CN105289650A - Preparation method of catalyst used for carrying out catalytic combustion on volatile organic compound containing low-concentration methane - Google Patents
Preparation method of catalyst used for carrying out catalytic combustion on volatile organic compound containing low-concentration methane Download PDFInfo
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Abstract
The invention discloses a preparation method of a catalyst used for carrying out catalytic combustion on a volatile organic compound containing low-concentration methane. The catalyst consists of an active carrier, noble metal and assistant metallic oxide, wherein the noble metal and the assistant metallic oxide are loaded on the active carrier; the quality of the noble metal is 0.05 percent to 0.8 percent of active elements by element quality in final catalyst; the quality of the assistant metallic oxide is 0.0 percent to 20 percent of the quality of the final catalyst; the catalyst is prepared in a way that active ingredients are used as a carrier, and after the active ingredients are processed by aqueous alkali, the active ingredients dip in a solution which loads compound containing the active elements of the noble metal and the assistant metallic oxide, and the obtained product is dried in the shade, dried and roasted. The catalyst is used for the organic volatilization hydrocarbon catalytic combustion which contains low-concentration methane, and the catalytic combustion transformation effect of the methane is excellent while almost complete non-methane hydrocarbon transformation can be obtained.
Description
Technical field
The invention belongs to petrochemical catalyst technical field, be specifically related to the preparation method of the catalyst that a kind of catalytic combustion process uses, particularly relate to a kind of preparation method of noble metal catalyst of catalytic combustion volatility organic compound.
Background technology
Along with developing rapidly of modern industry and transportation, also increase the demand of the energy thereupon, and give off a large amount of pernicious gas in industrial process and cause high risks to health, environmental pollution has become global a great problem.Catalytic oxidation hydro carbons and derivative (comprising low-concentration methane and volatile organic matter) thereof are one and make full use of the energy and accomplish the effective way of pernicious gas zero-emission.Under volatile organic matter (VOCs) typically refers to room temperature, saturated vapor pressure is greater than 133.3Pa, boiling point at the organic compound of the effumability of 50-260 DEG C, mainly comprises fat hydrocarbon, halogenated hydrocarbon, arene and alcohol aldoketones etc.In recent years, VOCs has become the current important presoma and the partner that affect the regional compound pollution of In The Atmosphere Over China.Therefore, develop efficient VOCs end-of-pipe control technology, the discharge capacity of strict control VOCs, has become global important topic.
At present, reported multiple VOCs end-of-pipe control technology, mainly contained Physical and chemical method.Physical comprises absorption method, condensation method and membrane separation process, and this is a kind of nondestructive method, and its advantage to reclaim VOCs, but easily cause secondary pollution; Chemical method comprises burning method, low-temperature plasma method, photocatalytic oxidation, biological treatment and Production by Catalytic Combustion Process etc., and this is a kind of destructive method, and advantage is that VOCs clearance is high, but energy consumption is also high.Wherein Production by Catalytic Combustion Process has the advantages such as efficient and energy consumption is relatively low, effectively multiple VOCs can be oxidized to CO
2and H
2o, thus cause and study widely.The method is mainly catalyst with metal oxide, this catalysis has two large classes: noble metal and transition metal oxide, noble metal catalyst mainly refers to the catalyst such as Pd, Pt of support type, and catalyst of transition metal oxide then comprises the transition metal oxide of the various metals such as Mn, V, Fe, Co, Cu.According to the difference of the VOCs of process, suitable catalyst is selected to process.Because VOCs is of a great variety, development is efficient, universality is strong, the catalyst of good stability, has become the key point that Production by Catalytic Combustion Process administers VOCs pollutant in industrial tail gas.General VOCs does not comprise methane content, because methane is stable especially not easily carry out catalytic combustion conversion, but often containing a certain amount of methane in the petrochemical industry discharge VOCs component in reality, if one can be developed can process VOCs, the catalyst for catalytic combustion that also can process low-concentration methane is a research topic being rich in challenge and actual application value, has very wide application prospect.
