CN102764646A - Preparation method of supported room-temperature combustion catalyst - Google Patents
Preparation method of supported room-temperature combustion catalyst Download PDFInfo
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- CN102764646A CN102764646A CN201210225486XA CN201210225486A CN102764646A CN 102764646 A CN102764646 A CN 102764646A CN 201210225486X A CN201210225486X A CN 201210225486XA CN 201210225486 A CN201210225486 A CN 201210225486A CN 102764646 A CN102764646 A CN 102764646A
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Abstract
The invention discloses a preparation method of a supported room-temperature combustion catalyst. The preparation method is an incipient wetness impregnation-organic compound reduction method, and the supported room-temperature combustion catalyst is prepared by the method. The incipient wetness impregnation-organic compound reduction method overcomes the defects that the reduction operation is complicated and the metal reduction degree is difficult to control due to the explosiveness of hydrogen in the traditional incipient wetness impregnation-hydrogen reduction method. The supported room-temperature combustion catalyst prepared by the method includes one or more among noble metal as the active component, and the carrier is one of oxide and activated carbon. The catalyst has very high catalytic combustion activity, and can easily combust alcohol, aldehyde, alkane, carbon monoxide, hydrogen and the like at room temperature or even below.
Description
Technical field
The present invention relates to a kind of preparation method of room temperature combustion catalyst; Relating in particular to a kind of is active component with the noble metal; With various oxides, active carbon etc. is the catalyst of carrier: this catalyst can at room temperature make the methyl alcohol burning, and can be used for the catalytic combustion of other alcohols, aldehydes, alkanes, carbon monoxide, hydrogen etc.
Background technology
Along with the development and the progress of society, the growth and the contradiction between the scarcity of resources of world energy sources consumption are sharp-pointed day by day, and therefore, the innovation of traditional energy utilization technology becomes the focal issue that receives much concern.Catalytic combustion has caused the generally attention of academia and industrial quarters as the novel utilization technology of traditional energy.
Compare with flame combustion, catalytic combustion mainly has the following advantages: 1) initiation temperature is low, realizes smooth combustion easily; 2) help improving efficiency of combustion, reduce the discharging of pollutant; 3) can use in than scope in bigger combustion gas; 4) noise is low.
Just because of possessing above-mentioned advantage, catalytic combustion is that a kind of energy consumption is low, and efficient is high, and eco-friendly organic waste is administered technology, also is one of optimal path of using energy source.For catalyst combustion reaction; Study the more catalytic combustion that methane catalytic combustion, catalyzing carbon monoxide burning, volatile organic matter (VOC) (like methyl alcohol, benzene,toluene,xylene, acetone, ethyl acetate etc.) are arranged, the catalytic combustion of volatility chlorinated organics (CVOC) (like chlorobenzene, trichloro-ethylene etc.).
In methane catalytic combustion reaction, studying more is palladium catalyst.In document (Carraz à n et al, Catal Today. 112 (2006) 161), as (CH
4/ O
2/ CO
2/ He=1/10/3/86, V/V/V/ V) mass space velocity is 1,875 m
3During/g/h, the temperature that methane transforms fully is about 500 ℃, and in the document (Wang et al, Chin J Catal. 29 (2008) 1043), as (CH
4/ O
2/ N
2=1/4/45, the volume space velocity of V/V/V) is 48,000 h
-1The time, the temperature that methane transforms fully is about 350 ℃.
In the catalyzing carbon monoxide combustion reaction; Studying more is catalyst such as platinum, palladium, gold; Wherein load type gold catalyst just has very high activity below zero centigrade, in document (Yan et al, J Am Chem Soc. 127 (2005) 10480); When (CO/Air=1/100, the flow velocity of V/V) is 37 cm
3During/min, the temperature that carbon monoxide transforms fully on the 50 mg load type gold catalysts is about-20 ℃.
In the catalyst combustion reaction of VOC and CVOC, noble metal catalysts such as load type palladium, platinum, rhodium, ruthenium obtain broad research with its good low temperature ignition performance, and its catalytic activity is different because of catalyst and reactant species.In document (Guillemot et al, Catal Lett. 40 (1996) 175), when passing through VOC and CVOC saturated vapor (N
2/ O
2=1/4, the air speed of V/V) is 30,600 h
-1The time, the temperature of tetrachloro-ethylene and methyl ethyl ketone completing combustion on 1.2 % Pt/HFAU and 1 % Pt/NaX catalyst is respectively 500 and 220 ℃.
