CN105727950B - A kind of Oxidation of Carbon Monoxide catalyst and preparation method thereof - Google Patents
A kind of Oxidation of Carbon Monoxide catalyst and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of Oxidation of Carbon Monoxide catalyst, including carrier and the active component being carried on carrier, and the carrier is CeO2And Al2O3Composite oxides, CeO2And Al2O3Composite oxides in Ce and Al molar ratio be not more than 3;The active component is Pd and La, and the quality that the quality of Pd is 0.1%~2.5%, La of catalyst quality is the 0.3%~5.6% of catalyst quality.In addition, the invention also discloses the preparation methods of the catalyst.The present invention uses CeO2And Al2O3Composite oxides as carrier, with larger specific surface area, be conducive to improve dispersion degree of the Pd metals on carrier, carrier itself has the Oxidation of Carbon Monoxide activity that more oxygen vacancies position is conducive to improve catalyst, in addition, using the synergistic effect of Ce and Pd, be conducive to the Oxidation of Carbon Monoxide activity for further increasing catalyst.
Description
Technical field
The invention belongs to catalyst preparation technical fields, and in particular to a kind of Oxidation of Carbon Monoxide catalyst and its preparation
Method.
Background technology
CO room-temperature catalytic oxidation processes are related to eliminating environmental pollution, air purification, CO2Purification for gas, CO are passed in laser
The elimination etc. of CO in sensor, breathing mask and closed system.But in low temperature, especially there is condition existing for vapor
Under, there is the shortcomings of activity is low, water repelling property is poor in many catalyst, its use is made to be restricted.Therefore, have under cryogenic conditions
There are the CO oxidation catalysts of high activity and stability to become the hot spot of research.
The forward position of CO low-temperature catalytic oxidations research field is concentrated mainly on the following aspects at present:Optimize the system of catalyst
Preparation Method, improve have catalyst performance, further investigate catalyst the mechanism of action and design can commercial Application catalyst.
In the preparation method research of optimization catalyst, there are many researchs to be absorbed in and constantly look for new carrier or the original carrier of change
To improve catalytic activity.Heterogeneous reaction carries out under relatively severe condition mostly, and carrier often occurs and the sintering of active phase is existing
As shortening the service life of catalyst.Therefore catalyst carrier must have high mechanical strength, stability is good, heat transfer is good
The features such as not being sintered at reaction conditions, find a kind of novel catalyst carrier of good properties have it is highly important
Meaning.Common catalyst carrier mainly has aluminium oxide, silica gel, activated carbon, ceramic honey comb, metal alloy and zeolite etc..But
Using different nCe/nAl than CeO2/Al2O3Composite oxides are that carrier prepares Pd based carbon monoxide oxidation catalysts and applies
Related patents and document report are yet there are no in Oxidation of Carbon Monoxide reaction.
Invention content
Technical problem to be solved by the present invention lies in view of the above shortcomings of the prior art, provide a kind of carbon monoxide oxygen
Change catalyst.The catalyst uses CeO2And Al2O3Composite oxides as carrier, there is larger specific surface area, favorably
In improving dispersion degree of the Pd metals on carrier, carrier itself has the carbon monoxide that more oxygen vacancies position is conducive to improve catalyst
Oxidation activity is conducive to the Oxidation of Carbon Monoxide activity for further increasing catalyst in addition, using the synergistic effect of Ce and Pd.
Catalyst has higher catalytic activity and stability, is 10000h in gas space velocity-1~30000h-1, CO contents are 500ppm
Under the reaction condition of~2000ppm, CO effectively catalysis oxidations, active duration can be not less than to 300min, and can letter
Single regeneration is reused.
In order to solve the above technical problems, the technical solution adopted by the present invention is:A kind of Oxidation of Carbon Monoxide catalyst,
It is characterized in that, including carrier and the active component being carried on carrier, the carrier is CeO2And Al2O3Composite oxides,
CeO2And Al2O3Composite oxides in Ce and Al molar ratio be not more than 3;The active component is Pd and La, and the quality of Pd is
The quality of 0.1%~2.5%, La of catalyst quality is the 0.3%~5.6% of catalyst quality.
A kind of above-mentioned Oxidation of Carbon Monoxide catalyst, which is characterized in that the CeO2And Al2O3Composite oxides
The molar ratio 0.05~1 of middle Ce and Al, the quality that the quality of Pd is 1%~2.5%, La of catalyst quality are catalyst quality
0.5%~3%.
