CN102059115A - CO normal-temperature catalytic oxidation catalyst and preparation method thereof - Google Patents
CO normal-temperature catalytic oxidation catalyst and preparation method thereof Download PDFInfo
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- CN102059115A CN102059115A CN2010105952116A CN201010595211A CN102059115A CN 102059115 A CN102059115 A CN 102059115A CN 2010105952116 A CN2010105952116 A CN 2010105952116A CN 201010595211 A CN201010595211 A CN 201010595211A CN 102059115 A CN102059115 A CN 102059115A
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- attapulgite clay
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Abstract
The invention relates to a CO normal-temperature catalytic oxidation catalyst and a preparation method thereof. The catalyst is loaded with an active component nano Pd and an assistant V2O5 or MoO3 by taking attapulgite clay as a carrier, wherein the mass of the active component nano Pd is 0.5-3 percent of the mass of the carrier; the mass of the assistant is 0.1-2 percent of the mass of the carrier, and the balance is the carrier. The poison affect of harmful gases such as NOx, THC, SO2 and the like on the catalyst can be effectively overcome, and the service life of the catalyst can be prolonged. The catalyst has the characteristics of high activity, high stability, capability of effectively overcoming the poison affect of other gases on the catalyst, and the like.
Description
Technical field
The present invention relates to a kind of carbon monoxide room-temperature catalytic oxidation catalyst and preparation method thereof, particularly a kind of is the carbon monoxide room-temperature catalytic oxidation catalyst and preparation method thereof of carrier with the attapulgite clay.
Background technology
Attapulgite clay is a kind of natural minerals, have high-specific surface area, characteristics such as the ion exchangeable ability is strong, chemical stability good, strong absorptive, be widely used as in fields such as petrochemical industry, daily-use chemical industry, fine chemistry industry, food processing, using for adsorbent, catalyst carrier and antiseptic carrier.The CO room-temperature catalytic oxidation catalyst is had a large amount of research both at home and abroad, mainly can be divided into two classes: a class is a noble metal catalyst, mainly the series of products that are made of Pt, Pd, Au etc. and various carriers; Another kind of is non-precious metal catalyst, and main the employing has the transition metal of catalytic oxidation-reduction characteristic, the composite oxides or the mixture of rare earth metal.Retrieval to prior art is found, the disclosed palladium catalyst of Chinese invention patent publication number CN1583258 is carrier with the active carbon, Li, K, P, Cu, one or more elements among the V are auxiliary agent, the preparation of employing step impregnation method, this catalyst normal temperature is active down high, bullion content low (accounting for vehicle weight percentage 0.1～3%), and the life-span is long, moisture-proof is good, but it is narrower by (5～30ppm), and absorbent charcoal carrier needs boil through acid to remove the CO concentration range, preliminary treatment such as washing, the catalyst precursor of making also needs wet reducing under the normal temperature, filter, make catalyst or after filtration after the oven dry, behind the vacuum drying, make catalyst with hydrogen reduction, the step complexity, cost is higher.It is the catalyzing carbon monoxide oxidation catalyst of carrier loaded 4 ~ 30wt% cupric oxide that Chinese invention patent CN 101288847A utilizes the natural attapulgite clay, can be CO with the complete catalytic oxidation of 10%CO in the air under 120 ℃ condition
2But its serviceability temperature is higher, is not suitable for constant temperature catalyzing and purifies CO, has limited it and has used more widely.
Summary of the invention
It is the carbon monoxide room-temperature catalytic oxidation catalyst of carrier with the attapulgite clay that one of purpose of the present invention is to provide a kind of.
Two of purpose of the present invention is to provide this Preparation of catalysts method.
For achieving the above object, the present invention adopts following technical scheme:
A kind of carbon monoxide room-temperature catalytic oxidation catalyst is characterized in that this catalyst is carrier with the attapulgite clay, and load has active component nanometer palladium and auxiliary agent vanadic anhydride or molybdenum trioxide; Wherein the quality of active component nanometer palladium accounts for carrier quality 0.5 ~ 3%; The quality of auxiliary agent accounts for 0.1 ~ 2% of carrier quality; Remaining is carrier.The granularity of above-mentioned attapulgite clay is: 300 ~ 400 orders.