In all combustion reactions; Catalytic combustion researcher about under the methyl alcohol catalytic combustion especially room temperature condition is less; In the methyl alcohol catalyst combustion reaction, it is more that palladium and platinum catalyst are studied, like document (la Pe a O ' Shea et al; Appl Catal B:Environ. 57 (2005) 191) in, as (122.9 ml/min N
2+ 29.9 ml/min O
2+ 0.34 ml/min CO) through behind the methyl alcohol saturator, methyl alcohol complete conversion temperature on 0.1 g palladium-containing catalyst is about 80 ℃.
To sum up, noble metal has higher activity to catalyst combustion reaction.The preparation method of the most frequently used loaded noble metal catalyst is just wet dipping-hydrogen reduction method, and the shortcoming of this method is: the combustibility of hydrogen makes restoring operation, and more the reducing degree of complicacy and metal is wayward.Therefore, develop very necessity of simple and easy to do method for preparing catalyst.
Summary of the invention
Prepare the existing problem of loaded noble metal catalyst to just wet dipping-hydrogen reduction method, we disclose a kind of new Preparation of Catalyst forwarding method: just wet dipping-organic compound reducing process.This method has overcome restoring operation more complicated and dangerous bigger shortcoming in the just wet dipping-hydrogen reduction method, and the catalyst activity of preparation is higher, has more wide application prospect.
The technology path that the present invention adopts is: utilize the salting liquid of noble metal that metal oxide carrier is flooded earlier, utilize organic compound that slaine is reduced again.The reduction reaction energy needed both can provide through the outer heating equipment of system, also can provide through the burning of reducing agent in the system.The latter is more simple, only needs 5 min just can accomplish.
The preparation method of a kind of support type room temperature of the present invention combustion catalyst is characterized in that having following preparation process and step:
A. get a certain amount of organic precious metal salt and be dissolved in the certain amount of organic solvent, organic precious metal salt is acetylacetone,2,4-pentanedione platinum
Or in the palladium acetylacetonate any; Organic solvent is an acetone; It is mixed with the solution that concentration is 1.0 ~ 2.0 mg/ml;
B. in the solution of above-mentioned acetylacetone,2,4-pentanedione platinum or palladium acetylacetonate, add a certain amount of carrier mass, carrier mass does
Aluminium oxide or titanium oxide metal oxide; The quality percentage composition of control noble metal active component is 0.05 ~ 2.0 % in this system; The proportioning quantitative relation of organic precious metal salting liquid and carrier mass is: the carrier mass that correspondingly adds 0.1 ~ 0.15 g in per 1 ml organic precious metal salting liquid;
C. adopt just wet dipping-organic compound reducing process to prepare combustion catalyst: above-mentioned system is evenly stirred ultrasonic 20 ~ 30 min in back, and dry 6 ~ 8 hours at ambient temperature; Then with its compressing tablet and be crushed to 20 ~ 40 orders;
D. above-mentioned gained particulate matter is placed tube type resistance furnace, do carrier gas, the saturated vapor of organic reducing agent is brought in the above-mentioned catalyst system, make the generation reduction reaction with inert gas; Described organic reducing agent is any in methyl alcohol, formaldehyde or the acetone; Gas flow is 40 ~ 50 ml/min; Heating rate is 2 ℃/min; After being heated to 220 ℃, be incubated 1 hour, reduce to room temperature then, promptly make the room temperature combustion catalyst.
Described organic reducing agent also can directly add catalyst system with organic reducing agent liquid and carry out ignition operation except above-mentioned can the saturated vapor of organic reducing agent being brought into by inert gas makes in the catalyst system the generation reduction reaction; Institute's energy requirement is provided by the outer heater of system in the former reduction process; Latter's reduction process institute energy requirement is provided by the burning of reducing agent in the system self.
The invention has the advantages that the Preparation of catalysts method is simple and safe, activity of such catalysts is high.
The specific embodiment
Embodiment 1
Acetylacetone,2,4-pentanedione platinum is dissolved in the amount of acetone, is made into the solution that concentration is 1.081 mg/ml, in the acetone soln of 18.5 ml acetylacetone,2,4-pentanedione platinum, add 2 g Al
2O
3Powder evenly stirs back ultrasonic immersing 20 min, and vacuum drying is 6 hours at ambient temperature; With its compressing tablet and be crushed to 20～40 orders, catalyst granules is placed tube type resistance furnace at last, do carrier gas with inert gas; Utilize the saturated vapor reduction of methyl alcohol, gas flow is 40 ml/min, temperature programming (heating rate be 2 ℃/min) after 220 ℃, kept 1 hour; Cooling promptly makes catalyst.Catalyst detects test: the catalyst that makes is placed reactor; The gaseous mixture of bubbling air and methanol steam reacts; Catalyst amount is 0.2 g, and air mass flow is 100 ml/min, and methanol content is its saturated vapor; Temperature of reactor is 27 ℃, utilizes that gas chromatograph is online to record that conversion of methanol is 99 % on this catalyst.