A kind of above-mentioned Oxidation of Carbon Monoxide catalyst, which is characterized in that the CeO2And Al2O3Composite oxides
The molar ratio 0.2 of middle Ce and Al, the quality that the quality of Pd is 2%, La of catalyst quality are the 1% of catalyst quality.
In addition, the present invention also provides a kind of methods preparing above-mentioned Oxidation of Carbon Monoxide catalyst, which is characterized in that
Include the following steps:
Step 1: by Al (NO3)3With Ce (NO3)3It is dissolved in deionized water, obtains Al (NO3)3With Ce (NO3)3Mixing
The mixed solution is placed in precipitation reaction kettle by solution, and heating water bath is to 70 DEG C~90 DEG C, then under agitation to mixed
It is 8.0~9.0 to close the pH value that ammonium hydroxide is added dropwise to mixed solution in solution, is filtered after standing aging 1h~3h, obtains filter cake;
Step 2: being drained after filter cake described in step 1 is washed with deionized, then done at 100 DEG C~120 DEG C
Dry 10h~for 24 hours, then the filter cake after drying is roasted into 2h~3h at 400 DEG C~500 DEG C, obtain CeO2And Al2O3Composite oxygen
Compound;
Step 3: by H2PdCl6Solution and lanthanum nitrate aqueous solution are uniformly mixed, and obtain maceration extract;
Step 4: by CeO described in step 22And Al2O3Composite oxides be placed in maceration extract described in step 3 and soak
Stain 2h~filter afterwards for 24 hours, by the solid being obtained by filtration at 100 DEG C~120 DEG C dry 10h~for 24 hours, then by consolidating after drying
Body roasts 2h~3h at 400 DEG C~500 DEG C, obtains catalyst precursor;
Step 5: restored to catalyst precursor described in step 4 with hydrogen, Oxidation of Carbon Monoxide is obtained with urging
Agent.
Above-mentioned method, which is characterized in that H described in step 32PdCl6A concentration of 0.01g/mL of Pd in solution~
0.1g/mL, a concentration of 0.1M~1.5M of lanthanum nitrate aqueous solution.
Above-mentioned method, which is characterized in that the flow of hydrogen described in step 5 is 100mL/min~200mL/min, also
Former temperature is 200 DEG C~300 DEG C, and the time of reduction is 1h~2h.
Compared with the prior art, the present invention has the following advantages:
1, the present invention uses CeO2And Al2O3Composite oxides as carrier, there is larger specific surface area, be conducive to
Dispersion degree of the Pd metals on carrier is improved, in addition, carrier itself has the oxygen that more oxygen vacancies position is conducive to improve catalyst
Change oxidation of coal activity.
2, the present invention uses CeO2And Al2O3Composite oxides as carrier, using the synergistic effect of Ce and Pd, favorably
In the Oxidation of Carbon Monoxide activity for further increasing catalyst.
3, catalyst preparation process of the invention is simple, and noble-metal-supported amount is low, and catalyst activity is high, complete conversion temperature
It is low, there is apparent application value.
4, catalyst of the invention has higher catalytic activity and stability, is 10000h in gas space velocity-1~
30000h-1, CO contents are under the reaction condition of 500ppm~2000ppm, can be by CO effectively catalysis oxidations, active duration
Not less than 300min, and can simple regeneration reuse.
Below by embodiment, technical scheme of the present invention will be described in further detail.
Specific implementation mode
Embodiment 1
The catalyst of the present embodiment includes carrier and the active component that is carried on carrier, and the carrier is CeO2And Al2O3
Composite oxides, CeO2And Al2O3Composite oxides in Ce and Al molar ratio be 0.2;The active component be Pd and
The quality of La, Pd are that the quality of 2%, La of catalyst quality is the 1% of catalyst quality.
