CN101879454A - Catalyst for catalyzing and oxidizing carbon monoxide at low temperature and preparation method thereof - Google Patents
Catalyst for catalyzing and oxidizing carbon monoxide at low temperature and preparation method thereof Download PDFInfo
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- CN101879454A CN101879454A CN2010102330597A CN201010233059A CN101879454A CN 101879454 A CN101879454 A CN 101879454A CN 2010102330597 A CN2010102330597 A CN 2010102330597A CN 201010233059 A CN201010233059 A CN 201010233059A CN 101879454 A CN101879454 A CN 101879454A
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Abstract
The invention discloses a catalyst for catalyzing and oxidizing carbon monoxide at low temperature and a preparation method thereof. The catalyst comprises an active component Pd, additive Fe and a carrier, wherein the carrier is active carbon modified from chitosan; and the active component Pd and the additive Fe are loaded on the carrier. In the catalyst, the mass of the active component Pd is 0.5 to 3 percent of that of the carrier, and the mass of the additive Fe is 3 to 24 percent of that of the carrier. The preparation method of the catalyst comprises the following steps: adopting a step impregnation method, acidizing the active carbon, treating the acidized active carbon with chitosan solution, then sequentially soaking and absorbing the additive Fe and the active component Pd, filtering, washing and drying to obtain the catalyst. The catalyst is characterized by low precious metal content, high activity at low temperature, good moisture resistance property and the like.
Description
Technical field
The invention belongs to catalyst field, be specifically related to eliminate under a kind of low temperature the Catalysts and its preparation method of carbon monoxide.
Background technology
Carbon monoxide is a kind of typically inflammable, explosive, toxic compounds, is the primary pollutant in many industrial environments and the indoor air.The binding ability of carbon monoxide and human body hemoglobin is 250 times of oxygen, thereby can stop hemoglobin to carry the oxygen that absorbs to tissue.The content of carbon monoxide surpasses 30mg/m in air
3The time will be to the toxic effect of human body.Therefore, the elimination of carbon monoxide has important and practical meanings under the realization cryogenic conditions.In addition, the low temperature elimination of carbon monoxide also has very widely to be used, as: 1. manned enclosed system, as the elimination of micro CO in aircraft, submarine, the spacecraft module; 2. the gas breathing mask is used for the occasion that coal mining and fire incident etc. produce carbon monoxide; 3. the elimination of micro CO in the smoke from cigarette; 4. produce the occasion of carbon monoxide in the organic waste burning process; 5. gas purification is as the elimination of carbon monoxide in separated nitrogen from air, the oxygen; 6. elimination of micro CO etc. in the carbon dioxide gas laser.This shows that the low temperature elimination of carbon monoxide relates to a plurality of fields such as the energy, EHS.In numerous carbon monoxide removing methods, characteristics such as catalytic oxidation is low because of its operating temperature, burning usefulness height, environmental friendliness are considered to the most effective a kind of approach.
The catalyst that is used for the CO catalytic oxidation at present mainly contains three types: non-noble metal oxide type, perofskite type oxide type and noble metal type catalyst.
The non-noble metal oxide catalyst that is used for the CO low-temperature oxidation mainly is hopcalite (Hopcalite), and it is a kind of with CuO-MnO
xComposite oxide catalysts for main component, this catalyst is a kind of no-load build catalyst, under room temperature environment, can remove CO effectively, the Lattice Oxygen of catalyst surface is participated in reaction directly, with preferential adsorption on catalyst surface and the CO molecular reaction that is activated, the Lattice Oxygen omission that reaction causes is adsorbed in catalyst surface and becomes Lattice Oxygen by airborne oxygen and replenished, and so circulation just realizes the oxidation of CO.The advantage of this catalyst is that cost is lower, and shortcoming is that humidity-proof ability is poor, easily inactivation.Non-noble metal oxide Co
3O
4Also have higher CO low-temperature catalytic oxidation activity, it is to be predecessor with the cobalt nitrate, adopts NaOH to make precipitating reagent, and (DBS) could obtain high low temperature active as surfactant but use dodecyl sodium sulfate in the preparation process.Co by the preparation of precipitation oxidizing process
3O
4The minimum temperature that catalyst is used for the CO catalytic oxidation is 98 ℃, and needs to add H in the preparation process
2O
2As oxidant.