Embodiment 2
Acetylacetone,2,4-pentanedione platinum is dissolved in the amount of acetone, is made into the solution that concentration is 1.081 mg/ml, in the acetone soln of 18.5 ml acetylacetone,2,4-pentanedione platinum, add 2 g Al
2O
3Powder evenly stirs back ultrasonic immersing 20 min, and vacuum drying is 6 hours at ambient temperature; With its compressing tablet and be crushed to 20～40 orders, catalyst granules is placed tube type resistance furnace at last, do carrier gas with inert gas; Utilize the saturated vapor reduction of formaldehyde, gas flow is 40 ml/min, temperature programming (heating rate be 2 ℃/min) after 220 ℃, kept 1 hour; Cooling promptly makes catalyst.Catalyst detects test: the catalyst that makes is placed reactor; The gaseous mixture of bubbling air and methanol steam reacts; Catalyst amount is 0.2 g, and air mass flow is 100 ml/min, and methanol content is its saturated vapor; Temperature of reactor is 27 ℃, utilizes that gas chromatograph is online to record that conversion of methanol is 94 % on this catalyst.
Embodiment 3
Acetylacetone,2,4-pentanedione platinum is dissolved in the amount of acetone, is made into the solution that concentration is 1.081 mg/ml, in the acetone soln of 18.5 ml acetylacetone,2,4-pentanedione platinum, add 2 g Al
2O
3Powder evenly stirs back ultrasonic immersing 20 min, and vacuum drying is 6 hours at ambient temperature; With its compressing tablet and be crushed to 20～40 orders, catalyst granules is placed tube type resistance furnace at last, do carrier gas with inert gas; Utilize the saturated vapor reduction of ethanol, gas flow is 40 ml/min, temperature programming (heating rate be 2 ℃/min) after 220 ℃, kept 1 hour; Cooling promptly makes catalyst.Catalyst detects test: the catalyst that makes is placed reactor; The gaseous mixture of bubbling air and methanol steam reacts; Catalyst amount is 0.2 g, and air mass flow is 100 ml/min, and methanol content is its saturated vapor; Temperature of reactor is 27 ℃, utilizes that gas chromatograph is online to record that conversion of methanol is 88 % on this catalyst.
Embodiment 4
Acetylacetone,2,4-pentanedione platinum is dissolved in the amount of acetone, is made into the solution that concentration is 1.081 mg/ml, in the acetone soln of 18.5 ml acetylacetone,2,4-pentanedione platinum, add 2 g Al
2O
3Powder evenly stirs back ultrasonic immersing 20 min, and vacuum drying is 6 hours at ambient temperature; With its compressing tablet and be crushed to 20～40 orders, catalyst granules is placed tube type resistance furnace at last, do carrier gas with inert gas; Utilize the saturated vapor reduction of acetone, gas flow is 40 ml/min, temperature programming (heating rate be 2 ℃/min) after 220 ℃, kept 1 hour; Cooling promptly makes catalyst.Catalyst detects test: the catalyst that makes is placed reactor; The gaseous mixture of bubbling air and methanol steam reacts; Catalyst amount is 0.2 g, and air mass flow is 100 ml/min, and methanol content is its saturated vapor; Temperature of reactor is 27 ℃, utilizes that gas chromatograph is online to record that conversion of methanol is 80 % on this catalyst.
Embodiment 5
Acetylacetone,2,4-pentanedione platinum is dissolved in the acetone, is made into the solution that concentration is 1.081 mg/ml, in the acetone soln of 18.5 ml acetylacetone,2,4-pentanedione platinum, add 2 g Al
2O
3Fiber, shake add to even back methyl alcohol light to the methyl alcohol burning fully, promptly make catalyst.Catalyst detects test: the catalyst that makes is placed reactor; The gaseous mixture of bubbling air and methanol steam reacts; Catalyst amount is 0.2 g, and air mass flow is 100 ml/min, and methanol content is its saturated vapor; Temperature of reactor is 27 ℃, utilizes that gas chromatograph is online to record that conversion of methanol is 70 % on this catalyst.In the methanol solution top, the methanol steam that from solution, evaporates can burn at catalyst with this catalyst room temperature underlying, and the heat that burning is discharged can make alumina fibre redden.
