CN107442106A - The preparation method of VOCs catalytic decomposition O composite metallic oxide catalysts - Google Patents
The preparation method of VOCs catalytic decomposition O composite metallic oxide catalysts Download PDFInfo
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Abstract
The invention discloses the preparation method of VOCs catalytic decomposition O composite metallic oxide catalysts, with nanometer powder TiO2As carrier, transition metal salt is added after forming metal composite oxide layer, the O composite metallic oxide catalyst of multicomponent reactive component is formed after heat treatment.In low light-off temperature(300℃)Under there is higher catalysis oxidation ability to esters and benzene type organic(>98%).Catalyst is prepared using the normal temperature precipitation method, method is easy.And precious metal element is free of, cost is cheap.Prepared using two-step precipitation, it is ensured that Ce and TiO2It is in close contact, is easy to form solid solution during roasting, there is good oxygen delivery capacity.The transition metal of final load is uniformly distributed in catalyst surface, beneficial to the absorption to VOCs molecules, there is provided avtive spot, improves catalytic capability.Obtained catalyst is used for VOCs being oxidized to CO2And H2O, there is high catalytic conversion efficiency, low light-off temperature, high stability, cheap, there is good application value and prospect.
Description
Technical field
The present invention relates to environmental protection technical field, specially VOCs catalytic decompositions O composite metallic oxide catalyst
Preparation method.
Background technology
Volatile organic matter VOCs(volatile organic compounds), refer to that saturated vapor pressure is more than under normal temperature
Organic compound of the boiling point below 260 DEG C under 70 Pa, normal pressure, or vapour pressure is more than or equal to 10 Pa under the conditions of 20 DEG C
With corresponding volatile whole organic compounds.VOC presses its chemical constitution, can be further divided into:Alkanes, aromatic hydrocarbons, ester
Class, aldehydes and other etc..What is identified at present has kind more than 300.It is most common to have benzene,toluene,xylene, styrene, trichlorine
Ethene, chloroform, trichloroethanes, diisocyanate(TDI), two isocyanide toluene esters etc..Volatile organic in room air
It is easy to cause acute poisoning during compound excessive concentration, headache, dizziness, cough, Nausea and vomiting or in dead drunk liquor-saturated occurs in the lighter
Shape;Hepatotoxicity occurs or even goes into a coma quickly, and some there may also be life danger in severe one.
Industrial VOCs purification techniques mainly has absorption process, absorption method, condensation method, biochemical process, low temperature plasma at present
Method, photocatalytic oxidation and Production by Catalytic Combustion Process etc..Production by Catalytic Combustion Process is current most widely used VOCs purification techniques, refers to utilization
Activation energy required for the reaction of catalyst degradation oxidation operation, improves reaction efficiency, VOCs is carried out into nothing at a lower temperature
Flame burns, and is eventually converted into CO2And H2The innocuous substances such as O.At present, VOCs catalysts for treating mainly includes noble metal(Pd、
Pt, Ru etc.), transition metal(Cu, Mn, Mo, Ni, Co, Fe, Cr etc.)And rare earth metal(Ce, La etc.)And other composite oxides.
Although noble metal catalyst catalytic efficiency is higher, expensive, this limits the popularization and application of catalyst to a certain extent.
Therefore, it is technical problem urgently to be resolved hurrily at present to prepare high-performance and cheap catalyst.
The content of the invention
It is an object of the invention to provide one kind to have high catalytic activity, low light-off temperature, long life and cost low
Honest and clean new VOCs oxidation catalysts.Semiconductor TiO2As carrier, the CeO of generation2With TiO2Eutectic is formed to provide very well
Oxygen delivery capacity, the element such as Ag, Cu, Ni, Fe, Co, Mo, Mn that surface is formed after high-temperature roasting can effectively adsorb oxygen, compound
The synergy of metal oxide each component improves catalysis oxidation ability of the catalyst to VOCs gases.Prepared with this technology
Catalyst, not only catalytic capability is efficient but also cheap, can be widely popularized use, to solve to propose in above-mentioned background technology
The problem of.
