfactant reaction, get precipitated liquid;
4) with the washing of the precipitated liquid of step 3) gained, filtration under diminished pressure, drying, roasting obtains the ternary compound oxides catalyst of carbon monoxide oxidation.
In step 1), the concentration of the precursor solution of said CuO metal oxide can be 1mol/L, and the concentration of the precursor solution of said CeO metal oxide can be 1mol/L, and the concentration of the precursor solution of said M metal oxide can be 1mol/L; The presoma of said CuO metal oxide is the nitrate of copper, and the presoma of said CeO metal oxide is the nitrate of cerium, and the presoma of said M metal oxide is the nitrate of M metal.
In step 2) in, said precipitating reagent can be selected from NaOH etc.; The concentration of said precipitant solution can be 0.1～0.4mol/L, and the temperature of said heating can be 40～70 ℃, said join mixed liquor A in the precipitant solution after, scalable pH is 8.5～10.
In step 3), said surfactant can be selected from L-glutamic acid etc., and the mol ratio of the presoma of said surfactant and metal oxide can be (0.007～0.06): 10; The temperature of said reaction can be 40～70 ℃, and the time of reaction can be 1～3h.
In step 4), the temperature of said drying can be 80～120 ℃, and the dry time can be 4～8h; The temperature of said roasting can be 300～600 ℃, and the time of roasting can be 3～6h.
The ternary compound oxides catalyst of prepared carbon monoxide oxidation can carry out CO catalytic oxidation performance evaluation on atmospheric fixed bed reactor, unstripped gas consists of: CO:1%, O
2: 1%, N
2: 98%, the gas volume air speed is 18000h
-1, reaction temperature is 40～120 ℃, the conversion ratio of CO is obtained by gas chromatographic analysis.
The ternary compound oxides catalyst activity of the carbon monoxide oxidation that the present invention is prepared is high, can be under 70 ℃ low reaction temperatures, under the situation of anoxic with the quick and complete oxidation of CO.And the preparation method is simple, and cost is low, less energy consumption and discharge of noxious gases not, and environmental friendliness, broad application temperature range has good mithridatism to water and carbon dioxide.
Description of drawings
Fig. 1 is the XRD spectra of the ternary compound oxides catalyst embodiment of carbon monoxide oxidation according to the invention.At Fig. 1, abscissa is angle of diffraction 2Theta (degrees), and ordinate is intensity I ntensity (a.u.).
Uv raman spectroscopy (325-nm) figure of the ternary compound oxides catalyst embodiment of Fig. 2 carbon monoxide oxidation according to the invention.In Fig. 2, abscissa is Raman shift Raman shift (cm
-1), ordinate is intensity I ntensity (a.u.).
Fig. 3 is the ESR spectrum of the ternary compound oxides catalyst embodiment of carbon monoxide oxidation according to the invention.In Fig. 3, abscissa is magnetic field Magnetic Field (G), and ordinate is intensity I ntensity (a.u.).
The infrared spectrum of the ternary compound oxides catalyst embodiment of Fig. 4 carbon monoxide oxidation according to the invention.In Fig. 4, abscissa is wave number Wavenumbers (cm
-1), ordinate is intensity I ntensity (a.u.).
The specific embodiment
Catalyst according to the invention carries out CO catalytic oxidation performance evaluation on atmospheric fixed bed reactor, unstripped gas consists of CO:1%, O
2: 1%, N
2: 98%, the gas volume air speed is 18000h
-1Reaction temperature is 40 ℃ to 120 ℃, and the conversion ratio of CO is obtained by gas chromatographic analysis.
The dissolution of sodium hydroxide that takes by weighing 6.4g is in 400 milliliters deionized water; Be heated to 40 ℃ while stirring; Rotating speed 640r/min is measured the cerous nitrate solution (1mol/L) of 40ml, and the nickel nitrate solution (1mol/L) of the copper nitrate solution of 10ml (1mol/L) and 10ml fully mixes.Mixed liquor with above-mentioned three kinds of components under vigorous stirring dropwise joins in the sodium hydroxide solution.Regulate PH=9 with precipitating reagent NaOH, under agitation add the L-glutamic acid of 1.03g.At 40 ℃, rotating speed 640r/min is reaction 2h down.Again with 60 ℃ deionized water washing 5 times.Filtration under diminished pressure, at 110 ℃ of following dry 5h, 400 ℃ of following roasting 3h (heating rate be 3 ℃/min) obtain the ternary compound oxides catalyst.Fig. 1 provides the XRD spectra of the ternary compound oxides catalyst embodiment of carbon monoxide oxidation according to the invention.The XRD figure spectrum of embodiment 1 catalyst is shown in the curve a among Fig. 1, and ultraviolet Raman collection of illustrative plates is shown in the curve a among Fig. 2, and the electron spin resonance collection of illustrative plates is shown in the curve a among Fig. 3.