The preparation method of the catalyst of the present embodiment includes the following steps:
Step 1: by Al (NO3)3With Ce (NO3)3According to 1:0.2 molar ratio is dissolved in deionized water, obtains Al
(NO3)3With Ce (NO3)3Mixed solution, the mixed solution is placed in precipitation reaction kettle, heating water bath is to 80 DEG C, then
It is under agitation 8.5 to the pH value of mixed solution to mixed solution and dripping ammonium hydroxide, filters, filtered after standing aging 2h
Cake;
Step 2: being drained after filter cake described in step 1 is washed with deionized, 15h is then dried at 110 DEG C, then
Filter cake after drying is roasted into 2.5h at 450 DEG C, obtains CeO2And Al2O3Composite oxides;
Step 3: by 20mL H2PdCl6Solution and 72mL lanthanum nitrate aqueous solutions are uniformly mixed, and obtain maceration extract;It is described
H2PdCl6A concentration of 0.1g/mL of Pd in solution, a concentration of 0.1M of lanthanum nitrate aqueous solution;
Step 4: by CeO described in 97g step 22And Al2O3Composite oxides be placed in maceration extract described in step 3
It is filtered after middle dipping 20h, the solid being obtained by filtration is dried into 18h at 110 DEG C, then by the solid after drying at 450 DEG C
2.5h is roasted, catalyst precursor is obtained;
Step 5: restored to catalyst precursor described in step 4 with hydrogen, Oxidation of Carbon Monoxide is obtained with urging
Agent;The flow of the hydrogen is 150mL/min, and the temperature of reduction is 250 DEG C, and the time of reduction is 2h.
Catalyst manufactured in the present embodiment is applied in CO catalytic oxidations, specific method is:Accurately 1g is weighed to urge
The catalyst weighed is placed in quartzy straight reaction tube constant temperature zone by agent, reaction tube is loaded in reaction heating furnace, to reaction
The gaseous mixture (volume content of CO is 500ppm~2000ppm in gaseous mixture) that CO and air are passed through in pipe is reacted, gas
Air speed is 10000h-1~30000h-1, product analysis is using the gas-chromatography automatic sampling analysis equipped with methane reborner, record
The concentration of CO at different temperatures evaluates the activity of catalyst, minimum complete conversion temperature with the minimum complete conversion temperature of CO
The time of lower continuous transformation investigates catalyst stability.The results show that catalyst manufactured in the present embodiment has excellent catalysis
Performance, under above-mentioned evaluation condition, under conditions of conversion temperature is 100 DEG C, CO can be converted completely, and can continuously be made
Use 600min.The restoring operation that step 5 is repeated after catalyst inactivation regenerates catalyst, you can restores catalytic activity.
Embodiment 2
The catalyst of the present embodiment includes carrier and the active component that is carried on carrier, and the carrier is CeO2And Al2O3
Composite oxides, CeO2And Al2O3Composite oxides in Ce and Al molar ratio be 3;The active component is Pd and La,
The quality of Pd is that the quality of 2.5%, La of catalyst quality is the 0.3% of catalyst quality.
The preparation method of the catalyst of the present embodiment includes the following steps:
Step 1: by Al (NO3)3With Ce (NO3)3According to 1:3 molar ratio is dissolved in deionized water, obtains Al (NO3)3
With Ce (NO3)3Mixed solution, the mixed solution is placed in precipitation reaction kettle, then heating water bath is being stirred to 90 DEG C
Under the conditions of to mixed solution and dripping ammonium hydroxide to the pH value of mixed solution be 8.0, filtered after standing aging 3h, obtain filter cake;
Step 2: being drained after filter cake described in step 1 is washed with deionized, 10h is then dried at 120 DEG C, then
Filter cake after drying is roasted into 2h at 500 DEG C, obtains CeO2And Al2O3Composite oxides;
Step 3: by 250mL H2PdCl6Solution and 1.44mL lanthanum nitrate aqueous solutions are uniformly mixed, and obtain maceration extract;It is described
H2PdCl6A concentration of 0.01g/mL of Pd in solution, a concentration of 1.5M of lanthanum nitrate aqueous solution;
Step 4: by CeO described in 97.2g step 22And Al2O3Composite oxides be placed in described in step 3 and impregnate
It is filtered after impregnating 2h in liquid, the solid being obtained by filtration is dried at 100 DEG C for 24 hours, then by the solid after drying at 400 DEG C
3h is roasted, catalyst precursor is obtained;
Step 5: restored to catalyst precursor described in step 4 with hydrogen, Oxidation of Carbon Monoxide is obtained with urging
Agent;The flow of the hydrogen is 100mL/min, and the temperature of reduction is 200 DEG C, and the time of reduction is 2h.