To achieve the above object, the present invention provides following technical scheme:A kind of VOCs catalytic decompositions are aoxidized with composition metal
The preparation method of thing catalyst, comprises the following steps:
Step 1, by appropriate nano-TiO purchased in market2Powder is dissolved in distilled water, is configured to 0.05 M solution;
Step 2: take a certain amount of Ce (NO3)3•6H2O is dissolved in step 1 resulting solution, and stirring and dissolving 1H obtains mixing molten
Liquid;
Step 3, take a certain amount of NaOH and NH3•H2O is configured to 0.1 M precipitating reagent, and precipitating reagent is added with vigorous stirring
Enter in step 2 solution;
Step 4, after the solution that step 3 obtains is well mixed, heating stirring 1H in 80 DEG C of oil baths is placed in, is put into after filtering while hot
12H is dried in 80 DEG C of baking ovens, obtains Ce/TiO2Mixture powder;
Step 5, the solid powder that step 4 is obtained again disperse after, weigh a certain amount of transition metal salt (Ag, Cu, Ni,
Fe, Co, Mo, Mn) 0.1M solution is configured to, it is 18 ~ 25% additions by theoretical transition metal/cerium titanium mixture quality ratio, then adds
Enter 0.1 M precipitating reagent;
Step 6, after step 5 resulting solution is well mixed, the H of heating stirring 1 in 80 DEG C of oil baths is placed in, is put into after filtering while hot
12 H are dried in 80 DEG C of baking ovens, grinding obtains solid powder;
Step 7, solid powder obtained by step 6 is placed in tube furnace, in 400 DEG C and N2Under atmosphere, 5H is calcined, is obtained compound
Metal oxide catalyst.
Preferably, the mixed solution mol ratio obtained in step 2 is Ce/Ti=3/1 ~ 1/5.
Preferably, it is [OH that precipitating reagent addition, which controls mol ratio, in step 3-]/[Ce3+]=3/1~4/1。
Preferably, O composite metallic oxide catalyst is prepared into slurry and carried coated on ceramics, molecular sieve, the fixed of activated carbon
On body, for being carbon dioxide and water by volatile organic matter oxidation Decomposition.
Preferably, volatile organic matter is included in ethanol, ethyl acetate, toluene, butyl acetate, dimethylbenzene, styrene
It is one or more of.
Compared with prior art, the beneficial effects of the invention are as follows:
(1)In low light-off temperature(300℃)Under there is higher catalysis oxidation ability to esters and benzene type organic(>98%).
(2)The inventive method prepares catalyst using the normal temperature precipitation method, and method is easy.And be free of precious metal element, cost
It is cheap.
(3)Prepared using two-step precipitation, it is ensured that Ce and TiO2It is in close contact, is easy to form solid solution during roasting, has
Good oxygen delivery capacity.The transition metal of final load is uniformly distributed in catalyst surface, beneficial to the suction to VOCs molecules
It is attached, there is provided avtive spot, to improve catalytic capability.
To sum up, the catalyst that the present invention is prepared is used for VOCs being oxidized to CO2And H2O, there is high catalyzed conversion effect
Rate, low light-off temperature, high stability, it is cheap the advantages that, there is good application value and prospect.
Embodiment
The technical scheme in the embodiment of the present invention will be clearly and completely described below, it is clear that described implementation
Example only part of the embodiment of the present invention, rather than whole embodiments.It is common based on the embodiment in the present invention, this area
The every other embodiment that technical staff is obtained under the premise of creative work is not made, belong to the model that the present invention protects
Enclose.
The preparation method of VOCs catalytic decomposition O composite metallic oxide catalysts, with nanometer powder TiO2As carrier,
Transition metal salt is added after forming metal composite oxide layer, the metal composite oxide of multicomponent reactive component is formed after heat treatment
Catalyst, comprise the following steps that:
Step 1: by appropriate commercially available nano-TiO2Powder (P25) is dissolved in distilled water, is configured to 0.05 M solution.