Claims (2)
1. the preparation method of a support type room temperature combustion catalyst is characterized in that having following preparation process and step:
A. get a certain amount of organic precious metal salt and be dissolved in the certain amount of organic solvent, organic precious metal salt is acetylacetone,2,4-pentanedione platinum
Or in the palladium acetylacetonate any; Organic solvent is an acetone; It is mixed with the solution that concentration is 1.0 ~ 2.0 mg/ml;
B. in the solution of above-mentioned acetylacetone,2,4-pentanedione platinum or palladium acetylacetonate, add a certain amount of carrier mass, carrier mass does
Aluminium oxide or titanium oxide metal oxide; The quality percentage composition of control noble metal active component is 0.05 ~ 2.0 % in this system; The proportioning quantitative relation of organic precious metal salting liquid and carrier mass is: the carrier mass that correspondingly adds 0.1 ~ 0.15 g in per 1 ml organic precious metal salting liquid;
C. adopt just wet dipping-organic reducing agent reducing process to prepare combustion catalyst: above-mentioned system is evenly stirred ultrasonic 20 ~ 30 min in back, and dry 6 ~ 8 hours at ambient temperature; Then with its compressing tablet and be crushed to 20 ~ 40 orders;
D. above-mentioned gained particulate matter is placed tube type resistance furnace, do carrier gas, the saturated vapor of organic reducing agent is brought in the above-mentioned catalyst system, make the generation reduction reaction with inert gas; Described organic reducing agent is any in methyl alcohol, formaldehyde or the acetone; Gas flow is 40 ~ 50 ml/min; Heating rate is 2 ℃/min; After being heated to 220 ℃, be incubated 1 hour, reduce to room temperature then, promptly make the room temperature combustion catalyst.
2. the preparation method of a kind of support type room temperature combustion catalyst according to claim 1; It is characterized in that: described organic reducing agent also can directly add catalyst system with organic reducing agent liquid and carry out ignition operation except above-mentioned can the saturated vapor of organic reducing agent being brought into by inert gas makes in the catalyst system the generation reduction reaction; Institute's energy requirement is provided by the outer heater of system in the former reduction process; Latter's reduction process institute energy requirement is provided by the burning of reducing agent in the system self.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109289834A (en) * | 2018-09-26 | 2019-02-01 | 中国科学院武汉物理与数学研究所 | A kind of synthetic method and its application of no template agent hydrothermal synthesis alumina nano fiber material |
| CN111151247A (en) * | 2018-11-08 | 2020-05-15 | 中国科学院大连化学物理研究所 | Supported catalyst and preparation method and application thereof |
| CN112871153A (en) * | 2021-01-14 | 2021-06-01 | 广东醇氢新能源研究院有限公司 | Catalyst for normal-temperature combustion of methanol and preparation method thereof |
| CN113908831A (en) * | 2021-09-23 | 2022-01-11 | 四川大学 | Hydrophobic catalyst for hydrogen negative low-temperature catalytic combustion and preparation method thereof |
| CN115414933A (en) * | 2022-09-30 | 2022-12-02 | 重庆市生态环境科学研究院 | Noble metal supported catalyst and preparation method and application thereof |
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2012
- 2012-07-03 CN CN201210225486XA patent/CN102764646A/en active Pending
Non-Patent Citations (3)
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| 张春等: "甲醇室温催化燃烧负载型铂催化剂的制备及性能研究", 《分子催化》 * |
| 杨玉霞等: "负载型钯催化剂上甲烷催化燃烧的研究进展", 《工业催化》 * |
| 王志伟等: "负载型Pt／Ti02催化剂的制备及其催化燃烧性能研究", 《价值工程》 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109289834A (en) * | 2018-09-26 | 2019-02-01 | 中国科学院武汉物理与数学研究所 | A kind of synthetic method and its application of no template agent hydrothermal synthesis alumina nano fiber material |
| CN111151247A (en) * | 2018-11-08 | 2020-05-15 | 中国科学院大连化学物理研究所 | Supported catalyst and preparation method and application thereof |
| CN112871153A (en) * | 2021-01-14 | 2021-06-01 | 广东醇氢新能源研究院有限公司 | Catalyst for normal-temperature combustion of methanol and preparation method thereof |
| CN113908831A (en) * | 2021-09-23 | 2022-01-11 | 四川大学 | Hydrophobic catalyst for hydrogen negative low-temperature catalytic combustion and preparation method thereof |
| CN115414933A (en) * | 2022-09-30 | 2022-12-02 | 重庆市生态环境科学研究院 | Noble metal supported catalyst and preparation method and application thereof |
| CN115414933B (en) * | 2022-09-30 | 2024-01-30 | 重庆市生态环境科学研究院 | Noble metal supported catalyst and preparation method and application thereof |
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Application publication date: 20121107 |