Catalyst manufactured in the present embodiment is applied in CO catalytic oxidations, specific method is:Accurately 1g is weighed to urge
The catalyst weighed is placed in quartzy straight reaction tube constant temperature zone by agent, reaction tube is loaded in reaction heating furnace, to reaction
The gaseous mixture (volume content of CO is 500ppm~2000ppm in gaseous mixture) that CO and air are passed through in pipe is reacted, gas
Air speed is 10000h-1~30000h-1, product analysis is using the gas-chromatography automatic sampling analysis equipped with methane reborner, record
The concentration of CO at different temperatures evaluates the activity of catalyst, minimum complete conversion temperature with the minimum complete conversion temperature of CO
The time of lower continuous transformation investigates catalyst stability.The results show that catalyst manufactured in the present embodiment has excellent catalysis
Performance, under above-mentioned evaluation condition, under conditions of conversion temperature is 120 DEG C, CO can be converted completely, and can continuously be made
Use 560min.The restoring operation that step 5 is repeated after catalyst inactivation regenerates catalyst, you can restores catalytic activity.
Embodiment 3
The catalyst of the present embodiment includes carrier and the active component that is carried on carrier, and the carrier is CeO2And Al2O3
Composite oxides, CeO2And Al2O3Composite oxides in Ce and Al molar ratio be 2;The active component is Pd and La,
The quality of Pd is that the quality of 0.1%, La of catalyst quality is the 5.6% of catalyst quality.
The preparation method of the catalyst of the present embodiment includes the following steps:
Step 1: by Al (NO3)3With Ce (NO3)3According to 1:2 molar ratio is dissolved in deionized water, obtains Al (NO3)3
With Ce (NO3)3Mixed solution, the mixed solution is placed in precipitation reaction kettle, then heating water bath is being stirred to 70 DEG C
Under the conditions of to mixed solution and dripping ammonium hydroxide to the pH value of mixed solution be 9.0, filtered after standing aging 1h, obtain filter cake;
Step 2: being drained after filter cake described in step 1 is washed with deionized, then dried for 24 hours at 100 DEG C, then
Filter cake after drying is roasted into 3h at 400 DEG C, obtains CeO2And Al2O3Composite oxides;
Step 3: by 2mL H2PdCl6Solution and 403mL lanthanum nitrate aqueous solutions are uniformly mixed, and obtain maceration extract;It is described
H2PdCl6A concentration of 0.05g/mL of Pd in solution, a concentration of 0.1M of lanthanum nitrate aqueous solution;
Step 4: by CeO described in 94.3g step 22And Al2O3Composite oxides be placed in described in step 3 and impregnate
It impregnates in liquid and filters afterwards for 24 hours, the solid being obtained by filtration is dried into 10h at 120 DEG C, then by the solid after drying at 500 DEG C
Lower roasting 2h, obtains catalyst precursor;
Step 5: restored to catalyst precursor described in step 4 with hydrogen, Oxidation of Carbon Monoxide is obtained with urging
Agent;The flow of the hydrogen is 200mL/min, and the temperature of reduction is 300 DEG C, and the time of reduction is 1h.
Catalyst manufactured in the present embodiment is applied in CO catalytic oxidations, specific method is:Accurately 1g is weighed to urge
The catalyst weighed is placed in quartzy straight reaction tube constant temperature zone by agent, reaction tube is loaded in reaction heating furnace, to reaction
The gaseous mixture (volume content of CO is 500ppm~2000ppm in gaseous mixture) that CO and air are passed through in pipe is reacted, gas
Air speed is 10000h-1~30000h-1, product analysis is using the gas-chromatography automatic sampling analysis equipped with methane reborner, record
The concentration of CO at different temperatures evaluates the activity of catalyst, minimum complete conversion temperature with the minimum complete conversion temperature of CO
The time of lower continuous transformation investigates catalyst stability.The results show that catalyst manufactured in the present embodiment has excellent catalysis
Performance, under above-mentioned evaluation condition, under conditions of conversion temperature is 130 DEG C, CO can be converted completely, and can continuously be made
Use 300min.The restoring operation that step 5 is repeated after catalyst inactivation regenerates catalyst, you can restores catalytic activity.
Embodiment 4
The catalyst of the present embodiment includes carrier and the active component that is carried on carrier, and the carrier is CeO2And Al2O3
Composite oxides, CeO2And Al2O3Composite oxides in Ce and Al mole be 1;The active component is Pd and La, Pd
Quality be the quality of 2.5%, La of catalyst quality be the 3% of catalyst quality.
