CN104138756A - Supported catalyzer for low-temperature catalytic combustion of VOCs and method for preparing supported catalyzer for low-temperature catalytic combustion of VOCs - Google Patents
Supported catalyzer for low-temperature catalytic combustion of VOCs and method for preparing supported catalyzer for low-temperature catalytic combustion of VOCs Download PDFInfo
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Abstract
The invention discloses a supported mesoporous carbon catalyzer RTCC-1 for low-temperature catalytic combustion of VOCs and a method for preparing the supported mesoporous carbon catalyzer RTCC-1. Due to the fact that the TSC-1 mesoporous carbon material which has the unique physicochemical property serves as the carrier of the catalyzer, the disadvantages of a traditional catalyzer for catalytic combustion that the active metal load is high and the cost is high are eliminated. The active components of the supported catalyzer, for low-temperature catalytic combustion, prepared with the carrier include one of the precious metal Pd and the precious metal Pt and one or more of copper oxide, cerium oxide, zirconium oxide, silicon oxide and aluminium oxide. The catalyzer has extremely high room-temperature catalytic combustion activity and enables complete catalytic combustion of the VOCs such as formaldehyde, methylbenzene and benzene to be achieved at room temperature or at even lower temperature.
Description
Technical field
The invention belongs to environmental protection and technical field of chemistry and chemical engineering, be specifically related to a kind of for the complete catalytic combustion of the VOC such as formaldehyde, toluene gas is resolved into CO
2and H
2the support type mesoporous carbon method for preparing catalyst of O.
Background technology
Now, the mankind are faced with " smoke pollution ", " photochemical pollution " afterwards, taking " room air pollution " as main environmental pollution for the third time.US Experts detects to be found, in room air, have more than 500 kind of volatile organic matter, wherein carcinogen just has kind more than 20, and Causative virus is kind more than 200.What wherein harm was larger mainly contains the radioactive pollution taking radon as representative; Volatile organic matter taking formaldehyde, toluene, benzene, trichloro-ethylene etc. as representative pollutes.A large amount of startling facts confirmations, room air pollution has become " the stealthy killer " of harm humans health, also becomes the common problem of paying close attention in whole world various countries.Research shows, serious 2～5 times than outdoor air of the pollution levels of room air, can reach 100 times under special circumstances.Therefore, need to be to the purification of volatile organic matter, be the key that ensures health of people in indoor environment, also for indoor environment Study on purification has been opened up a new field.In addition, in the tail gas of many industrial production discharges, also contain the volatile organic matters such as a large amount of formaldehyde, the fast purification technology of development cost, has very strong practical value.
Catalytic combustion, as a kind of effective ways of processing organic exhaust gas, has and can process organic exhaust gas and can not produce the advantages such as harmful side product by high-speed.For catalytic combustion technology, active completely oxidizing catalyst good, good stability is crucial.The catalyst for catalytic combustion of the volatile organic matters such as formaldehyde, adopts noble metal catalyst more, and active component is mainly Pd, Pt etc.But, along with using noble metal as active component in a large amount of uses in the fields such as vehicle exhaust processing, the noble metal prices such as Pt, Pd, Rh sharp rise, therefore how to make noble metal catalyst in keeping for volatile organic compounds high catalytic activity, at utmost reducing costs is researcher's question of common concern.
Summary of the invention
The high cost problem existing for traditional noble metal catalyst, a kind of new catalyst RTCC-1 and preparation method thereof is disclosed, by the use of TSC-1 mesoporous carbon carrier, based on its unique pore passage structure and chemical composition, can be in keeping high activity of catalyst, the carrying capacity that significantly reduces noble metal active species in catalyst, greatly reduces production cost, has very wide range of application.
The technology path that the present invention adopts is: first noble metal precursor body is added in metal or nonmetal oxide precursor solution, mix rear regulation system pH and form gel to appropriate value, again mixed above-mentioned gel is joined in a certain amount of TSC-1 mesoporous carbon carrier, finally by compressing tablet after roasting and hydrogen reducing and be ground into 20-60 order particle.
