CN111111656A - High-temperature-resistant catalytic combustion catalyst for normal-temperature catalytic ignition of VOCs self-sustaining combustion and preparation method and application thereof - Google Patents
High-temperature-resistant catalytic combustion catalyst for normal-temperature catalytic ignition of VOCs self-sustaining combustion and preparation method and application thereof Download PDFInfo
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
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Abstract
The invention relates to a high-temperature-resistant catalytic combustion catalyst for catalyzing and igniting VOCs (volatile organic compounds) to burn by self at normal temperature, and a preparation method and application thereof, belonging to the field of catalysts. The high-temperature-resistant catalytic combustion catalyst for catalyzing and igniting VOCs to burn in a self-sustaining manner at normal temperature comprises a precious metal active component, an oxygen storage material cerium-zirconium solid solution and a carrier; the carrier contains Al2O3A carrier; wherein, the total weight of the catalyst is 100 parts by weight, the content of the noble metal active component is 0.03-5 parts by weight, the content of the oxygen storage material cerium zirconium solid solution is 5-40 parts by weight, and the balance is a carrier. The catalyst can ignite VOCs material flow containing a certain amount of low unsaturated hydrocarbon and hydrogen at normal temperature (not less than 30 ℃) and normal pressure and realize self-sustaining combustion. Can remove the VOCs waste gas without external auxiliary heating energy, the ignition is quick and effective, and the catalyst has good hydrothermal stabilityQualitative and high-temperature stability, so that the treatment of the VOCs waste gas is greatly simplified.
Description
Technical Field
The invention relates to a high-temperature-resistant catalytic combustion catalyst for normal-temperature catalytic ignition of self-sustaining combustion of VOCs in the field of catalysts, and further relates to a high-temperature-resistant catalytic combustion catalyst for normal-temperature catalytic ignition of self-sustaining combustion of VOCs, and a preparation method and application thereof.
Background
Volatile Organic Compounds (VOCs) are Organic Compounds having a saturated vapor pressure of greater than 70Pa at ambient temperature and a boiling point of less than 260 ℃ at ambient pressure. Mainly comprises aromatic hydrocarbon, aliphatic hydrocarbon, halogenated hydrocarbon, oxygenated hydrocarbon, terpene hydrocarbon, alcohol, aldehyde, ketone, ester and the like. They are the main pollutants in the exhaust gas discharged by petrochemical industry, pharmacy, printing, spray painting and other industries. Most of the organic matters have toxicity and are accompanied by malodor, some of the organic matters can also cause cancer, and most of VOCs have destructive effect on the ozone layer. The society pays more and more attention to the treatment of the VOCs, and common VOCs purification technologies comprise a condensation method, an adsorption method, an absorption method, a catalysis method, a biological method and the like, and the methods are widely applied. The catalytic method is to heat VOCs to the ignition temperature (200-400 ℃) to realize the catalytic and non-catalytic combustion reaction of the VOCs to generate carbon dioxide and water.
The catalysts adopted by the catalytic method at present are supported noble metal catalysts which have the advantages of low ignition temperature and high activity, but have the defects of high price, easy sintering and sublimation inactivation of active components at high temperature, poor stability, low poisoning resistance and the like, so that the application of the supported noble metal catalysts is limited to a certain extent. Researches show that the addition of rare earth and oxides thereof can improve the activity of the catalyst, improve the thermal stability of the catalyst and improve the sulfur resistance and lead resistance of the catalyst. The other is a non-metal catalyst, mainly comprising transition metal oxide catalyst, double oxide catalyst (perovskite type double oxide and spinel type double oxide) and the like, and the catalyst has higher ignition temperature although the high temperature stability is slightly better. The basic requirements of the catalyst for catalytic combustion of VOCs are: good low-temperature catalytic activity, good hydrothermal stability, good high-temperature stability, and good frequent thermal load impact resistance and carbon deposition resistance.
The catalyst adopted by the catalysis method at present is usually required to heat material flow to the ignition temperature (200-400 ℃) and catalyze and non-catalytically combust VOCs to generate carbon dioxide and water, and the catalyst capable of catalyzing and igniting VOCs to burn in a self-sustaining mode at normal temperature is required in the market at present.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides a high-temperature-resistant catalytic combustion catalyst for catalyzing and igniting VOCs to burn in a self-sustaining manner at normal temperature. In particular to a high-temperature resistant catalytic combustion catalyst for catalyzing and igniting VOCs to burn by itself at normal temperature, a preparation method and application thereof. The catalyst can catalyze and ignite VOCs material flow containing a certain amount of low unsaturated hydrocarbon and hydrogen at the temperature of more than or equal to 30 ℃, has good hydrothermal stability and high-temperature stability, and still has good catalytic combustion activity after accelerated aging at the temperature of 1000 ℃.