The preparation method of embodiment 2～4 is identical with embodiment 1, and the amount of NaOH changes 6g respectively into, 5.68g, and 5.6g, nickel nitrate solution change 5ml, 1ml, 0.2ml respectively into.The XRD figure spectrum of embodiment 2～4 catalyst is shown in the curve b among Fig. 1, c, d, and ultraviolet Raman collection of illustrative plates is shown in the curve b among Fig. 2, c, d, and the electron spin resonance collection of illustrative plates is shown in the curve b among Fig. 3, c, d.
The catalysis CO conversion ratio of embodiment 1～4 catalyst is seen table 1.
Table 1 (%)
Embodiment 5
The dissolution of sodium hydroxide that takes by weighing 5.6g is in 400 milliliters deionized water; Be heated to 40 ℃ while stirring; Rotating speed 640r/min is measured the cerous nitrate solution (1mol/L) of 40ml, and the cobalt nitrate solution (1mol/L) of the copper nitrate solution of 10ml (1mol/L) and 0.1ml fully mixes.Mixed liquor with above-mentioned three kinds of components under vigorous stirring dropwise joins in the sodium hydroxide solution.Regulate PH=9 with precipitating reagent NaOH, behind the 5min, under agitation add the L-glutamic acid of 1.03g.At 40 ℃, rotating speed 640r/min is reaction 1h down.With 60 ℃ deionized waters washing 5 times, filtration under diminished pressure, at 120 ℃ of dry 4h down, 600 ℃ of following roasting 3h (heating rate be 3 ℃/min) obtain the ternary compound oxides catalyst.The infrared spectrum of the catalyst of embodiment 5 is as shown in Figure 4.
Embodiment 6～8
The preparation method of embodiment 6～8 is identical with embodiment 5, and the amount of NaOH changes 5.68g respectively into, 6g, and 6.4g, cobalt nitrate solution change 1ml, 5ml, 10ml respectively into.
The catalysis CO conversion ratio of embodiment 5～8 catalyst is seen table 2.
Table 2 (%)
Embodiment 9
The dissolution of sodium hydroxide that takes by weighing 6.4g is in 400 milliliters deionized water; Be heated to 40 ℃ while stirring; Rotating speed 640r/min is measured the cerous nitrate solution (1mol/L) of 40ml, and the zinc nitrate solution (1mol/L) of the copper nitrate solution of 10ml (1mol/L) and 10ml fully mixes.Mixed liquor with above-mentioned three kinds of components under vigorous stirring dropwise joins in the sodium hydroxide solution.Regulate PH=9 with precipitating reagent NaOH, behind the 5min, under agitation add the L-glutamic acid of 1.03g.At 40 ℃, rotating speed 640r/min is reaction 2h down.With 60 ℃ deionized waters washing 5 times, filtration under diminished pressure, at 110 ℃ of dry 4h down, 350 ℃ of following roasting 3h (heating rate be 3 ℃/min) obtain the ternary compound oxides catalyst.
Embodiment 10～12
The preparation method of embodiment 10～12 is identical with embodiment 9, and the amount of NaOH changes 6g respectively into, and 5.68g.5.6g, zinc nitrate solution change 5ml, 1ml, 0.1ml respectively into.
The catalysis CO conversion ratio of embodiment 9～12 catalyst is seen table 3.