The preparation method of the catalyst of the present embodiment includes the following steps:
Step 1: by Al (NO3)3With Ce (NO3)3According to 1:1 molar ratio is dissolved in deionized water, obtains Al (NO3)3
With Ce (NO3)3Mixed solution, the mixed solution is placed in precipitation reaction kettle, then heating water bath is being stirred to 90 DEG C
Under the conditions of to mixed solution and dripping ammonium hydroxide to the pH value of mixed solution be 8.5, filtered after standing aging 2h, obtain filter cake;
Step 2: being drained after filter cake described in step 1 is washed with deionized, then dried for 24 hours at 100 DEG C, then
Filter cake after drying is roasted into 2h at 450 DEG C, obtains CeO2And Al2O3Composite oxides;
Step 3: by 250mL H2PdCl6Solution and 21.6mL lanthanum nitrate aqueous solutions are uniformly mixed, and obtain maceration extract;It is described
H2PdCl6A concentration of 0.01g/mL of Pd in solution, a concentration of 1.0M of lanthanum nitrate aqueous solution;
Step 4: by CeO described in 94.5g step 22And Al2O3Composite oxides be placed in described in step 3 and impregnate
It is filtered after impregnating 10h in liquid, the solid being obtained by filtration is dried into 12h at 110 DEG C, then by the solid after drying at 450 DEG C
Lower roasting 2h, obtains catalyst precursor;
Step 5: restored to catalyst precursor described in step 4 with hydrogen, Oxidation of Carbon Monoxide is obtained with urging
Agent;The flow of the hydrogen is 150mL/min, and the temperature of reduction is 250 DEG C, and the time of reduction is 1.5h.
Catalyst manufactured in the present embodiment is applied in CO catalytic oxidations, specific method is:Accurately 1g is weighed to urge
The catalyst weighed is placed in quartzy straight reaction tube constant temperature zone by agent, reaction tube is loaded in reaction heating furnace, to reaction
The gaseous mixture (volume content of CO is 500ppm~2000ppm in gaseous mixture) that CO and air are passed through in pipe is reacted, gas
Air speed is 10000h-1~30000h-1, product analysis is using the gas-chromatography automatic sampling analysis equipped with methane reborner, record
The concentration of CO at different temperatures evaluates the activity of catalyst, minimum complete conversion temperature with the minimum complete conversion temperature of CO
The time of lower continuous transformation investigates catalyst stability.The results show that catalyst manufactured in the present embodiment has excellent catalysis
Performance, under above-mentioned evaluation condition, under conditions of conversion temperature is 110 DEG C, CO can be converted completely, and can continuously be made
Use 500min.The restoring operation that step 5 is repeated after catalyst inactivation regenerates catalyst, you can restores catalytic activity.
Embodiment 5
The catalyst of the present embodiment includes carrier and the active component that is carried on carrier, and the carrier is CeO2And Al2O3
Composite oxides, CeO2And Al2O3Composite oxides in Ce and Al molar ratio be 0.05;The active component be Pd and
The quality of La, Pd are that the quality of 1%, La of catalyst quality is the 0.5% of catalyst quality.
The preparation method of the catalyst of the present embodiment includes the following steps:
Step 1: by Al (NO3)3With Ce (NO3)3According to 1:0.05 molar ratio is dissolved in deionized water, obtains Al
(NO3)3With Ce (NO3)3Mixed solution, the mixed solution is placed in precipitation reaction kettle, heating water bath is to 80 DEG C, then
It is under agitation 8.0 to the pH value of mixed solution to mixed solution and dripping ammonium hydroxide, filters, filtered after standing aging 3h
Cake;
Step 2: being drained after filter cake described in step 1 is washed with deionized, 12h is then dried at 120 DEG C, then
Filter cake after drying is roasted into 3h at 400 DEG C, obtains CeO2And Al2O3Composite oxides;
Step 3: by 100mL H2PdCl6Solution and 36mL lanthanum nitrate aqueous solutions are uniformly mixed, and obtain maceration extract;It is described
H2PdCl6A concentration of 0.01g/mL of Pd in solution, a concentration of 0.1M of lanthanum nitrate aqueous solution;
Step 4: by CeO described in 98.5g step 22And Al2O3Composite oxides be placed in described in step 3 and impregnate
It is filtered after impregnating 20h in liquid, the solid being obtained by filtration is dried at 100 DEG C for 24 hours, then by the solid after drying at 400 DEG C
Lower roasting 3h, obtains catalyst precursor;
Step 5: restored to catalyst precursor described in step 4 with hydrogen, Oxidation of Carbon Monoxide is obtained with urging
Agent;The flow of the hydrogen is 200mL/min, and the temperature of reduction is 200 DEG C, and the time of reduction is 2h.