For the CO catalytic oxidation, perofskite type oxide (ABO
3) catalyst also has more report.As LaCoO
3At 1%CO/2%O
2/ N
2In, air speed 120000h
-1Under the condition, the CO initiation temperature is 138 ℃.The disclosed perovskite-type rare-earth composite oxides of Chinese patent CN1058357A, directly loading on mullite is on the carrier of main thing phase, is 1.0% in CO concentration, air speed is 60000h
-1Condition under, the conversion ratio of CO reached 99% when reaction temperature was 250 ℃.As seen, perofskite type oxide is used for the general higher reaction temperature of needs of CO catalytic oxidation.
Opposite with non-precious metal catalyst, the activity of noble metal catalysts such as palladium and stability are better, but the cost height.Pd/SnO as the disclosed a kind of carbon monoxide oxidation of US4490482
2Catalyst, since the content height of precious metal palladium, the preparation cost height, and can't use in industrial scale.In recent years, people begin to pay close attention to mutual synergy between noble metal and some transition metal to improving catalyst performance, reduce bullion content and reduce catalyst cost aspect role, and this helps the scale of catalyst to use.As the Pd-Ni/SnO that CN1053017 reported
2Catalyst, the Pd/C catalyst that auxiliary agents such as the disclosed Li of CN1583258, K, P, V improve etc.But this class Preparation of catalysts all adopts single carrier at present, and the active component skewness of its load causes the not high and unstable properties of its activity, thereby limited its application.
Summary of the invention
It is low to the purpose of this invention is to provide a kind of bullion content, at low temperatures to the high Catalysts and its preparation method of catalyzing carbon monoxide oxidation efficiency in the environment.
Catalyst provided by the present invention is made up of active component Pd, auxiliary agent Fe and carrier, and wherein, described carrier is chitin modified active carbon; Described active component Pd and auxiliary agent Fe load on the described carrier.
In the described catalyst, the quality of active component Pd is the 0.5%-3% of described carrier quality, is preferably 0.5%-2%, specifically can be 0.5%, 1% or 2%; The quality of auxiliary agent Fe is the 3%-24% of described carrier quality, is preferably 3%-12%, specifically can be 3%, 6% or 12%.
Described chitin modified active carbon is made up of shitosan and active carbon, and wherein, the mass ratio of shitosan and activated carbon is 1: 5-1: 40, be preferably 1: 10-1: 20.
The Preparation of catalysts method of catalyzing and oxidizing carbon monoxide at low temperature provided by the present invention comprises the steps:
(1) the solubility divalent iron salt is mixed with perferrite solution; Adopt the equi-volume impregnating active carbon that described carrier is chitin modified to place described perferrite solution dipping 2-8 hour, filter then, wash, 60 ℃ of-80 ℃ of oven dry, obtain the active carbon of load auxiliary agent Fe;
(2) solubility divalence palladium salt is mixed with the palladium saline solution; Adopt equi-volume impregnating that the active carbon of the load auxiliary agent Fe of step 1) preparation was placed described palladium saline solution dipping 2-8 hour, filter then, wash, 60 ℃ of-80 ℃ of oven dry, obtain described catalyst.
Wherein, described in the step (1) in the perferrite solution concentration of ferrous ion be 3mg/ml-12mg/ml; The described chitin modified active carbon and the mass volume ratio 1g of perferrite solution: (5-10) ml.
Described in the step (2) in the palladium saline solution concentration of divalence palladium ion be 0.25mg/ml-1.5mg/ml; The active carbon of described load auxiliary agent Fe and the mass volume ratio of described palladium saline solution are 1g: (5-20) ml.