Step 2: take a certain amount of Ce (NO3)3•6H2O is added in step 1 resulting solution, stirring and dissolving 1H.Wherein, control
Mol ratio Ce/Ti=3/1 ~ 1/5 processed.
Step 3: take a certain amount of NaOH and NH3•H2O is configured to 0.1M precipitating reagent, by precipitating reagent with vigorous stirring
Add in step 2 solution, it is [OH that addition, which controls mol ratio,-]/[Ce3+]=3/1~4/1。
Step 4: after above-mentioned solution is well mixed, it is placed in heated at constant temperature in 80 DEG C of oil baths and stirs 1H, be put into after filtering while hot
12H is dried in 80 DEG C of baking ovens, obtains Ce/TiO2Mixture powder.
Step 5: after above-mentioned solid powder is disperseed again, weighing a certain amount of transition metal salt, (Mn is configured to 0.1 M
Solution, by theoretical transition metal/Ce/TiO2Mix body mass ratio=18 ~ 25% to add, then add 0.1 M precipitating reagent.
Step 6: after above-mentioned solution is well mixed, it is placed in heated at constant temperature in 80 DEG C of oil baths and stirs 1H, be put into after filtering while hot
12 H are dried in 80 DEG C of baking ovens, grinding obtains solid powder.
Step 7: above-mentioned solid is placed in tube furnace, in 400 DEG C and N2Under atmosphere, 5H is calcined, obtains composition metal oxygen
Compound catalyst.
The above-mentioned catalyst being prepared is used for catalysis oxidation VOCs gases, reaction condition is 220 ~ 400 DEG C, by VOCs
Oxidation Decomposition is CO2And H2O.The volatile organic matter includes ethanol, ethyl acetate, toluene, butyl acetate, dimethylbenzene, benzene second
It is one or more of in alkene.
Embodiment 1
(1)Weigh 3.32 g TiO2Powder is placed in 1000 mL conical flasks, adds the min of 400 mL distilled water stirring and dissolving 30.
(2)Weigh 3.61 g Ce (NO3)3•6H2O adds above-mentioned(1)In solution, continue the min of stirring and dissolving 30.
(3)Weigh 1.6 g NaOH+20 mL NH3•H2O, add 400 mL distilled water stirring and dissolvings and precipitating reagent is made.
(4)Precipitating reagent is placed in separatory funnel, is added dropwise with vigorous stirring(2)Resulting solution, after being added dropwise,
Conical flask is placed in oil bath pan, filtered while hot after stirring 1H at 80 DEG C of constant temperature, gained solid is in 80 DEG C of baking ovens
10H is dried, grinds to obtain Ce/TiO2Mixture A.
(5)Take(4)The g of gained mixture A 0.95, add in 150 mL distilled water, the min of stirring and dissolving 30.Weigh Cu
(NO3)20.33 g is added, and continues the min of stirring and dissolving 30.
(6)Weigh 0.16 g NaOH+2 mL NH3•H2O, add stirring and dissolving in 40 mL distilled water and precipitating reagent is made.
(7)Precipitating reagent is placed in separatory funnel, is added dropwise with vigorous stirring(5)Resulting solution, after being added dropwise,
Conical flask is placed in oil bath pan, filtered while hot after stirring 1H at 80 DEG C of constant temperature, gained solid is in 80 DEG C of baking ovens
10H is dried, grinds to obtain solid powder B.
(8)Solid powder B is placed in tube furnace, at 400 DEG C and N2Under atmosphere, 5H is calcined, obtains metal composite oxide
Catalyst.
(9)Above-mentioned catalyst is used to handle VOCs gases, wherein, active testing condition:300 DEG C of temperature, concentration 900-
1100ppm, gases used detection is ethanol:Ethyl acetate:Toluene:Butyl acetate:Dimethylbenzene:Styrene solution by volume 3:
3:1:3:3:3 are blended in the gas evaporated at 50 DEG C.Experimental facilities:VOCs catalysis oxidations gas chromatographic detection evaluation dress
Put.