The methyl hydride combustion process catalyst of current excellence mainly concentrates on noble metal catalyst, properties of perovskite mixed-oxide etc., wherein precious metal catalyst is the most excellent, but active component Pd/Pt etc. are expensive, limit its application to the requirements such as raw material impurity are higher; Perovskite type composite oxide catalyst better heat stability, but when processing the volatile organic content containing methane, its low temperature active is poor, methane poor processing effect.American Studies personnel etc. (Science, 2000,403:65-67) develop a kind of " core-shell structure copolymer " nanostructured newly CeO2-BHA noble metal catalyst, and precious metal palladium particle diameter only has 1.8nm.This catalyst is stronger 30 times than the methyl hydride combustion catalyst used at present, and methane substantially can burn completely at 400 DEG C.Shortcoming is that preparation is complicated, and catalyst cost is too high.Article (AppliedCatalysisA:General203 (2000) 37-45) develops a kind of free from chloride precious metals pd load methyl hydride combustion catalyst, substantially the complete catalytic combustion of methane can be completed at 420 DEG C, shortcoming is catalyst long-term operation under having water vapour to exist, and methane conversion reduces.Article (AppliedCatalysisA:General226 (2002) 281-291) studies in great detail at steam at two supporting Pt-Pd/Al
2o
3methyl hydride combustion impact on catalyst, develop a kind of methyl hydride combustion catalyst of resistance to steam, shortcoming is that catalyst preparing flow process is longer, and catalyst cost is higher.
Based on above article and patent analyses, prior art prepares loaded noble metal catalyst in process containing in the VOCs burning of methane content, and ubiquity noble-metal-supported amount is high, cost is high or there is the problems such as preparation link is complicated, the active reduction of catalyst long period methyl hydride combustion.The preparation method of noble metal catalyst on the serviceability impact of catalyst obviously, for the noble metal catalyst in different application field, must carry out the preparation method be suitable for.
Summary of the invention
Technical problem to be solved by this invention is for above-mentioned deficiency of the prior art, provide a kind of can the preparation method of the simultaneously catalyst of catalytic combustion low-concentration methane and VOCs.Catalyst prepared by the method is for containing in the VOCs of low-concentration methane, can while obtaining higher methane conversion, completely by other VOCs catalytic combustion, final organic emission index reaches state environmental emissioning standard, this catalyst activity is high, has good adaptability to raw materials and cost is low.
For solving the problems of the technologies described above, the technical solution used in the present invention is: this catalyst is made up of the noble metal of active carrier and load thereon and auxiliary agent metal oxides; Wherein the quality of noble metal be its active element by final catalyst in 0.05% ~ 0.8% of element quality, the quality of auxiliary agent metal oxides is 0.0% ~ 20% of final catalyst quality; This catalyst is carrier with active component, and after alkaline solution treatment, dip loading is containing the solution of noble metal active element and auxiliary agent metal oxides compound, obtained through drying in the shade, after dry and roasting; Specifically comprise the following steps:
(1) active carrier modification: under the condition of temperature 80 ~ 90 DEG C, active carrier is placed in certain density dilute sodium hydroxide process 2 ~ 3h, then by deionized water, carrier is washed till neutrality, the baking oven being placed in 110 ~ 120 DEG C is dried, the active carrier of obtained porous;
(2) preparation of maceration extract: prepare active component precious metals pd or/and the solution of Pt by the percentage by weight of component each in catalyst, or containing the solution of precious metal ion and the mixed solution of promoter metal nitrate, obtain maceration extract;
(3) preparation of catalyst: under normal temperature and pressure conditions, treated active carrier in step (1) is placed in the medium volume impregnation process of maceration extract described in step (2), then by the dry 6 ~ 12h at 100 ~ 150 DEG C of the active carrier after dipping, finally by dried active carrier roasting 3 ~ 6h under 500 ~ 800 DEG C of conditions, obtain VOCs catalyst for catalytic combustion.
Adopt technique scheme, containing the VOCs catalyst for catalytic combustion of low-concentration methane, be carrier with active component, after alkaline solution treatment, dip loading is containing the solution of noble metal active element and auxiliary agent metal oxides compound, and through drying in the shade, dry and roasting obtains final catalyst; This catalyst can simultaneously catalytic combustion low-concentration methane and VOCs gas or both mists, can while obtaining higher methane conversion, completely by other VOCs catalytic combustion, final organic emission index reaches state environmental emissioning standard, this catalyst activity is high, has good adaptability to raw materials; And preparation method's cost of this catalyst is low, is applicable to extensive popularization.