Described soluble ferric iron salt specifically can be FeCl
2Or FeSO
47H
2O, described soluble palladium salt specifically can be PdCl
2Or H
2PdCl
4
Used chitin modified active carbon can prepare according to following method among the present invention: shitosan is dissolved in the acetum that mass concentration is 1%-3%, be mixed with the chitosan-acetic acid solution that chitosan mass concentration is 0.5%-1%, to be the 5%-10% nitric acid dousing through mass concentration then, washing, 105 ℃ (this temperature is the charcoal treatment temperature of using always, helping activated carbon surface under this temperature and form active group) active carbon after oven dry is handled put into the chitosan-acetic acid solution dipping prepared 2-3 hour, filter, 60 ℃ of-80 ℃ of oven dry promptly obtain chitin modified active carbon.
Compare with existing catalyst for eliminating carbon monoxide, the present invention has the following advantages:
(1) under the low temperature (40 ℃-80 ℃) to micro CO catalytic oxidation activity height in the air, long service life, moisture resistance properties is good;
(2) this catalyst carries out the modification processing by chitosan solution to carrier active carbon, has overcome the uneven problem of activity of such catalysts central distribution of single preparing carriers, has improved the performance of catalyst;
(3) add an amount of auxiliary agent Fe element in this catalyst, made Pd content reduction in the catalyst, overcome catalyst cost height, the narrow limitation of range of application;
(4) this catalyst preparation process mild condition, method is simple, and handling safety is easy to implement.
The specific embodiment
The present invention will be described below by specific embodiment, but the present invention is not limited thereto.
Experimental technique described in the following embodiment if no special instructions, is conventional method; Described reagent and material if no special instructions, all can obtain from commercial channels.
Among the following embodiment used active carbon if no special instructions, being with mass concentration is that 10% salpeter solution soaks, washs the active carbon after being neutral, oven dry and handling to filtrate.
The performance evaluation experiment of the carbon monoxide under low temperature catalyst that following embodiment is prepared is carried out in the anaerobism pipe, take by weighing a certain amount of catalyst in the anaerobism pipe, inject the CO gas of certain volume then, react certain hour, utilize the concentration of CO gas in the gas chromatography detector tube.Chromatographic condition: GC-14C day island proper functional activities of the body fluid chromatography, detector: TCD; Column temperature: 50 ℃; Injector temperature: 100 ℃; Detector temperature: 100 ℃; Chromatographic column: TDX-01,1m; Sample size: 1mL.
The CO amount of cancellation can calculate by following formula:
In the formula,
q
0: the primary quantity of CO (mg);
q
1: the amount (mg) of reaction back CO;
M: the quality of catalyst (g);
Q: amount of cancellation (mg/g).
Embodiment 1, carbon monoxide under low temperature Preparation of catalysts
1) accurately takes by weighing the 0.1g shitosan, be dissolved in the 20mL mass concentration and be in 2% the acetum, be prepared into concentration and be 0.5% chitosan solution; In above-mentioned chitosan solution, add the active carbon of 2g then through acidifying, 30 ℃ of 2h that vibrate down, filtration, 60 ℃ of oven dry down obtain chitin modified active carbon (carrier), and wherein the mass ratio of shitosan and active carbon is 1: 20.
2) get Fe
2+Concentration is the salting liquid 20mL of 6mg/mL, adds the above-mentioned active carbon of handling through chitosan solution of 2g, 30 ℃ of oscillating reactions 8h, filtration, washing, 60 ℃ of oven dry.
3) get Pd
2+Concentration is the salting liquid 10mL of 1mg/mL, adds the above-mentioned composite that contains Fe of 2g, 30 ℃ of oscillating reactions 8h, and filtration, washing, 60 ℃ of oven dry place drier standby.The quality of Pd is 0.5% of a carrier quality in this product, and the quality of Fe is 6% of a carrier quality.