Above-mentioned attapulgite clay is through acidified modified, and method of modifying is: utilizing mass content is that rare nitric acid of 5 ~ 20% stirs down at 20 ~ 80 ℃ and soaked 1 ~ 24 hour.
A kind of method for preparing above-mentioned carbon monoxide room-temperature catalytic oxidation catalyst is characterized in that the concrete steps of this method are:
A. take by weighing a certain amount of metavanadic acid amine or amine molybdate and be dissolved in and be mixed with maceration extract in the deionized water, impregnation concentration is 0.0025 ~ 0.1g/ml;
B. attapulgite clay is immersed in the step a gained maceration extract, floods after 1 ~ 24 hour,,, sieve through compressing tablet and to get 20 ~ 40 order particles, make the attapulgite clay carrier of modification again 500 ~ 650 ℃ of following roastings 1 ~ 6 hour again 90 ~ 150 ℃ of down oven dry 2 ~ 12 hours;
C. with PdCl
2Be dissolved in 3% NH
4In the Cl deionized water solution, be mixed with the PdCl that impregnation concentration is 0.005 ~ 0.05g/ml
2, in this maceration extract, dipping is 1 hour under the room temperature with the attapulgite clay carrier impregnation of step b gained modification, catalyst precursor;
D. after step c gained catalyst precursor being reduced 1 hour at ambient temperature, for neutral, control pH=7 ~ 7.5 through the deionized water washing, drying makes the catalyst finished product again.
The reducing agent that adopts among the above-mentioned steps d is sodium borohydride, hydrazine hydrate or formaldehyde.
The present invention utilizes the attapulgite clay of acidified processing to be carrier, and the nanometer palladium is an active component, and vanadium or molybdenum are that auxiliary agent is prepared into carbon monoxide room-temperature catalytic oxidation catalyst.This catalyst can effectively overcome NOx, THC and SO
2Deng the poisoning effect that has gas to catalyst, prolonged its service life.This catalyst has high activity, high stability, effectively overcomes the characteristics such as poisoning effect of other gases to catalyst.
The specific embodiment:
The present invention is further described below in conjunction with the concrete preparation process of catalyst
Embodiment 1:Take by weighing a certain amount of PdCl
2Be dissolved in 3% NH
4In the Cl deionized water solution, be mixed with the 0.017g/ml maceration extract, take the incipient impregnation mode to be impregnated on the attapulgite clay carrier of acidification this maceration extract, dipping is 1 hour under the room temperature, is prepared into catalyst precursor.Take by weighing a certain amount of sodium borohydride and be dissolved in the deionized water, at ambient temperature reducing solution is poured into catalyst precursor reduction 1 hour as reducing solution., dried 4 hours down through 120 ℃ again for neutral through the deionized water washing, make the catalyst finished product that contains 1%Pd.
Made catalyst is carried out catalytic performance test according to the afore-mentioned test condition, and catalyst is 56.2% to the conversion ratio of carbon monoxide.
Embodiment 2:Take by weighing a certain amount of metavanadic acid amine solvent and in 0.45 ml deionized water, be mixed with the 0.005g/ml maceration extract, the 0.5 attapulgite clay powder through acidification that restrains is placed small beaker, the maceration extract for preparing is poured into wherein, flooded 1 hour.Then 120 ℃ of down oven dry 4 hours, 550 ℃ of following roastings 3 hours are sieved through compressing tablet and are got 20 ~ 40 orders and make the modified attapulgite clay carrier.
Take by weighing a certain amount of PdCl
2Be dissolved in 3% NH
4In the Cl deionized water solution, be mixed with the 0.017g/ml maceration extract, take the incipient impregnation mode to be impregnated on the attapulgite clay carrier of modification this maceration extract, dipping is 1 hour under the room temperature, is prepared into catalyst precursor.Take by weighing a certain amount of sodium borohydride and be dissolved in and be configured to the reducing solution that concentration is 0.03g/ml in the deionized water, at ambient temperature reducing solution is poured into catalyst precursor reduction 1 hour.Through the deionized water washing is neutral, dries 4 hours down through 120 ℃ again, makes to contain 0.5%V
2O
5Catalyst finished product with 1%Pd.