The invention discloses a kind of new catalyst and preparation method thereof, it is characterized in that following preparation process:
(1) getting a certain amount of metal or nonmetal oxide presoma is dissolved in a certain amount of solvent, metal or nonmetal oxide are any one or a few in ethyl orthosilicate, sodium metasilicate, cerous nitrate, butyl titanate, isopropyl titanate, copper nitrate, aluminum nitrate, aluminium isopropoxide, zirconium oxychloride, and solvent is the one in deionized water, absolute ethyl alcohol, 2-propyl alcohol;
(2) in above-mentioned gel rubber system, add noble metal active species presoma, noble metal active species presoma is palladium acetylacetonate, Pd (NO
2)
2(NH
3)
2, acetylacetone,2,4-pentanedione platinum, Pt (NO
2)
2(NH
3)
2in any, and with between nitric acid, sodium hydroxide solution or ammoniacal liquor regulation system pH to 3.5-10.5, add if desired precipitating reagent, form gel;
(3) mixed system is added in a certain amount of TSC-1 mesoporous carbon molecular sieve carrier material, mixes and leave standstill 12～24 hours; Adjust noble metal: oxide: the mass ratio between TSC-1 carrier is 0.1～2.5:10～25:250;
(4) under nitrogen atmosphere protection, by catalyst in 350-550 DEG C of roasting temperature 6 hours, 5 DEG C/min of heating rate;
(5) noble metal reduction: use hydrogen in 300-350 DEG C of reduction noble metal species, 2 DEG C/min of heating rate, keeps 4 hours.
The invention has the advantages that: greatly reduce the production cost of volatile organic compounds by catalytic combustion noble metal catalyst, make its large-scale commercial application become possibility.Catalyst activity prepared by the present invention is high, the volatile organic matters such as formaldehyde can be oxidized to carbon dioxide and water, conversion ratio can reach 100%, generates without the accessory substance such as CO, methyl alcohol, has thoroughly eliminated the harm of the volatile organic matters such as formaldehyde to environmental and human health impacts.Meanwhile, the catalyst preparation process of the present invention's use is simple, cost controlled stability is good.Therefore, the present invention has a good application prospect.
Detailed description of the invention
Embodiment 1
Pd/SiO
2/ TSC-1 catalyst preparation process:
10.0 g ethyl orthosilicates are added in 50 ml deionized water, according to target carrying capacity, add appropriate Pd (NO
2)
2(NH
3)
2, subsequently with nitric acid regulation system pH value to 2～3, within aging 2 hours, form gel.This gel is mixed and leaves standstill 12 hours with TSC-1 mesoporous carbon molecular sieve, regulate Pd:SiO
2: TSC-1 mass ratio is 0.25:25:250, is warming up to 500 DEG C and keep 6 hours under 80 DEG C of oven dry, nitrogen protection, obtains Pd/SiO finally by 350 DEG C of reduction of hydrogen atmosphere
2/ TSC-1 catalyst.
Be 20-60 object Pd/SiO by 1.0 g compressing tablets
2/ TSC-1 catalyst packs in the crystal reaction tube of 5 millimeters of diameters, by passing in reactor tube after formaldehyde and air mixing, enters catalytic bed reaction, and the total gas hourly space velocity of gas is 20000 h
-1, the volume content of formaldehyde gas in total gas is 0.5%, and reaction temperature is 50～60 DEG C, and reaction system pressure is 0.1 MPa, and formaldehyde conversion ratio is 100%.
Embodiment 2
Pt/CeO
2/ TSC-1 catalyst preparation process:
12.0 g cerous nitrates are dissolved in 60 g deionized waters, according to target carrying capacity, add appropriate Pd (NO
2)
2(NH
3)
2, under agitation adding subsequently oxalic acid solution, oxalic acid is 2:1 with the ratio of cerous nitrate amount of substance, and aging until be completed into gel at 80 DEG C.After this gel is mixed with TSC-1 mesoporous carbon molecular sieve, leave standstill 12 hours, control Pt:CeO
2: TSC-1 mass ratio is 0.25:25:250pH value to 8～9, within aging 8 hours, forms gel.This gel is mixed and leaves standstill 12 hours with TSC-1 mesoporous carbon molecular sieve, regulate Pt:ZrO
2: TSC-1 mass ratio is 0.25:20:250, and under 80 DEG C of oven dry, nitrogen protection, roasting is warming up to 550 DEG C and keep 6 hours, obtains Pt/ZrO finally by 350 DEG C of reduction of hydrogen atmosphere
2/ TSC-1 catalyst.