Table 3 (%)
Embodiment 13
The dissolution of sodium hydroxide that takes by weighing 5.62g is in 400 milliliters deionized water; Be heated to 40 ℃ while stirring; Rotating speed 640r/min is measured the cerous nitrate solution (1mol/L) of 40ml, and the zirconyl chloride solution (1mol/L) of the copper nitrate solution of 10ml (1mol/L) and 0.1ml fully mixes.Mixed liquor with above-mentioned three kinds of components under vigorous stirring dropwise joins in the sodium hydroxide solution.Regulate PH=9 with precipitating reagent NaOH, behind the 5min, under agitation add the L-glutamic acid of 1.03g.At 40 ℃, rotating speed 640r/min is reaction 1h down.With 60 ℃ deionized waters washing 5 times, filtration under diminished pressure, at 110 ℃ of dry 8h down, 400 ℃ of following roasting 6h (heating rate be 3 ℃/min) obtain the ternary compound oxides catalyst.
Embodiment 14～16
The preparation method of embodiment 14～16 is identical with embodiment 13.The amount of NaOH changes 5.76g respectively into, 6.4g, and 7.2g, zirconyl chloride solution change 1ml, 5ml, 10ml respectively into.
The catalysis CO conversion ratio of embodiment 13～16 catalyst is seen table 4.
Table 4 (%)
Embodiment 17
The dissolution of sodium hydroxide that takes by weighing 6.4g is in 400 milliliters deionized water; Be heated to 40 ℃ while stirring; Rotating speed 640r/min is measured the cerous nitrate solution (1mol/L) of 40ml, and the magnesium nitrate solution (1mol/L) of the copper nitrate solution of 10ml (1mol/L) and 10ml fully mixes.Mixed liquor with above-mentioned three kinds of components under vigorous stirring dropwise joins in the sodium hydroxide solution.Regulate PH=9 with precipitating reagent NaOH, behind the 5min, under agitation add the L-glutamic acid of 1.03g.At 70 ℃, rotating speed 640r/min is reaction 2h down.With 60 ℃ deionized waters washing 5 times, filtration under diminished pressure, at 110 ℃ of dry 4h down, 350 ℃ of following roasting 3h (heating rate be 3 ℃/min) obtain the ternary compound oxides catalyst.
Embodiment 18～20
The preparation method of embodiment 18～20 is identical with embodiment 17, and the amount of NaOH changes 6g respectively into, 5.68g, and 5.6g, zirconyl chloride solution change 5ml, 1ml, 0.1ml respectively into.
The catalysis CO conversion ratio of embodiment 17～20 catalyst is seen table 5.
Table 5 (%)
Claims (10)
1. the ternary compound oxides catalyst of carbon monoxide oxidation is characterized in that it consists of CuO-CeO-M, and M is Co, Ni, Zn, Mg, at least a in the Zr metal oxide; The mol ratio of each component content of catalyst is CuO: CeO: M=20: 80: (0.1～20).
2. the ternary compound oxides catalyst of carbon monoxide oxidation as claimed in claim 1 the preparation method, it is characterized in that may further comprise the steps:
1) prepare the precursor solution of CuO, CeO and M metal oxide respectively, press the catalyst component proportioning and mix, mixed liquor A;
2) the preparation precipitant solution joins mixed liquor A in the precipitant solution after the heating, gets mixed liquid B;
3) in mixed liquid B, add the surfactant reaction, get precipitated liquid;
4) with the washing of the precipitated liquid of step 3) gained, filtration under diminished pressure, drying, roasting obtains the ternary compound oxides catalyst of carbon monoxide oxidation.
3. the ternary compound oxides catalyst of carbon monoxide oxidation as claimed in claim 1 the preparation method; It is characterized in that in step 1); The concentration of the precursor solution of said CuO metal oxide is 1mol/L; The concentration of the precursor solution of said CeO metal oxide is 1mol/L, and the concentration of the precursor solution of said M metal oxide is 1mol/L.
4. the ternary compound oxides catalyst of carbon monoxide oxidation as claimed in claim 1 the preparation method; It is characterized in that in step 1); The presoma of said CuO metal oxide is the nitrate of copper; The presoma of said CeO metal oxide is the nitrate of cerium, and the presoma of said M metal oxide is the nitrate of M metal.
5. the ternary compound oxides catalyst of carbon monoxide oxidation as claimed in claim 1 the preparation method, it is characterized in that in step 2) in, said precipitating reagent is selected from NaOH; The concentration of said precipitant solution is 0.1～0.4mol/L.
6. the ternary compound oxides catalyst of carbon monoxide oxidation as claimed in claim 1 the preparation method, it is characterized in that in step 2) in, the temperature of said heating is 40～70 ℃.