Further improvement is, the active carrier in described step (1) is Al
2o
3or TiO
2or Ti-Al composite oxide carrier.Catalyst carrier can be prepared into suitable shape as required; For the carrier commercially bought or storage time longer carrier, all dry certain hours at 80 ~ 120 DEG C before using and to dry process.
Further improvement is, the specific area of the described active carrier in described step (1) is 200
2/ g ~ 320m
2/ g, pore volume is 0.3ml/g ~ 0.6ml/g.
Further improvement is, the concentration of the described sodium hydroxide solution in described step (1) is 0.8 ~ 1.2mol/L, and the mass ratio of sodium hydroxide solution and active carrier is 5 ~ 8:1.
As preferred version of the present invention, the active element component of noble metal is Pt and/or Pd.
As preferred version of the present invention, the quality of noble metal be its active element by final catalyst in 0.1% ~ 0.5% of element quality.
As preferred version of the present invention, in described step (2), the compound of active component precious metals pd and Pt is palladium nitrate and four ammino platinum nitrates respectively.
As preferred version of the present invention, described in described step (2), promoter metal nitrate is Ni (NO
3)
2and/or Ce (NO
3)
3.
As preferred version of the present invention, described auxiliary agent metal oxides is transformed after being through described promoter metal nitrate load roasting, and auxiliary agent metal oxides is NiO and/or CeO
2.
As preferred version of the present invention, in described step (3), dip time is 30 ~ 120 minutes, and the atmosphere of roasting is air.
Compared with catalyst prepared by the catalyst for catalytic combustion adopting method of the present invention to prepare and existing method, preparation process is simple, bullion content is lower, formed activity stabilized through high-temperature roasting with another kind of promoter metal, the alloy that catalytic effect is more excellent, the catalyst noble metal dispersion of preparation evenly, particle diameter is less, catalyst activity and stability all mention raising.
The present invention compared with prior art has the following advantages:
1, the carrier that catalyst of the present invention is used processes through alkaline solution before impregnated activated component, carrier after process is provided with larger pore volume, the active component of catalyst for catalytic combustion is made to have better decentralization at carrier surface, significantly improve catalytic activity and stability, accelerate the oxidation rate of VOC molecule (VOCs), significantly reduce reaction temperature.
2, the catalyst prepared of the inventive method when with existing catalyst performance close to, utilize and add the consumption that transition metal decreases noble metal significantly, reduce catalyst cost.Active component particle diameter is less simultaneously, and active component is more stable mutually, not easily leakage occurs, the significant stability improving catalyst.
3, first the present invention carries out alkali treatment modifying to active carrier, the Al on its surface (Lewis acid position) is removed through alkali treatment, effectively can improve the distribution of carrier surface acidity like this and expand catalyst pore volume, again by the modification of transition metal total immersion stain, make the more smooth weight of electric transmission between oxidationreduction further, significantly improve activity and the hydrothermal stability of catalyst.
4, catalyst of the present invention is low for solving methane conversion in prior art in organic volatile compound (VOCs) reaction of catalytic combustion low-concentration methane under the process conditions that relative temperature is lower, the problems such as poor catalyst stability, there is methane catalytic combustion conversion ratio high, the features such as catalyst stability is good.
Accompanying drawing explanation
Fig. 1 is catalyst preparing schematic flow sheet of the present invention;
Fig. 2 is the transmission electron microscope figure (TEM) of catalyst A prepared by the embodiment of the present invention 1;
Fig. 3 is the transmission electron microscope figure (TEM) of the catalyst G of comparative example 1 of the present invention preparation.
Detailed description of the invention
Give further instruction below by specific embodiment to technology of the present invention, but the preparation method of catalyst of the present invention is not limited to the following example.Percentage composition is wherein mass fraction; Preparation flow as shown in Figure 1.