1.0 g are prepared to 20-60 object Pt/ZrO
2/ TSC-1 catalyst packs in the crystal reaction tube of 5 millimeters of diameters, by passing in reactor tube after formaldehyde and air mixing, enters catalytic bed reaction, and the total gas hourly space velocity of gas is 20000 h
-1, the volume content of formaldehyde gas in total gas is 0.5%, 40～45 DEG C of reaction temperatures, and reaction system pressure is 0.1 MPa, formaldehyde conversion ratio is 100%.
Embodiment 3
Pd/Al
2o
3/ TSC-1 catalyst preparation process:
15.0 g aluminium isopropoxides are added in 90 ml deionized water, according to target carrying capacity, add appropriate Pd (NO
2)
2(NH
3)
2, subsequently with nitric acid regulation system pH value to 8～10, within agitation aging 2 hours, form gel.This gel is mixed and leaves standstill 12 hours with TSC-1 mesoporous carbon molecular sieve, regulate Pd:Al
2o
3: TSC-1 mass ratio is 0.25:12.5:250, and under 80 DEG C of oven dry, nitrogen protection, roasting is warming up to 550 DEG C and keep 6 hours, obtains Pd/Al finally by 350 DEG C of reduction of hydrogen atmosphere
2o
3/ TSC-1 catalyst.
1.0 g are prepared to 20-60 object Pd/Al
2o
3/ TSC-1 catalyst packs in the crystal reaction tube of 5 millimeters of diameters, by passing in reactor tube after formaldehyde and air mixing, enters catalytic bed reaction, and the total gas hourly space velocity of gas is 20000 h
-1, the volume content of formaldehyde gas in total gas is 0.5%, 65～70 DEG C of reaction temperatures, and reaction system pressure is 0.1 MPa, formaldehyde conversion ratio is 100%.
Embodiment 4
Pt/ZrO
2/ TSC-1 catalyst preparation process:
10.0 g zirconium oxychlorides are added in 60 ml deionized water, according to target carrying capacity, add appropriate Pt (NO
2)
2(NH
3)
2, subsequently with ammoniacal liquor regulation system pH value to 8～9, within aging 8 hours, form gel.This gel is mixed and leaves standstill 12 hours with TSC-1 mesoporous carbon molecular sieve, regulate Pt:ZrO
2: TSC-1 mass ratio is 0.25:20:250, and under 80 DEG C of oven dry, nitrogen protection, roasting is warming up to 550 DEG C and keep 6 hours, obtains Pt/ZrO finally by 350 DEG C of reduction of hydrogen atmosphere
2/ TSC-1 catalyst.
1.0 g are prepared to 20-60 object Pt/ZrO
2/ TSC-1 catalyst packs in the crystal reaction tube of 5 millimeters of diameters, by passing in reactor tube after formaldehyde and air mixing, enters catalytic bed reaction, and the total gas hourly space velocity of gas is 20000 h
-1, the volume content of formaldehyde gas in total gas is 0.5%, 40～45 DEG C of reaction temperatures, and reaction system pressure is 0.1 MPa, formaldehyde conversion ratio is 100%.
Embodiment 5
Pt/TiO
2/ TSC-1 catalyst preparation process:
10.0 g butyl titanates are added in 150 milliliters of 2-propyl alcohol, according to target carrying capacity, add appropriate Pt (NO
2)
2(NH
3)
2, subsequently by nitric acid regulation system pH value to 2-3, aging 2 hours form gel.This gel is mixed with TSC-1 mesoporous carbon molecular sieve, regulate Pt:TiO
2: TSC-1 mass ratio is 0.5～2.5:12.5:250, and under 80 DEG C of oven dry, nitrogen protection, roasting is warming up to 550 DEG C and keep 6 hours, obtains Pt/TiO finally by 350 DEG C of reduction of hydrogen atmosphere
2/ TSC-1 catalyst.