Made catalyst is carried out catalytic performance test according to the afore-mentioned test condition, and catalyst is 86.7% to the conversion ratio of carbon monoxide.
Embodiment 3:Take by weighing a certain amount of amine molybdate and be dissolved in and be mixed with the 0.007g/ml maceration extract in 0.45 ml deionized water, the attapulgite clay powder through acidification of 0.5 gram is placed small beaker, the maceration extract for preparing is poured into wherein, flooded 1 hour.Then 120 ℃ of down oven dry 4 hours, 550 ℃ of following roastings 3 hours are sieved through compressing tablet and are got 20 ~ 40 orders and make the modified attapulgite clay carrier.
Take by weighing a certain amount of PdCl
2Be dissolved in 3% NH
4In the Cl deionized water solution, be mixed with the 0.017g/ml maceration extract, take the incipient impregnation mode to be impregnated on the attapulgite clay carrier of modification this maceration extract, dipping is 1 hour under the room temperature, is prepared into catalyst precursor.Take by weighing a certain amount of sodium borohydride and be dissolved in and be configured to the reducing solution that concentration is 0.03g/ml in the deionized water, at ambient temperature reducing solution is poured into catalyst precursor reduction 1 hour.Through the deionized water washing is neutral, dries 4 hours down through 120 ℃ again, makes to contain 0.5%MnO
3Catalyst finished catalyst finished product with 1%Pd.
Made catalyst is carried out catalytic performance test according to the afore-mentioned test condition, and catalyst is 83.5% to the conversion ratio of carbon monoxide.
Embodiment 4:Taking by weighing a certain amount of metavanadic acid amine and amine molybdate is dissolved in and is mixed with the maceration extract that concentration is respectively 0.005g/ml and 0.007g/ml in 0.45 ml deionized water, the attapulgite clay powder through acidification of 0.5 gram is placed small beaker, the maceration extract for preparing is poured into wherein, flooded 1 hour.Then 120 ℃ of down oven dry 4 hours, 550 ℃ of following roastings 3 hours are sieved through compressing tablet and are got 20 ~ 40 orders and make the modified attapulgite clay carrier.
Take by weighing a certain amount of PdCl
2Be dissolved in 3% NH
4In the Cl deionized water solution, be mixed with the 0.017g/ml maceration extract, take the incipient impregnation mode to be impregnated on the attapulgite clay carrier of modification this maceration extract, dipping is 1 hour under the room temperature, is prepared into catalyst precursor.Take by weighing a certain amount of sodium borohydride and be dissolved in the deionized water, at ambient temperature reducing solution is poured into catalyst precursor reduction 1 hour as reducing solution.Through the deionized water washing is neutral, dries 4 hours down through 120 ℃ again, makes to contain 0.5%V
2O
5, 0.5%MnO
3Catalyst finished catalyst finished product with 1%Pd.Made catalyst is carried out catalytic performance test according to the afore-mentioned test condition, and catalyst is 99.4% to the conversion ratio of carbon monoxide.
Catalyst performance evaluation is carried out in U type glass tube reactor, catalyst amount 0.5ml, and it is 10～200ppm that granularity 20～40 orders, unstripped gas consist of CO content, all the other are air.30 ℃ of reaction temperatures, pressure 0.1MPa, relative humidity 40～90%, reaction gas volume air speed (GHSV) is 12000h
-1
Claims (5)
1. a carbon monoxide room-temperature catalytic oxidation catalyst is characterized in that this catalyst is carrier with the attapulgite clay, and load has active component nanometer palladium and auxiliary agent vanadic anhydride or molybdenum trioxide; Wherein the quality of active component nanometer palladium accounts for 0.5 ~ 3% of carrier quality; The quality of auxiliary agent accounts for 0.1 ~ 2% of carrier quality; Remaining is carrier.
2. carbon monoxide room-temperature catalytic oxidation catalyst according to claim 1 is characterized in that the granularity of described attapulgite clay is: 300 ~ 400 orders.
3. carbon monoxide room-temperature catalytic oxidation catalyst according to claim 1 and 2 is characterized in that described attapulgite clay through acidified modified, and method of modifying is: utilizing mass content is that rare nitric acid of 5 ~ 20% stirs down at 20 ~ 80 ℃ and soaked 1 ~ 24 hour.