The catalyst of getting the 0.05g prepared fresh injects the CO gas of 1mL in the anaerobism pipe of 25mL, 60 ℃ of following static reaction 5min, and recording catalyst is 14.98mg.g to the removal amount of CO
-1, clearance is 59.9%.
Embodiment 2, carbon monoxide under low temperature Preparation of catalysts
1) accurately takes by weighing the 0.1g shitosan, be dissolved in the 20mL mass concentration and be in 2% the acetum, be prepared into concentration and be 0.5% chitosan solution; In above-mentioned chitosan solution, add the active carbon of 2g then through acidifying, 30 ℃ of 2h that vibrate down, filtration, 60 ℃ of oven dry down obtain chitin modified active carbon (carrier), and wherein the mass ratio of shitosan and active carbon is 1: 20.
2) get Fe
2+Concentration is the salting liquid 10mL of 6mg/mL, adds the above-mentioned active carbon of handling through chitosan solution of 2g, 30 ℃ of oscillating reactions 8h, filtration, washing, 60 ℃ of oven dry.
3) get Pd
2+Concentration is the salting liquid 20mL of 1mg/mL, adds the above-mentioned composite that contains Fe of 2g, 30 ℃ of oscillating reactions 8h, and filtration, washing, 60 ℃ of oven dry place drier standby.The quality of Pd is 1% of a carrier quality in this product, and the quality of Fe is 3% of a carrier quality.
The catalyst of getting the 0.05g prepared fresh injects the CO gas of 1mL in the anaerobism pipe of 25mL, 60 ℃ of following static reaction 5min, and recording catalyst is 18.28mg.g to the removal amount of CO
-1, clearance is 73.1%.
Embodiment 3, carbon monoxide under low temperature Preparation of catalysts
1) accurately takes by weighing the 0.1g shitosan, be dissolved in the 20mL mass concentration and be in 2% the acetum, be prepared into concentration and be 0.5% chitosan solution; In above-mentioned chitosan solution, add the active carbon of 2g then through acidifying, 30 ℃ of 2h that vibrate down, filtration, 60 ℃ of oven dry down obtain chitin modified active carbon (carrier), and wherein the mass ratio of shitosan and active carbon is 1: 20.
2) get Fe
2+Concentration is the salting liquid 20mL of 6mg/mL, adds the above-mentioned active carbon of handling through chitosan solution of 2g, 30 ℃ of oscillating reactions 8h, filtration, washing, 60 ℃ of oven dry.
3) get Pd then
2+Concentration is the salting liquid 20mL of 1mg/mL, adds the above-mentioned composite that contains Fe of 2g, 30 ℃ of oscillating reactions 8h, and filtration, washing, 60 ℃ of oven dry place drier standby.The quality of Pd is 1% of a carrier quality in this product, and the quality of Fe is 6% of a carrier quality.
The catalyst of getting the 0.05g prepared fresh injects the CO gas of 1mL in the anaerobism pipe of 25mL, 40 ℃ of following static reaction 5min, and recording catalyst is 6.15mg.g to the removal amount of CO
-1, clearance is 24.6%.
Embodiment 4, carbon monoxide under low temperature Preparation of catalysts
1) accurately takes by weighing the 0.1g shitosan, be dissolved in the 20mL mass concentration and be in 2% the acetum, be prepared into concentration and be 0.5% chitosan solution; In above-mentioned chitosan solution, add the active carbon of 2g then through acidifying, 30 ℃ of 2h that vibrate down, filtration, 60 ℃ of oven dry down obtain chitin modified active carbon (carrier), and wherein the mass ratio of shitosan and active carbon is 1: 20.
2) get Fe
2+Concentration is the salting liquid 20mL of 6mg/mL, adds the above-mentioned active carbon of handling through chitosan solution of 2g, 30 ℃ of oscillating reactions 8h, filtration, washing, 60 ℃ of oven dry.