7. the ternary compound oxides catalyst of carbon monoxide oxidation as claimed in claim 1 the preparation method, it is characterized in that in step 2) in, said join mixed liquor A in the precipitant solution after, regulating pH is 8.5～10.
8. the ternary compound oxides catalyst of carbon monoxide oxidation as claimed in claim 1 the preparation method; It is characterized in that in step 3); Said surfactant is selected from L-glutamic acid, and the mol ratio of the presoma of said surfactant and metal oxide is (0.007～0.06): 10.
9. the ternary compound oxides catalyst of carbon monoxide oxidation as claimed in claim 1 the preparation method, it is characterized in that in step 3) the temperature of said reaction is 40～70 ℃, the time of reaction is 1～3h.
10. the ternary compound oxides catalyst of carbon monoxide oxidation as claimed in claim 1 the preparation method, it is characterized in that in step 4) the temperature of said drying is 80～120 ℃, the dry time is 4～8h; The temperature of said roasting is 300～600 ℃, and the time of roasting is 3～6h.
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| CN104475114A (en) * | 2014-11-19 | 2015-04-01 | 上海化工研究院 | Copper-zinc-cerium-based catalyst for low-temperature deep removal of carbon monoxide and preparation method and application of catalyst |
| CN106378142A (en) * | 2016-08-30 | 2017-02-08 | 上海化工研究院 | Catalyst for removing alkene material flow impurity through deep purification at room temperature, preparation method and application thereof |
| CN108745345A (en) * | 2018-06-20 | 2018-11-06 | 杭州同久净颢科技有限责任公司 | A kind of no vanadium denitration catalyst and preparation method thereof |
| CN109603837A (en) * | 2019-01-18 | 2019-04-12 | 中国科学院青岛生物能源与过程研究所 | A kind of preparation method of the Cu/Ce/Co catalyst for furfural liquid-phase hydrogenatin |
| CN111185181A (en) * | 2020-01-08 | 2020-05-22 | 北京机械设备研究所 | Acetic acid catalytic oxidation amorphous catalyst, preparation method and catalytic oxidation process |
| CN113134358A (en) * | 2020-01-20 | 2021-07-20 | 中大汇智源创(北京)科技有限公司 | Water-resistant carbon monoxide catalyst and preparation method thereof |
| CN115337931A (en) * | 2022-08-20 | 2022-11-15 | 山东亮剑环保新材料有限公司 | Preparation method of rare earth composite catalyst for degrading organic pollutants |
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2011
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| CN106378142A (en) * | 2016-08-30 | 2017-02-08 | 上海化工研究院 | Catalyst for removing alkene material flow impurity through deep purification at room temperature, preparation method and application thereof |
| CN106378142B (en) * | 2016-08-30 | 2019-09-27 | 上海化工研究院有限公司 | The catalyst of room temperature deep purifying removing olefin stream impurity and its preparation and application |
| CN108745345A (en) * | 2018-06-20 | 2018-11-06 | 杭州同久净颢科技有限责任公司 | A kind of no vanadium denitration catalyst and preparation method thereof |
| CN109603837A (en) * | 2019-01-18 | 2019-04-12 | 中国科学院青岛生物能源与过程研究所 | A kind of preparation method of the Cu/Ce/Co catalyst for furfural liquid-phase hydrogenatin |
| CN109603837B (en) * | 2019-01-18 | 2021-12-31 | 中国科学院青岛生物能源与过程研究所 | Preparation method of Cu/Ce/Co catalyst for furfural liquid-phase hydrogenation |
| CN111185181A (en) * | 2020-01-08 | 2020-05-22 | 北京机械设备研究所 | Acetic acid catalytic oxidation amorphous catalyst, preparation method and catalytic oxidation process |
| CN111185181B (en) * | 2020-01-08 | 2023-02-03 | 北京机械设备研究所 | Acetic acid catalytic oxidation amorphous catalyst, preparation method and catalytic oxidation process |
| CN113134358A (en) * | 2020-01-20 | 2021-07-20 | 中大汇智源创(北京)科技有限公司 | Water-resistant carbon monoxide catalyst and preparation method thereof |
| CN115337931A (en) * | 2022-08-20 | 2022-11-15 | 山东亮剑环保新材料有限公司 | Preparation method of rare earth composite catalyst for degrading organic pollutants |
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Application publication date: 20120118 |