Embodiment 1:
By spherical gamma-Al
2o
3carrier (specific area 320m
2/ g, pore volume 0.4ml/g) in an oven after dry process, 8:1 puts in the NaOH solution of 0.8mol/L in mass ratio, 2 hours are processed at 80 DEG C, washing, after drying, by its incipient impregnation in the solution of palladium nitrate and nickel nitrate, loading Pd is 0.5% of catalyst quality, NiO is 10% of catalyst quality, and dip time is 30 minutes, dries 8 hours for 120 DEG C in the baking oven of air atmosphere, the lower 500 DEG C of roastings of last Muffle furnace air atmosphere 6 hours, obtain catalyst A; Catalyst A is through N
2it is 292m that its specific area is tested in absorption complete analysis
2/ g, pore volume is 0.36ml/g.TEM electronic microscope photos active component particle diameter concentrates on 2 ~ 4nm (as Fig. 2).
Embodiment 2:
By spherical TiO
2carrier (specific area 286m
2/ g, pore volume 0.3ml/g) in an oven after dry process, 5:1 puts in the NaOH solution of 1.2mol/L in mass ratio, at 90 DEG C, process 2 hours, washing, after drying, by its incipient impregnation in the solution of palladium nitrate, four ammino platinum nitrates and cerous nitrate, loading is 0.3%, Pt of catalyst quality by Pd is 0.05%, CeO of catalyst quality
2for 10% of catalyst quality, dip time is 120 minutes, and dry 6 hours for 100 DEG C in the baking oven of air atmosphere, the lower 800 DEG C of roastings of last Muffle furnace air atmosphere 3 hours, obtain catalyst B.Catalyst B is through N
2it is 262m that its specific area is tested in absorption complete analysis
2/ g, pore volume is 0.26ml/g.The particle diameter of TEM electronic microscope photos active component concentrates on 2 ~ 4nm.
Embodiment 3:
By spherical Ti-Al oxide carrier (specific area 200m
2/ g, pore volume 0.5ml/g) in an oven after dry process, 6:1 puts in the NaOH solution of 1.0mol/L in mass ratio, 2 hours are processed at 85 DEG C, washing, after drying, by its incipient impregnation in the solution of palladium nitrate, four ammino platinum nitrates and nickel nitrate, loading Pd is 0.25%, Pt of catalyst quality be 0.10%, NiO of catalyst quality is 15% of catalyst quality, dip time is 90 minutes, dry 10 hours for 150 DEG C in the baking oven of air atmosphere, the lower 700 DEG C of roastings of last Muffle furnace air atmosphere 5 hours, obtain catalyst C.Catalyst C is through N
2it is 202m that its specific area is tested in absorption complete analysis
2/ g, pore volume is 0.46ml/g.TEM electronic microscope photos active component particle diameter concentrates on 3 ~ 8nm.
Embodiment 4:
By spherical gamma-Al
2o
3carrier (specific area 220m
2/ g, pore volume 0.6ml/g) in an oven after dry process, 6:1 puts in the NaOH solution of 1.0mol/L in mass ratio, at 85 DEG C, process 2 hours, washing, after drying, by its incipient impregnation in the solution of palladium nitrate, four ammino platinum nitrates and nickel nitrate, loading Pd is 0.05%, Pt of catalyst quality be 0.20%, NiO of catalyst quality is 15% of catalyst quality.Dip time is 60 minutes, and dry 6 hours for 120 DEG C in the baking oven of air atmosphere, the lower 700 DEG C of roastings of last Muffle furnace air atmosphere 5 hours, obtain catalyst D.Catalyst D is through N
2it is 202m that its specific area is tested in absorption complete analysis
2/ g, pore volume is 0.46ml/g.TEM electronic microscope photos active component particle diameter concentrates on 2 ~ 5nm.