3) get Pd then
2+Concentration is the salting liquid 20mL of 1mg/mL, adds the above-mentioned composite that contains Fe of 2g, 30 ℃ of oscillating reactions 8h, and filtration, washing, 60 ℃ of oven dry place drier standby.The quality of Pd is 1% of a carrier quality in this product, and the quality of Fe is 6% of a carrier quality.
The catalyst of getting the 0.05g prepared fresh injects the CO gas of 1mL in the anaerobism pipe of 25mL, 60 ℃ of following static reaction 5min, and recording catalyst is 20.27mg.g to the removal amount of CO
-1, clearance is 81.1%.
Embodiment 5, carbon monoxide under low temperature Preparation of catalysts
1) accurately takes by weighing the 0.1g shitosan, be dissolved in the 20mL mass concentration and be in 2% the acetum, be prepared into concentration and be 0.5% chitosan solution; In above-mentioned chitosan solution, add the active carbon of 2g then through acidifying, 30 ℃ of 2h that vibrate down, filtration, 60 ℃ of oven dry down obtain chitin modified active carbon (carrier), and wherein the mass ratio of shitosan and active carbon is 1: 20.
2) get Fe
2+Concentration is the salting liquid 20mL of 6mg/mL, adds the above-mentioned active carbon of handling through chitosan solution of 2g, 30 ℃ of oscillating reactions 8h, filtration, washing, 60 ℃ of oven dry.
3) get Pd then
2+Concentration is the salting liquid 40mL of 1mg/mL, adds the above-mentioned composite that contains Fe of 2g, 30 ℃ of oscillating reactions 8h, and filtration, washing, 60 ℃ of oven dry place drier standby.The quality of Pd is 2% of a carrier quality in this product, and the quality of Fe is 6% of a carrier quality.
The catalyst of getting the 0.05g prepared fresh injects the CO gas of 1mL in the anaerobism pipe of 25mL, 60 ℃ of following static reaction 5min, and recording catalyst is 24.02mg.g to the removal amount of CO
-1, clearance is 96.1%.
Claims (9)
1. the catalyst of a catalyzing and oxidizing carbon monoxide at low temperature is made up of active component Pd, auxiliary agent Fe and carrier, and wherein, described carrier is chitin modified active carbon; Described active component Pd and auxiliary agent Fe load on the described carrier.
2. catalyst according to claim 1 is characterized in that: in the described catalyst, the quality of active component Pd is the 0.5%-3% of described carrier quality, is preferably 1%-2%; The quality of auxiliary agent Fe is the 3%-24% of described carrier quality, is preferably 3%-12%.
3. catalyst according to claim 1 and 2 is characterized in that: described chitin modified active carbon is made up of shitosan and active carbon, and wherein, the mass ratio of shitosan and activated carbon is 1: 5-1: 40, be preferably 1: 10-1: 20.
4. according to arbitrary described catalyst among the claim 1-3, it is characterized in that: described chitin modified active carbon prepares according to following method: shitosan is dissolved in the acetum that mass concentration is 1%-3%, be mixed with the chitosan-acetic acid solution that chitosan mass concentration is 0.5%-1%, to put into the chitosan-acetic acid solution of being prepared through the active carbon after mass concentration is 5%-10% nitric acid dousing, washing, oven dry processing then flooded 2-3 hour, filter, 60 ℃ of-80 ℃ of oven dry promptly obtain chitin modified active carbon.
5. according to arbitrary described catalyst among the claim 1-4, it is characterized in that: described catalyst is prepared according to the method that comprises the steps:
(1) the solubility divalent iron salt is mixed with perferrite solution; Adopt the equi-volume impregnating active carbon that described carrier is chitin modified to place described perferrite solution dipping 2-8 hour, filter then, wash, 60 ℃ of-80 ℃ of oven dry, obtain the active carbon of load auxiliary agent Fe;
(2) solubility divalence palladium salt is mixed with the palladium saline solution; Adopt equi-volume impregnating that the active carbon of the load auxiliary agent Fe of step 1) preparation was placed described palladium saline solution dipping 2-8 hour, filter then, wash, 60 ℃ of-80 ℃ of oven dry, obtain described catalyst.