1.0 g are prepared to 20-60 object Pt/TiO
2/ TSC-1 catalyst packs in the crystal reaction tube of 5 millimeters of diameters, by passing in reactor tube after formaldehyde and air mixing, enters catalytic bed reaction, and the total gas hourly space velocity of gas is 20000 h
-1, the volume content of formaldehyde gas in total gas is 0.5%, 40～50 DEG C of reaction temperatures, and reaction system pressure is 0.1 MPa, formaldehyde conversion ratio is 100%.
Embodiment 6
Pd/Cu
0.5ce
0.5o
y/ TSC-1 catalyst preparation process:
The copper nitrate and the cerous nitrate that wait molal quantity are added to 80 ml deionized water, according to target carrying capacity, add appropriate Pd (NO
2)
2(NH
3)
2, under agitation adding subsequently oxalic acid solution, oxalic acid is 2:1 with the ratio of nitrate amount of substance, and aging until be completed into gel at 80 DEG C.This gel is mixed with TSC-1 mesoporous carbon molecular sieve and leave standstill after 12 hours Pd:Cu
0.5ce
0.5o
y: TSC-1 mass ratio is 0.125:25:250, is warming up to 550 DEG C and keep 6 hours under 80 DEG C of oven dry, nitrogen protection, obtains Pd:Cu finally by 350 DEG C of reduction of hydrogen atmosphere
0.5ce
0.5o
y: TSC-1 catalyst.
1.0 g are prepared to 20-60 object Pd/Cu
0.5ce
0.5o
y/ TSC-1 catalyst packs in the crystal reaction tube of 5 millimeters of diameters, by passing in reactor tube after formaldehyde and air mixing, enters catalytic bed reaction, and the total gas hourly space velocity of gas is 20000 h
-1, the volume content of formaldehyde gas in total gas is 0.5%, 15～20 DEG C of reaction temperatures, and reaction system pressure is 0.1 MPa, formaldehyde conversion ratio is 100%.
1.0 g are prepared to 20-60 object Pd/Cu
0.5ce
0.5o
y/ TSC-1 catalyst packs in the crystal reaction tube of 5 millimeters of diameters, by passing in reactor tube after toluene and air mixing, enters catalytic bed reaction, and the total gas hourly space velocity of gas is 20000 h
-1, the volume content of toluene gas in total gas is 0.5%, 120～125 DEG C of reaction temperatures, and reaction system pressure is 0.1 MPa, toluene conversion is 98.6%.
1.0 g are prepared to 20-60 object Pd/Cu
0.5ce
0.5o
y/ TSC-1 catalyst packs in the crystal reaction tube of 5 millimeters of diameters, by passing in reactor tube after benzene and air mixing, enters catalytic bed reaction, and the total gas hourly space velocity of gas is 20000 h
-1, the volume content of benzene in total gas is 0.5%, reaction temperature 100～105
oc, reaction system pressure is 0.1 MPa, the conversion ratio of benzene is 99.6%.
Embodiment 7
Pt/Cu
0.33ce
0.67o
y/ TSC-1 catalyst preparation process:
The copper nitrate of molal quantity 1:2 and cerous nitrate are added in 300 milliliters of 2-propyl alcohol, according to target carrying capacity, add appropriate Pt (NO
2)
2(NH
3)
2, subsequently with NaOH solution regulation system pH value to 10～12, within aging 3 hours, form gel.This gel mixed with TSC-1 mesoporous carbon molecular sieve and leave standstill after 12 hours, regulating Pt:Cu
0.33ce
0.67o
y: TSC-1 mass ratio is 0.5～2.5:12.5:250, is warming up to 550 DEG C and keep 6 hours under 80 DEG C of oven dry, nitrogen protection, obtains Pt/Cu finally by 350 DEG C of reduction of hydrogen atmosphere
0.33ce
0.67o
y/ TSC-1 catalyst.