Catalyst manufactured in the present embodiment is applied in CO catalytic oxidations, specific method is:Accurately 1g is weighed to urge
The catalyst weighed is placed in quartzy straight reaction tube constant temperature zone by agent, reaction tube is loaded in reaction heating furnace, to reaction
The gaseous mixture (volume content of CO is 500ppm~2000ppm in gaseous mixture) that CO and air are passed through in pipe is reacted, gas
Air speed is 10000h-1~30000h-1, product analysis is using the gas-chromatography automatic sampling analysis equipped with methane reborner, record
The concentration of CO at different temperatures evaluates the activity of catalyst, minimum complete conversion temperature with the minimum complete conversion temperature of CO
The time of lower continuous transformation investigates catalyst stability.The results show that catalyst manufactured in the present embodiment has excellent catalysis
Performance, under above-mentioned evaluation condition, under conditions of conversion temperature is 110 DEG C, CO can be converted completely, and can continuously be made
Use 400min.The restoring operation that step 5 is repeated after catalyst inactivation regenerates catalyst, you can restores catalytic activity.
Embodiment 6
The catalyst of the present embodiment includes carrier and the active component that is carried on carrier, and the carrier is CeO2And Al2O3
Composite oxides, CeO2And Al2O3Composite oxides in Ce and Al molar ratio be 0.5;The active component be Pd and
The quality of La, Pd are that the quality of 2%, La of catalyst quality is the 2% of catalyst quality.
The preparation method of the catalyst of the present embodiment includes the following steps:
Step 1: by Al (NO3)3With Ce (NO3)3According to 1:0.5 molar ratio is dissolved in deionized water, obtains Al
(NO3)3With Ce (NO3)3Mixed solution, the mixed solution is placed in precipitation reaction kettle, heating water bath is to 90 DEG C, then
It is under agitation 8.0 to the pH value of mixed solution to mixed solution and dripping ammonium hydroxide, filters, filtered after standing aging 3h
Cake;
Step 2: being drained after filter cake described in step 1 is washed with deionized, 10h is then dried at 120 DEG C, then
Filter cake after drying is roasted into 2h at 500 DEG C, obtains CeO2And Al2O3Composite oxides;
Step 3: by 20mL H2PdCl6Solution and 144mL lanthanum nitrate aqueous solutions are uniformly mixed, and obtain maceration extract;It is described
H2PdCl6A concentration of 0.1g/mL of Pd in solution, a concentration of 0.1M of lanthanum nitrate aqueous solution;
Step 4: by CeO described in 96g step 22And Al2O3Composite oxides be placed in maceration extract described in step 3
It is filtered after middle dipping 2h, the solid being obtained by filtration is dried into 10h at 120 DEG C, then roasts the solid after drying at 500 DEG C
2h is burnt, catalyst precursor is obtained;
Step 5: restored to catalyst precursor described in step 4 with hydrogen, Oxidation of Carbon Monoxide is obtained with urging
Agent;The flow of the hydrogen is 100mL/min, and the temperature of reduction is 250 DEG C, and the time of reduction is 2h.
Catalyst manufactured in the present embodiment is applied in CO catalytic oxidations, specific method is:Accurately 1g is weighed to urge
The catalyst weighed is placed in quartzy straight reaction tube constant temperature zone by agent, reaction tube is loaded in reaction heating furnace, to reaction
The gaseous mixture (volume content of CO is 500ppm~2000ppm in gaseous mixture) that CO and air are passed through in pipe is reacted, gas
Air speed is 10000h-1~30000h-1, product analysis is using the gas-chromatography automatic sampling analysis equipped with methane reborner, record
The concentration of CO at different temperatures evaluates the activity of catalyst, minimum complete conversion temperature with the minimum complete conversion temperature of CO
The time of lower continuous transformation investigates catalyst stability.The results show that catalyst manufactured in the present embodiment has excellent catalysis
Performance, under above-mentioned evaluation condition, under conditions of conversion temperature is 110 DEG C, CO can be converted completely, and can continuously be made
Use 500min.The restoring operation that step 5 is repeated after catalyst inactivation regenerates catalyst, you can restores catalytic activity.