6. catalyst according to claim 5 is characterized in that: described in the step (1) in the perferrite solution concentration of ferrous ion be 3mg/ml-12mg/ml; The described chitin modified active carbon and the mass volume ratio 1g of perferrite solution: (5-10) ml; Described in the step (2) in the palladium saline solution concentration of divalence palladium ion be 0.25mg/ml-1.5mg/ml; The active carbon of described load auxiliary agent Fe and the mass volume ratio of described palladium saline solution are 1g: (5-20) ml; Described soluble ferrite is FeCl
2Or FeSO
47H
2O, described soluble palladium salt is PdCl
2Or H
2PdCl
4
7. prepare the method for arbitrary described catalyst among the claim 1-3, comprise the steps:
(1) the solubility divalent iron salt is mixed with perferrite solution; Adopt the equi-volume impregnating active carbon that described carrier is chitin modified to place described perferrite solution dipping 2-8 hour, filter then, wash, 60 ℃ of-80 ℃ of oven dry, obtain the active carbon of load auxiliary agent Fe;
(2) solubility divalence palladium salt is mixed with the palladium saline solution; Adopt equi-volume impregnating that the active carbon of the load auxiliary agent Fe of step 1) preparation was placed described palladium saline solution dipping 2-8 hour, filter then, wash, 60 ℃ of-80 ℃ of oven dry, obtain described catalyst.
8. method according to claim 7 is characterized in that: described in the step (1) in the perferrite solution concentration of ferrous ion be 3mg/ml-12mg/ml; The described chitin modified active carbon and the mass volume ratio 1g of perferrite solution: (5-10) ml; Described in the step (2) in the palladium saline solution concentration of divalence palladium ion be 0.25mg/ml-1.5mg/ml; The active carbon of described load auxiliary agent Fe and the mass volume ratio of described palladium saline solution are 1g: (5-20) ml; Described soluble ferrite is FeCl
2Or FeSO
47H
2O, described soluble palladium salt is PdCl
2Or H
2PdCl
4
9. according to claim 7 or 8 described methods, it is characterized in that: described chitin modified active carbon prepares according to following method: shitosan is dissolved in the acetum that mass concentration is 1%-3%, be mixed with the chitosan-acetic acid solution that chitosan mass concentration is 0.5%-1%, to be that active carbons after 5%-10% nitric acid dousing, washing, 105 ℃ of oven dry are handled were put into the chitosan-acetic acid solution dipping prepared 2-3 hour through mass concentration then, filter, 60 ℃ of-80 ℃ of oven dry promptly obtain chitin modified active carbon.
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| CN102921431A (en) * | 2012-10-19 | 2013-02-13 | 大连凯特利催化工程技术有限公司 | Catalyst used in oxidative desorption of carbon monoxide in hydrogen and preparation method for catalyst |
| CN104010699A (en) * | 2011-11-07 | 2014-08-27 | 庄信万丰股份有限公司 | Apparatus for the treatment of air |
| CN108126708A (en) * | 2017-12-08 | 2018-06-08 | 中国科学院兰州化学物理研究所 | A kind of CO room-temperature catalytic oxidation catalysts |
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| CN108126708A (en) * | 2017-12-08 | 2018-06-08 | 中国科学院兰州化学物理研究所 | A kind of CO room-temperature catalytic oxidation catalysts |
| CN108126708B (en) * | 2017-12-08 | 2020-11-10 | 中国科学院兰州化学物理研究所 | CO normal temperature catalytic oxidation catalyst |
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| Publication number | Publication date |
|---|---|
| CN101879454B (en) | 2012-11-14 |
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