One of the purposes of the invention is to provide a high-temperature-resistant catalytic combustion catalyst for normal-temperature catalytic ignition of VOCs self-sustaining combustion, which can comprise a noble metal active component, an oxygen storage material cerium-zirconium solid solution and a carrier; the carrier contains Al2O3A carrier;
wherein, the content of the noble metal active component is 0.03 to 5 parts by weight, preferably 0.05 to 3 parts by weight, more preferably 0.05 to 1.5 parts by weight, the content of the oxygen storage material cerium zirconium solid solution is 5 to 40 parts by weight, preferably 10 to 30 parts by weight, and the balance is the carrier, based on 100 parts by weight of the total weight of the catalyst.
Wherein the noble metal active component is selected from Pd and/or Pt.
The oxygen storage material cerium-zirconium solid solution is formed by performing high-temperature solid-phase reaction on a cerium-zirconium solid solution with a cerium-zirconium molar ratio (Ce/Zr) of 0.5-3 at 500-1200 ℃ (preferably 700-900 ℃).
The carrier comprises large-surface Al2O3A carrier; the Al is2O3The specific surface of the carrier can be 100-300 m2/g。
The preparation method of the cerium-zirconium solid solution comprises the following steps:
weighing cerium salt and zirconium salt according to the molar ratio of cerium to zirconium, dissolving the cerium salt and the zirconium salt in an aqueous solution to prepare a mixed solution with a solute total concentration of 0.1-5 mol/L (preferably 0.2-2 mol/L), diluting 25 wt% of ammonia water to 0.1-10 wt% (preferably 1-5 wt%) of the mixed solution to be used as a precipitator, placing the mixed solution in a three-neck flask, slowly dripping the mixed solution of cerium salt and zirconium salt under the condition of vigorous stirring until the pH value of the solution is 9-11, continuing stirring after dripping, standing overnight, washing with deionized water, filtering, drying a filter cake, then programming the temperature to 500-1200 ℃ under flowing air, preferably 700-900 ℃, roasting, and preparing the catalyst aid, namely the cerium-zirconium solid solution.
The cerium salt can be selected from cerium nitrate, cerium sulfate and cerium acetate;
the zirconium salt may be selected from zirconyl nitrate, zirconium oxychloride, or zirconium tetrachloride.
The invention also aims to provide a preparation method of the high-temperature-resistant catalytic combustion catalyst for catalyzing and igniting VOCs to burn by self at normal temperature. The method can be selected from common wet forming methods.
The wet forming method may specifically include the following steps:
mixing oxygen storage material cerium zirconium solid solution, auxiliary agent and Al2O3And kneading and extruding the carrier and a forming assistant for forming, drying at 80-120 ℃ for 3-10 h, roasting at 250-600 ℃ for 3-5 h to obtain the catalyst carrier, soaking the required noble metal active component in an equal volume, drying at 80-120 ℃ for 3-10 h, and roasting at 250-600 ℃ for 3-5 h to obtain the catalyst carrier.
The forming auxiliary agent can be selected from a binder, an extrusion aid and the like; the molding can be in the shapes of strips, raschig rings, honeycombs and the like. The molding aid can be used in an amount of Al2O3The carrier is 0.5-3% of the weight and can be adjusted according to actual conditions.
The auxiliary agent is selected from sol; the sol may be at least one selected from titanium sol, silica sol, water glass and silane. The dosage of the auxiliary agent is Al2O31-5% of the weight of the carrier.
The invention also aims to provide the application of the high-temperature-resistant catalytic combustion catalyst for the self-sustained combustion of the normal-temperature catalytic ignition VOCs in the normal-temperature catalytic ignition of VOCs material flow.
Wherein the stream of VOCs may comprise waste VOCs with low unsaturation and hydrogen;
the low unsaturated hydrocarbon can comprise C2-C4 alkene, alkyne, dialkene and the like;
the low unsaturated hydrocarbon can account for 10-60% of the volume of the VOCs material flow;
the hydrogen can account for 5-20% by volume of the VOCs stream.
The normal-temperature catalytic ignition VOCs self-sustaining combustion catalyst provided by the invention takes precious metal as an active component, takes cerium-zirconium solid solution as an auxiliary agent and takes alumina with a large specific surface as a carrier.