The above is only presently preferred embodiments of the present invention, not does any restrictions to the present invention, every according to invention skill
Art essence changes any simple modification, change and equivalent structure made by above example, still falls within the technology of the present invention
In the protection domain of scheme.
Claims (5)
1. a kind of Oxidation of Carbon Monoxide catalyst, which is characterized in that including carrier and the active component being carried on carrier, institute
It is CeO to state carrier2And Al2O3Composite oxides, CeO2And Al2O3Composite oxides in Ce and Al molar ratio 0.05~1;
The active component is Pd and La, and the quality that the quality of Pd is 1%~2.5%, La of catalyst quality is catalyst quality
0.5%~3%;
The preparation method of the Oxidation of Carbon Monoxide catalyst includes the following steps:
Step 1: by Al (NO3)3With Ce (NO3)3It is dissolved in deionized water, obtains Al (NO3)3With Ce (NO3)3Mixing it is molten
The mixed solution is placed in precipitation reaction kettle by liquid, and heating water bath is to 70 DEG C~90 DEG C, then under agitation to mixing
The pH value that ammonium hydroxide is added dropwise to mixed solution in solution is 8.0~9.0, is filtered after standing aging 1h~3h, obtains filter cake;
Step 2: being drained after filter cake described in step 1 is washed with deionized, 10h is then dried at 100 DEG C~120 DEG C
~for 24 hours, then the filter cake after drying roasted into 2h~3h at 400 DEG C~500 DEG C, obtain CeO2And Al2O3Composite oxides;
Step 3: by H2PdCl6Solution and lanthanum nitrate aqueous solution are uniformly mixed, and obtain maceration extract;
Step 4: by CeO described in step 22And Al2O3Composite oxides be placed in maceration extract described in step 3 and impregnate 2h
~filter afterwards for 24 hours, by the solid being obtained by filtration at 100 DEG C~120 DEG C dry 10h~for 24 hours, then the solid after drying is existed
2h~3h is roasted at 400 DEG C~500 DEG C, obtains catalyst precursor;
Step 5: being restored to catalyst precursor described in step 4 with hydrogen, Oxidation of Carbon Monoxide catalyst is obtained.
2. a kind of Oxidation of Carbon Monoxide catalyst according to claim 1, which is characterized in that the CeO2And Al2O3's
The molar ratio 0.2 of Ce and Al in composite oxides, the quality that the quality of Pd is 2%, La of catalyst quality are catalyst quality
1%.
3. a kind of method preparing Oxidation of Carbon Monoxide catalyst as claimed in claim 1 or 2, which is characterized in that including with
Lower step:
Step 1: by Al (NO3)3With Ce (NO3)3It is dissolved in deionized water, obtains Al (NO3)3With Ce (NO3)3Mixing it is molten
The mixed solution is placed in precipitation reaction kettle by liquid, and heating water bath is to 70 DEG C~90 DEG C, then under agitation to mixing
The pH value that ammonium hydroxide is added dropwise to mixed solution in solution is 8.0~9.0, is filtered after standing aging 1h~3h, obtains filter cake;
Step 2: being drained after filter cake described in step 1 is washed with deionized, 10h is then dried at 100 DEG C~120 DEG C
~for 24 hours, then the filter cake after drying roasted into 2h~3h at 400 DEG C~500 DEG C, obtain CeO2And Al2O3Composite oxides;
Step 3: by H2PdCl6Solution and lanthanum nitrate aqueous solution are uniformly mixed, and obtain maceration extract;
Step 4: by CeO described in step 22And Al2O3Composite oxides be placed in maceration extract described in step 3 and impregnate 2h
~filter afterwards for 24 hours, by the solid being obtained by filtration at 100 DEG C~120 DEG C dry 10h~for 24 hours, then the solid after drying is existed
2h~3h is roasted at 400 DEG C~500 DEG C, obtains catalyst precursor;
Step 5: being restored to catalyst precursor described in step 4 with hydrogen, Oxidation of Carbon Monoxide catalyst is obtained.
4. according to the method described in claim 3, it is characterized in that, H described in step 32PdCl6Pd's is a concentration of in solution
0.01g/mL~0.1g/mL, a concentration of 0.1M~1.5M of lanthanum nitrate aqueous solution.
5. according to the method described in claim 3, it is characterized in that, the flow of hydrogen described in step 5 be 100mL/min~
The temperature of 200mL/min, reduction are 200 DEG C~300 DEG C, and the time of reduction is 1h~2h.
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