Embodiment 5:
By spherical gamma-Al
2o
3carrier (specific area 220m
2/ g, pore volume 0.6ml/g) in an oven after dry process, 6:1 puts in the NaOH solution of 1.0mol/L in mass ratio, at 85 DEG C, process 2 hours, washing, after drying, by its incipient impregnation in palladium nitrate, in the solution of cerous nitrate and nickel nitrate, loading Pd is 0.5%, CeO of catalyst quality
2for 10%, NiO of catalyst quality is 5% of catalyst quality, dip time is 60 minutes, and dry 6 hours for 120 DEG C in the baking oven of air atmosphere, the lower 700 DEG C of roastings of last Muffle furnace air atmosphere 5 hours, obtain catalyst E.Catalyst E is through N
2it is 182m that its specific area is tested in absorption complete analysis
2/ g, pore volume is 0.36ml/g.TEM electronic microscope photos active component particle diameter concentrates on 2 ~ 5nm.
Embodiment 6:
By spherical gamma-Al
2o
3carrier (specific area 220m
2/ g, pore volume 0.6ml/g) in an oven after dry process, 6:1 puts in the NaOH solution of 1.0mol/L in mass ratio, at 85 DEG C, process 2 hours, washing, after drying, by its incipient impregnation in the solution of palladium nitrate, four ammino platinum nitrates and cerous nitrate, loading Pd is 0.05%, Pt of catalyst quality is 0.05%, CeO of catalyst quality
2for 15% of catalyst quality, dip time is 60 minutes, and dry 6 hours for 120 DEG C in the baking oven of air atmosphere, the lower 700 DEG C of roastings of last Muffle furnace air atmosphere 5 hours, obtain catalyst F.Catalyst F is through N
2it is 192m that its specific area is tested in absorption complete analysis
2/ g, pore volume is 0.5ml/g.TEM electronic microscope photos active component particle diameter concentrates on 2 ~ 5nm.
Comparative example 1:
By spherical gamma-Al
2o
3carrier (specific area 320m
2/ g, pore volume 0.4ml/g) in an oven after dry process, by its incipient impregnation in the solution of palladium nitrate and nickel nitrate, loading Pd is 0.5%, NiO of catalyst quality is 10% of catalyst quality.Dip time is 30 minutes, and dry 8 hours for 120 DEG C in the baking oven of air atmosphere, the lower 500 DEG C of roastings of last Muffle furnace air atmosphere 6 hours, obtain catalyst G.
Catalyst G is through N
2it is 292m that its specific area is tested in absorption complete analysis
2/ g, pore volume is 0.24ml/g.TEM electronic microscope photos active component particle diameter concentrates on 3 ~ 8nm (as shown in Figure 3).
Comparative example 2:
By spherical gamma-Al
2o
3carrier (specific area 320m
2/ g, pore volume 0.4ml/g) in an oven after dry process, 6:1 puts in the NaOH solution of 1.0mol/L in mass ratio, at 85 DEG C, process 2 hours, washing, after drying, by its incipient impregnation in the solution of palladium nitrate, loading Pd is 0.5% of catalyst quality, dip time is 60 minutes, dry 6 hours for 120 DEG C in the baking oven of air atmosphere, the lower 700 DEG C of roastings of last Muffle furnace air atmosphere 5 hours, obtain catalyst H.Catalyst H is through N
2it is 312m that its specific area is tested in absorption complete analysis
2/ g, pore volume is 0.49ml/g.TEM electronic microscope photos active component particle diameter concentrates on 3 ~ 8nm.
Embodiment 7:
Catalyst above-described embodiment and comparative example prepared carries out catalytic combustion properties evaluation, and choose simulated exhaust as process to picture, the NMHC concentration of this waste gas is 3000 ~ 5000mg/m
3, methane hydrocarbon concentration is 500mg/m
3, reaction velocity is 20000h
-1, inlet temperature 350 DEG C, within 4 hours, evaluation result is in table 1.
The catalytic combustion properties of table 1 embodiment 1 ~ 6 and the catalyst prepared by comparative example 1 ~ 2 evaluates comparing result
Tested as can be seen from comparative evaluation, the catalyst taking the method to prepare can well comprise the organic hydrocarbon of methane by catalytic combustion, its Catalytic Combustion Effect is higher than other preparation method, the catalyst noble metal content taking transition metal promoter technology obtained is low relative to methyl hydride combustion catalyst, catalytic effect is more excellent, has good prospects for commercial application.