The substantial difference between the present invention and the prior art is: the catalyst can catalyze and ignite VOCs material flow containing a certain amount of low unsaturated hydrocarbon and hydrogen at the temperature of more than or equal to 30 ℃, and has good hydrothermal stability and high-temperature stability.
The invention has the beneficial effects that: the catalyst provided by the invention can ignite VOCs material flow containing a certain amount of low unsaturated hydrocarbon and hydrogen at normal temperature (not less than 30 ℃) and normal pressure and realize self-sustaining combustion. Can be under the condition that does not need the outside auxiliary heating energy, get rid of VOCs waste gas, it is quick effective to ignite to the catalyst has good hydrothermal stability and high temperature stability, makes the processing of handling this type of VOCs waste gas simplify greatly.
Detailed Description
The present invention will be further described with reference to the following examples. However, the present invention is not limited to these examples.
Example 1
43g of cerium nitrate and 27g of zirconyl nitrate were weighed out to give a mixture of 0.25mol/LAnd (2) taking 85g of 25 wt% ammonia water to dilute to 5 wt% as a precipitator, placing the ammonia water in a three-neck flask, slowly dripping a mixed solution of cerium nitrate and zirconyl nitrate under the condition of vigorous stirring until the pH value of the solution is 9-11, continuing stirring for 0.5h after dripping is finished, standing and aging overnight, washing with deionized water, filtering, drying a filter cake at 100 ℃ for 5h, and then carrying out temperature programming to 900 ℃ under flowing air for roasting for 5h to prepare the catalyst aid, namely the cerium-zirconium solid solution CZ 1. CZ1 with a specific surface area of 250m2Alumina (Zibo major alumina science and technology ltd., model 80150) in a/g ratio of CZ1 to alumina 3:7, silica sol assistant JH-40 in 3 wt%, adhesive 1.5 wt% and extrusion assistant 1 wt% of alumina, drying at 100 deg.C for 3 hr, and calcining at 450 deg.C for 2 hr to obtain catalyst carrier CZ1-Al2O3. Adding CZ1-Al catalyst carrier2O3The palladium nitrate is impregnated by an isometric impregnation method to ensure that the Pd content of the catalyst is 0.1 percent, and the catalyst is dried after impregnation and calcined at 450 ℃ for 2 hours to obtain a finished catalyst A (in weight percentage, the Pd is 0.1 percent, and the cerium-zirconium solid solution CZ1 is 30 percent).
Example 2
Weighing 55g of cerium nitrate and 34g of zirconyl nitrate to prepare 0.25mol/L aqueous solution, diluting 85g of 25 wt% ammonia water to 5 wt% to be used as a precipitant, placing the precipitant in a three-neck flask, slowly dripping a mixed solution of the cerium nitrate and the zirconyl nitrate until the pH value of the solution is 9-11, continuing stirring for 0.5h after dripping is finished, standing and aging overnight, washing with deionized water, filtering, drying a filter cake at 100 ℃ for 5h, and then heating to 900 ℃ by a program under flowing air and roasting for 5h to prepare the catalyst aid, namely the cerium-zirconium solid solution CZ 2. CZ2 with a specific surface area of 250m2Alumina (Zibo major alumina technologies, Inc., model 80150) (where the weight ratio of CZ2 to alumina is 3:7), silica sol adjuvant (JH-40, Jiangyin softfly chemical Co., Ltd.) (3% by weight of alumina), binder (1.5% by weight of alumina), extrusion aid (1% by weight of alumina), kneading and extruding, drying at 100 deg.CRoasting for 2h at 450 ℃ for 3h to obtain the catalyst carrier CZ2-Al2O3. Adding CZ2-Al catalyst carrier2O3The palladium nitrate was impregnated by an isometric impregnation method to a Pd content of 0.1%, dried after impregnation, and calcined at 450 ℃ for 2h to obtain the final catalyst B (in weight percent: Pd 0.1%, 30% of the cerium-zirconium solid solution CZ 2).