Embodiment 2
(1)Weigh 0.332 g TiO2Powder is placed in 250 mL conical flasks, adds the min of 100 mL distilled water stirring and dissolving 30.
(2)Weigh 0.361 g Ce (NO3)3•6H2O adds above-mentioned(1)In solution, continue the min of stirring and dissolving 30.
(3)Weigh 0.16 g NaOH+2 mL NH3•H2O, add 40mL distilled water stirring and dissolving and precipitating reagent is made.
(4)Precipitating reagent is placed in separatory funnel, is added dropwise with vigorous stirring(2)Resulting solution, it is added dropwise
Afterwards, conical flask is placed in oil bath pan, 1H is stirred at 80 DEG C of constant temperature.
(5)Weigh 0.17 g AgNO3It is placed in after being dissolved in 50 mL distilled water in separatory funnel.(4)Solution is reduced to
It is added dropwise while stirring after room temperature.
(6)Weigh 0.16 g NaOH+2 mL NH3•H2O, add stirring and dissolving in 40 mL distilled water and precipitating reagent is made.
(7)Precipitating reagent is placed in separatory funnel, is added dropwise with vigorous stirring(5)Resulting solution, after being added dropwise,
Conical flask is placed in oil bath pan, filtered while hot after stirring 1H at 80 DEG C of constant temperature, gained solid is in 80 DEG C of baking ovens
10H is dried, grinds to obtain solid powder.
(8)Solid powder is placed in tube furnace, at 400 DEG C and N2Under atmosphere, 5H is calcined, metal composite oxide is obtained and urges
Agent.
(9)Above-mentioned catalyst is used to handle VOCs gases, wherein, active testing condition:300 DEG C of temperature, concentration 900-
1100 ppm, gases used detection is ethanol:Ethyl acetate:Toluene:Butyl acetate:Dimethylbenzene:Styrene solution is by volume
3:3:1:3:3:3 are blended in the gas evaporated at 50 DEG C.Experimental facilities:VOCs catalysis oxidations gas chromatographic detection evaluation dress
Put.
Embodiment 3
(1)Weigh 3.32 g TiO2Powder is placed in 1000 mL conical flasks, adds the min of 400 mL distilled water stirring and dissolving 30.
(2)Weigh 3.61gCe (NO3)3•6H2O adds above-mentioned(1)In solution, continue the min of stirring and dissolving 30.
(3)Weigh 1.6 g NaOH+20 mL NH3•H2O, add 400 mL distilled water stirring and dissolvings and precipitating reagent is made.
(4)Precipitating reagent is placed in separatory funnel, is added dropwise with vigorous stirring(2)Resulting solution, after being added dropwise,
Conical flask is placed in oil bath pan, filtered while hot after stirring 1H at 80 DEG C of constant temperature, gained solid is in 80 DEG C of baking ovens
10H is dried, grinds to obtain Ce/TiO2Mixture A.
(5)Take(4)The g of gained mixture A 0.95, add in 150 mL distilled water, the min of stirring and dissolving 30.Weigh anhydrous
MnCl20.48 g is added, and continues stirring and dissolving 30min.
(6)Weigh 0.16 g NaOH+2 mL NH3•H2O, add stirring and dissolving in 40 mL distilled water and precipitating reagent is made.
(7)Precipitating reagent is placed in separatory funnel, is added dropwise with vigorous stirring(5)Resulting solution, after being added dropwise,
Conical flask is placed in oil bath pan, filtered while hot after stirring 1H at 80 DEG C of constant temperature, gained solid is in 80 DEG C of baking ovens
10H is dried, grinds to obtain solid powder B.
(8)Solid powder B is placed in tube furnace, at 400 DEG C and N2Under atmosphere, 5H is calcined, obtains metal composite oxide
Catalyst.