Get 1.0 restraints ready 20-60 object Pt/Cu
0.33ce
0.67o
y/ TSC-1 catalyst packs in the crystal reaction tube of 5 millimeters of diameters, by passing in reactor tube after formaldehyde and air mixing, enters catalytic bed reaction, and the total gas hourly space velocity of gas is 20000 h
-1, the volume content of formaldehyde gas in total gas is 0.5%, reaction temperature 20～30
oc, reaction system pressure is 0.1 MPa, formaldehyde conversion ratio is 99.9%.
Get 1.0 restraints ready 20-60 object Pt/Cu
0.33ce
0.67o
y/ TSC-1 catalyst packs in the crystal reaction tube of 5 millimeters of diameters, by passing in reactor tube after toluene and air mixing, enters catalytic bed reaction, and the total gas hourly space velocity of gas is 20000 h
-1, the volume content of toluene gas in total gas is 0.5%, 135～140 DEG C of reaction temperatures, and reaction system pressure is 0.1 MPa, toluene conversion is 99.9%.
Get 1.0 restraints ready 20-60 object Pt/Cu
0.33ce
0.67o
y/ TSC-1 catalyst packs in the crystal reaction tube of 5 millimeters of diameters, by passing in reactor tube after benzene and air mixing, enters catalytic bed reaction, and the total gas hourly space velocity of gas is 20000 h
-1, the volume content of benzene in total gas is 0.5%, 110～115 DEG C of reaction temperatures, and reaction system pressure is 0.1 MPa, benzene conversion ratio is 99.9%.
Claims (4)
1. support type mesoporous carbon catalyst RTCC-1 for volatile organic matter (VOCs) low-temperature catalytic burning and preparation method thereof, is characterized in that having following preparation process and step:
A. preparing metal or nonmetal oxide precursor solution, metal or nonmetal oxide presoma are one or more in ethyl orthosilicate, sodium metasilicate, cerous nitrate, butyl titanate, isopropyl titanate, copper nitrate, aluminum nitrate, aluminium isopropoxide, zirconium oxychloride;
B. a certain amount of precious metal salt solution is added to above-mentioned solution, precious metal salt is Pd (NO
2)
2(NH
3)
2, Pt (NO
2)
2(NH
3)
2, one or more in palladium acetylacetonate, acetylacetone,2,4-pentanedione platinum, controlling mass ratio between metal and oxide is 1:10～1:80, regulation system pH, to appropriate value, adds precipitating reagent if desired, forms gel;
C. above-mentioned gel or colloid are mixed with a certain amount of carrier mass, carrier mass is TSC-1 mesoporous carbon, and the quality percentage composition of controlling noble metal active component in this system is 0.01～2.0%;
D. catalyst is through 120 DEG C after dry 12 hours, successively adopts roasting under nitrogen atmosphere, with hydrogen reducing, and reduction temperature is 300-350 DEG C and keeps 4～6 hours, finally by its compressing tablet and be sized to 20～60 orders.
2. a kind of support type mesoporous carbon catalyst RTCC-1 for volatile organic matter low-temperature catalytic burning according to claim 1 and preparation method thereof, it is characterized in that TSC-1 mesoporous carbon is not only as a kind of high-ratio surface, large pore volume, the good catalyst carrier of hydrophily, and can utilize its mesopore orbit structure, prevent that catalytic active species from reuniting, sintering.
3. a kind of support type mesoporous carbon catalyst RTCC-1 for volatile organic matter low-temperature catalytic burning according to claim 1 and preparation method thereof, it is characterized in that catalyst is made up of noble metal, oxide and TSC-1 mesoporous carbon carrier three parts, wherein noble metal is any one in Pd or Pt, and oxide is one or more in cupric oxide, cerium oxide, zirconia, titanium dioxide, silica, aluminium oxide.
4. a kind of support type mesoporous carbon catalyst RTCC-1 for volatile organic matter low-temperature catalytic burning according to claim 1 and preparation method thereof, is characterized in that at 15～80 DEG C of reaction temperatures, the complete catalytic combustions of VOC gas such as formaldehyde, toluene, benzene being decomposed into CO
2and H
2o.
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