CN101879454B - 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 PDF

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CN101879454B
CN101879454B CN2010102330597A CN201010233059A CN101879454B CN 101879454 B CN101879454 B CN 101879454B CN 2010102330597 A CN2010102330597 A CN 2010102330597A CN 201010233059 A CN201010233059 A CN 201010233059A CN 101879454 B CN101879454 B CN 101879454B
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active carbon
catalyst
carrier
palladium
auxiliary agent
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CN101879454A (en
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孙君社
苗翠玲
张秀清
刘萍
刘莉
张京声
胡锦蓉
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China Agricultural University
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China Agricultural University
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    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
    • Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
    • Y02A50/20—Air quality improvement or preservation, e.g. vehicle emission control or emission reduction by using catalytic converters

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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

A kind of Catalysts and its preparation method of catalyzing and oxidizing carbon monoxide at low temperature
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 3In time, will act on the toxic elements in human body evil.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, like 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 like 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 through 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, is prone to 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, but uses dodecyl sodium sulfate (DBS) could obtain high low temperature active as surfactant in the preparation process.Co through the preparation of deposition 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.Like 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 ℃.It is thus clear that 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 is better with stability, but cost is high.Pd/SnO like the disclosed a kind of carbon monoxide oxidation of US4490482 2Catalyst, because the content of precious metal palladium is high, preparation cost is high, and can't in industry, scale use.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.Like 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 type 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, said carrier is chitin modified active carbon; Said active component Pd and auxiliary agent Fe load on the said carrier.
In the said catalyst, the quality of active component Pd is the 0.5%-3% of said 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 said carrier quality, is preferably 3%-12%, specifically can be 3%, 6% or 12%.
Said 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 said carrier is chitin modified to place said 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 said palladium saline solution dipping 2-8 hour, filter then, wash, 60 ℃ of-80 ℃ of oven dry, obtain said catalyst.
Wherein, described in the step (1) in the perferrite solution concentration of ferrous ion be 3mg/ml-12mg/ml; The said 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 said load auxiliary agent Fe and the mass volume ratio of said palladium saline solution are 1g: (5-20) ml.
Said soluble ferric iron salt specifically can be FeCl 2Or FeSO 47H 2O, said 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 5%-10% nitric acid dousing, washing through mass concentration then, 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) high under the low temperature (40 ℃-80 ℃) to micro CO catalytic oxidation activity in the air, long service life, moisture resistance properties is good;
(2) this catalyst carries out the modification processing through 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) added an amount of auxiliary agent Fe element in this catalyst, Pd content is reduced, overcome that the catalyst cost is high, the limitation of narrow in application range;
(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 through specific embodiment below, but the present invention is not limited thereto.
Experimental technique described in the following embodiment like no specified otherwise, is conventional method; Said reagent and material like no specified otherwise, all can obtain from commercial sources.
Active carbon used among the following embodiment is like no specified otherwise, is and uses that mass concentration is that 10% salpeter solution soaks, the active carbon of washing to filtrating after being neutral, oven dry and handling.
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 draw through computes:
Q = q 0 - q 1 m
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 subsequent use.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 subsequent use.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 subsequent use.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 subsequent use.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 subsequent use.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 (10)

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, said carrier is chitin modified active carbon; Said active component Pd and auxiliary agent Fe load on the said carrier;
Said 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.
2. catalyst according to claim 1 is characterized in that: in the said catalyst, the quality of active component Pd is the 0.5%-3% of said carrier quality; The quality of auxiliary agent Fe is the 3%-24% of said carrier quality.
3. catalyst according to claim 2 is characterized in that: in the said catalyst, the quality of active component Pd is the 1%-2% of said carrier quality; The quality of auxiliary agent Fe is the 3%-12% of said carrier quality.
4. according to arbitrary described catalyst among the claim 1-3, it is characterized in that: said chitin modified active carbon is made up of shitosan and active carbon, and wherein, the mass ratio of shitosan and active carbon is 1: 5-1: 40.
5. catalyst according to claim 4 is characterized in that: the mass ratio of said shitosan and active carbon is 1: 10-1: 20.
6. catalyst according to claim 1 is characterized in that: said catalyst prepares 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 said carrier is chitin modified to place said 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 said palladium saline solution dipping 2-8 hour, filter then, wash, 60 ℃ of-80 ℃ of oven dry, obtain said catalyst.
7. catalyst according to claim 6 is characterized in that: described in the step (1) in the perferrite solution concentration of ferrous ion be 3mg/ml-12mg/ml; The said 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 said load auxiliary agent Fe and the mass volume ratio of said palladium saline solution are 1g: (5-20) ml; Soluble ferrite is FeCl 2Or FeSO 47H 2O, soluble palladium salt are PdCl 2Or H 2PdCl 4
8. prepare the method for arbitrary said catalyst among the claim 1-7, comprise the steps:
(1) the solubility divalent iron salt is mixed with perferrite solution; Adopt the equi-volume impregnating active carbon that said carrier is chitin modified to place said 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 said palladium saline solution dipping 2-8 hour, filter then, wash, 60 ℃ of-80 ℃ of oven dry, obtain said catalyst.
9. method according to claim 8 is characterized in that: described in the step (1) in the perferrite solution concentration of ferrous ion be 3mg/ml-12mg/ml; The said 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 said load auxiliary agent Fe and the mass volume ratio of said palladium saline solution are 1g: (5-20) ml; Soluble ferrite is FeCl 2Or FeSO 47H 2O, soluble palladium salt are PdCl 2Or H 2PdCl 4
10. according to Claim 8 or 9 described methods; It is characterized in that: said 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.
CN2010102330597A 2010-07-16 2010-07-16 Catalyst for catalyzing and oxidizing carbon monoxide at low temperature and preparation method thereof Expired - Fee Related CN101879454B (en)

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GB201119171D0 (en) * 2011-11-07 2011-12-21 Johnson Matthey Plc Gas treatment
CN102921431B (en) * 2012-10-19 2014-08-06 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
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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