The above; it is only preferred embodiment of the present invention; not the present invention is imposed any restrictions, every above embodiment is done according to the technology of the present invention essence any simple modification, change and equivalent structure change, all still belong in the protection domain of technical solution of the present invention.
Claims (10)
1. catalytic combustion is containing the preparation method of catalyst of the VOCs of low-concentration methane, and this catalyst is made up of the noble metal of active carrier and load thereon and auxiliary agent metal oxides; Wherein the quality of noble metal be its active element by final catalyst in 0.05% ~ 0.8% of element quality, the quality of auxiliary agent metal oxides is 0.0% ~ 20% of final catalyst quality; This catalyst is carrier with active component, and after alkaline solution treatment, dip loading is containing the solution of noble metal active element and auxiliary agent metal oxides compound, obtained through drying in the shade, after dry and roasting; Specifically comprise the following steps:
(1) active carrier modification: under the condition of temperature 80 ~ 90 DEG C, active carrier is placed in certain density dilute sodium hydroxide alkali treatment 2 ~ 3h, then by deionized water, carrier is washed till neutrality, the baking oven being placed in 110 ~ 120 DEG C is dried, the active carrier of obtained porous;
(2) preparation of maceration extract: prepare active component precious metals pd or/and the solution of Pt by the percentage by weight of component each in catalyst, or containing the solution of precious metal ion and the mixed solution of promoter metal nitrate, obtain maceration extract;
(3) preparation of catalyst: under normal temperature and pressure conditions, treated active carrier in step (1) is placed in the medium volume impregnation process of maceration extract described in step (2), then by the dry 6 ~ 12h at 100 ~ 150 DEG C of the active carrier after dipping, finally by dried active carrier roasting 3 ~ 6h under 500 ~ 800 DEG C of conditions, obtain VOCs catalyst for catalytic combustion.
2. catalytic combustion according to claim 1 is containing the preparation method of the catalyst of the VOCs of low-concentration methane, and it is characterized in that, the active carrier in described step (1) is Al
2o
3or TiO
2or Ti-Al composite oxide carrier.
3. catalytic combustion according to claim 2 is containing the preparation method of the catalyst of the VOCs of low-concentration methane, and it is characterized in that, the specific area of the described active carrier in described step (1) is 200
2/ g ~ 320m
2/ g, pore volume is 0.3ml/g ~ 0.6ml/g.
4. catalytic combustion according to claim 1 is containing the preparation method of the catalyst of the VOCs of low-concentration methane, it is characterized in that, the concentration of the described sodium hydroxide solution in described step (1) is 0.8-1.2mol/L, and the mass ratio of sodium hydroxide solution and active carrier is 5 ~ 8:1.
5. catalytic combustion according to claim 1 is containing the preparation method of the catalyst of the VOCs of low-concentration methane, and it is characterized in that, the active element component of noble metal is Pt and/or Pd.
6. catalytic combustion contains the preparation method of the catalyst of the VOCs of low-concentration methane according to claim 1 or 5, it is characterized in that, the quality of noble metal be its active element by final catalyst in 0.1% ~ 0.5% of element quality, the quality of auxiliary agent metal oxides is 10% ~ 15% of final catalyst quality.
7. catalytic combustion according to claim 6 is containing the preparation method of the catalyst of the VOCs of low-concentration methane, it is characterized in that, in described step (2), the compound of active component precious metals pd and Pt is palladium nitrate and four ammino platinum nitrates respectively.
8. catalytic combustion according to claim 7 is containing the preparation method of the catalyst of the VOCs of low-concentration methane, and it is characterized in that, described in described step (2), promoter metal nitrate is Ni (NO
3)
2and/or Ce (NO
3)
3.
9. catalytic combustion according to claim 8 is containing the preparation method of the catalyst of the VOCs of low-concentration methane, it is characterized in that, described auxiliary agent metal oxides is transformed after being through described promoter metal nitrate load roasting, and auxiliary agent metal oxides is NiO and/or CeO
2.
10. catalytic combustion according to claim 9 is containing the preparation method of the catalyst of the VOCs of low-concentration methane, it is characterized in that, in described step (3), dip time is 30 ~ 120 minutes, and the atmosphere of roasting is air.
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