(9)Above-mentioned catalyst is used to handle VOCs gases, wherein, active testing condition:300 DEG C of temperature, concentration 900-
1100 ppm, gases used detection is ethanol:Ethyl acetate:Toluene:Butyl acetate:Dimethylbenzene:Styrene solution is by volume
3:3:1:3:3:3 are blended in the gas evaporated at 50 DEG C.Experimental facilities:VOCs catalysis oxidations gas chromatographic detection evaluation dress
Put.
In preparation method of the present invention, Ce/Ti=3/1 ~ 1/5, transition metal and cerium magnesium-titanium solid solution mass ratio be 10% ~
30%, isothermal reaction condition is 70 ~ 90 DEG C and is stirred vigorously the min of 30 min ~ 90, is placed in after being dried in 80 DEG C of baking ovens in tube furnace,
5H is calcined under 400 DEG C and nitrogen atmosphere final catalyst is made.
Although invention has been described for examples detailed above, the invention is not limited in above-mentioned specific embodiment party
Formula, above-mentioned embodiment is only schematical, rather than restricted.Such as Ce/TiO2The composition deformation of mixture
Can be Ce/Al2O3,Ce/SiO2,Ce/ZrO2,Mn/TiO2, Mn/Al2O3, Mn/SiO2, Mn/ZrO2Deng transition metal
Can be Ag, Cr, Cu, Ni, Fe, Co, Mo etc..One of ordinary skill in the art can also make very under the enlightenment of the present invention
Shape changeable, these are belonged in protection scope of the present invention.
Claims (5)
- The preparation method of 1.VOCs catalytic decomposition O composite metallic oxide catalysts, it is characterised in that:Comprise the following steps:Step 1, by appropriate nano-TiO purchased in market2Powder is dissolved in distilled water, is configured to 0.05 M solution;Step 2: take a certain amount of Ce (NO3)3•6H2O is dissolved in step 1 resulting solution, and stirring and dissolving 1H obtains mixing molten Liquid;Step 3, take a certain amount of NaOH and NH3•H2O is configured to 0.1 M precipitating reagent, and precipitating reagent is added with vigorous stirring In step 2 solution;Step 4, after the solution that step 3 obtains is well mixed, heating stirring 1H in 80 DEG C of oil baths is placed in, is put into after filtering while hot 12H is dried in 80 DEG C of baking ovens, obtains Ce/TiO2Mixture powder;Step 5, after the solid powder that step 4 is obtained disperses again, weigh a certain amount of transition metal salt(Ag、Cu、Ni、 Fe、Co、Mo、Mn)0.1M solution is configured to, is 18 ~ 25% additions by theoretical transition metal/cerium titanium mixture quality ratio, then adds Enter 0.1 M precipitating reagent;Step 6, after step 5 resulting solution is well mixed, the H of heating stirring 1 in 80 DEG C of oil baths is placed in, is put into after filtering while hot 12 H are dried in 80 DEG C of baking ovens, grinding obtains solid powder;Step 7, solid powder obtained by step 6 is placed in tube furnace, in 400 DEG C and N2Under atmosphere, 5H is calcined, is obtained compound Metal oxide catalyst.
- 2. the preparation method of VOCs catalytic decompositions O composite metallic oxide catalyst according to claim 1, its feature It is:The mixed solution mol ratio obtained in the step 2 is Ce/Ti=3/1 ~ 1/5.
- 3. the preparation method of VOCs catalytic decompositions O composite metallic oxide catalyst according to claim 1, its feature It is:It is [OH that precipitating reagent addition, which controls mol ratio, in the step 3-]/[Ce3+]=3/1~4/1。
- 4. the preparation method of VOCs catalytic decompositions O composite metallic oxide catalyst according to claim 1, its feature It is:The O composite metallic oxide catalyst is prepared into slurry and is coated on the immobilization carrier of ceramics, molecular sieve, activated carbon, For being carbon dioxide and water by volatile organic matter oxidation Decomposition.
- 5. the preparation method of VOCs catalytic decompositions O composite metallic oxide catalyst according to claim 4, its feature It is:The volatile organic matter include ethanol, ethyl acetate, toluene, butyl acetate, dimethylbenzene, one kind in styrene or It is several.
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