4. method for preparing according to claim 1,2 or 3 described carbon monoxide room-temperature catalytic oxidation catalysts is characterized in that the concrete steps of this method are:
A. take by weighing a certain amount of metavanadic acid amine or amine molybdate and be dissolved in and be mixed with maceration extract in the deionized water, impregnation concentration is 0.0025 ~ 0.1g/ml;
B. attapulgite clay is immersed in the step a gained maceration extract, floods after 1 ~ 24 hour,,, sieve through compressing tablet and to get 20 ~ 40 order particles, make the attapulgite clay carrier of modification again 500 ~ 650 ℃ of following roastings 1 ~ 6 hour again 90 ~ 150 ℃ of down oven dry 2 ~ 12 hours;
C. with PdCl
2Be dissolved in 3% NH
4In Cl or the HCl deionized water solution, be mixed with the PdCl that concentration is 0.005 ~ 0.05g/ml
2Maceration extract, in this maceration extract, dipping is 1 hour under the room temperature with the attapulgite clay carrier impregnation of step b gained modification, catalyst precursor;
D. after step c gained catalyst precursor being reduced 1 ~ 3 hour at ambient temperature, for neutral, control pH=7 ~ 7.5 through the deionized water washing, drying makes the catalyst finished product again.
5. a kind of method for preparing carbon monoxide room-temperature catalytic oxidation catalyst according to claim 4 is characterized in that the reducing agent that adopts in the described steps d is sodium borohydride, hydrazine hydrate or formaldehyde.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103816861A (en) * | 2014-03-19 | 2014-05-28 | 盐城工学院 | Preparation method of attapulgite clay desulfurizing agent |
| CN108579733A (en) * | 2018-05-02 | 2018-09-28 | 河南师范大学 | Infusion method prepares application of the titanium dichloride load nano Pd catalyst in being catalyzed CO oxidation reactions |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6411642A (en) * | 1987-07-02 | 1989-01-17 | Idemitsu Kosan Co | Oxidation catalyst of carbon monoxide |
| CN1583258A (en) * | 2004-06-11 | 2005-02-23 | 湖北省化学研究院 | Micro-carbon monoxide normal temperature eliminating catalyst and preparing method thereof |
| CN101264445A (en) * | 2008-05-08 | 2008-09-17 | 南开大学 | Supported type nano catalyst for low temperature carbon monoxide oxidation and preparation thereof |
| CN101898137A (en) * | 2010-07-22 | 2010-12-01 | 华东理工大学 | Pd-Cu catalyst for CO low-temperature oxidation and preparation method thereof |
-
2010
- 2010-12-20 CN CN2010105952116A patent/CN102059115A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6411642A (en) * | 1987-07-02 | 1989-01-17 | Idemitsu Kosan Co | Oxidation catalyst of carbon monoxide |
| CN1583258A (en) * | 2004-06-11 | 2005-02-23 | 湖北省化学研究院 | Micro-carbon monoxide normal temperature eliminating catalyst and preparing method thereof |
| CN101264445A (en) * | 2008-05-08 | 2008-09-17 | 南开大学 | Supported type nano catalyst for low temperature carbon monoxide oxidation and preparation thereof |
| CN101898137A (en) * | 2010-07-22 | 2010-12-01 | 华东理工大学 | Pd-Cu catalyst for CO low-temperature oxidation and preparation method thereof |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103816861A (en) * | 2014-03-19 | 2014-05-28 | 盐城工学院 | Preparation method of attapulgite clay desulfurizing agent |
| CN103816861B (en) * | 2014-03-19 | 2016-04-06 | 盐城工学院 | The preparation method of attapulgite clay desulfurizing agent |
| CN108579733A (en) * | 2018-05-02 | 2018-09-28 | 河南师范大学 | Infusion method prepares application of the titanium dichloride load nano Pd catalyst in being catalyzed CO oxidation reactions |
| CN108579733B (en) * | 2018-05-02 | 2020-05-08 | 河南师范大学 | Application of titanium dioxide supported nano palladium catalyst prepared by soaking method in CO oxidation reaction catalysis |
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Application publication date: 20110518 |