Example 3
Weighing 55g of cerium nitrate and 34g of zirconyl nitrate to prepare 0.25mol/L aqueous solution, diluting 85g of 25 wt% ammonia water to 5 wt% to be used as a precipitant, placing the precipitant in a three-neck flask, slowly dropping a mixed solution of the cerium nitrate and the zirconyl nitrate until the pH value of the solution is 9-11, continuing stirring for 0.5h after dropping, standing and aging overnight, washing with deionized water, filtering, drying a filter cake at 100 ℃ for 5h, and then heating to 750 ℃ by a program under flowing air and roasting for 5h to prepare the catalyst aid, namely the cerium-zirconium solid solution CZ 3. CZ3 with a specific surface area of 250m2Alumina (Zibo major alumina science and technology ltd., model 80150) in a/g ratio of CZ3 to alumina 3:7, silica sol assistant JH-40 in 3 wt%, binder in 1.5 wt% and extrusion assistant in 1 wt% of alumina, drying at 100 deg.c for 3 hr, and calcining at 450 deg.c for 2 hr to obtain the catalyst carrier CZ3-Al2O3. Adding CZ3-Al catalyst carrier2O3The palladium nitrate was impregnated by an isometric impregnation method to a Pd content of 0.1%, dried after impregnation, and calcined at 450 ℃ for 2h to give finished catalyst C (in weight percent: Pd 0.1%, 30% of a cerium-zirconium solid solution CZ 3).
Example 4
Weighing 55g of cerium nitrate and 34g of zirconyl nitrate to prepare 0.25mol/L aqueous solution, diluting 85g of 25 wt% ammonia water to 5 wt% to be used as a precipitant, placing the precipitant in a three-neck flask, slowly dripping a mixed solution of the cerium nitrate and the zirconyl nitrate until the pH value of the solution is 9-11 under the condition of vigorous stirring, continuing stirring for 0.5h after dripping, standing and aging overnight, washing with deionized water, filtering, drying a filter cake at 100 ℃ for 5h, and then flowingAnd (3) raising the temperature to 750 ℃ in a programmed manner under the action of moving air, and roasting for 5 hours to prepare the catalyst auxiliary agent cerium-zirconium solid solution CZ 4. CZ4 with a specific surface area of 250m2Alumina (Zibo major alumina science and technology ltd., model 80150) in a weight ratio of CZ4 to alumina of 12:88, silica sol assistant (JH-40, 3 wt% of alumina), binder (1.5 wt% of alumina), extrusion assistant (1 wt% of alumina), drying at 100 deg.C for 3 hr, and calcining at 450 deg.C for 2 hr to obtain catalyst carrier CZ3-Al2O3. Adding CZ3-Al catalyst carrier2O3The palladium nitrate was impregnated by an isometric impregnation method to a Pd content of 0.1%, dried after impregnation, and calcined at 450 ℃ for 2h to obtain a finished catalyst D (in weight percent: Pd 0.1%, CZ4 as a cerium-zirconium solid solution 12%).
The light-off characteristics, catalytic combustion performance, and high-temperature stability of the catalyst were evaluated in a fixed bed reactor. The dosage of the catalyst is 10mL, and the VOCs gas adopts VH2：VC2H4：VC3H6：VC3H8：VC415:30:30:5:20, space velocity of 10000h-1During the reaction, firstly introducing VOCs gas, introducing metered air after the catalytic ignition, and introducing V air: vvocs 18:1, the reaction is developed into self-sustaining catalytic combustion, and after the reaction temperature is stabilized for 30min, the tail gas is collected and analyzed by gas chromatography.
Comparative example 1
The catalyst was prepared by the same method as in example 1 except that the content of Pd as the catalyst was 0.02 wt%, and the catalyst thus prepared was designated as a.
Comparative example 2
The preparation method of the catalyst is the same as that of example 1, except that the cerium zirconium hydroxide is calcined at 500 ℃ for 4h in the air atmosphere. The catalyst thus obtained is designated b.
Comparative example 3
The catalyst was prepared by the same method as in example 1, except that CZ1 was kneaded with alumina at a weight ratio of 1:1 and the catalyst obtained by extrusion molding was designated as c.
Comparative example 4
Weighing 87g of cerium nitrate and 14g of zirconyl nitrate to prepare 0.25mol/L aqueous solution, diluting 85g of 25 wt% ammonia water to 5 wt% to be used as a precipitant, placing the precipitant in a three-neck flask, slowly dropping a mixed solution of the cerium nitrate and the zirconyl nitrate until the pH value of the solution is 9-11, continuing stirring for 0.5h after dropping, standing and aging overnight, washing with deionized water, filtering, drying a filter cake at 100 ℃ for 5h, and then heating to 750 ℃ by a program under flowing air and roasting for 5h to prepare the catalyst aid, namely the cerium-zirconium solid solution CZ 4. CZ4 with a specific surface area of 250m2Alumina (Zibo major alumina science and technology ltd., model 80150) in a weight ratio of CZ4 to alumina of 12:88, silica sol assistant (JH-40, 3 wt% of alumina), binder (1.5 wt% of alumina), extrusion assistant (1 wt% of alumina), drying at 100 deg.C for 3 hr, and calcining at 450 deg.C for 2 hr to obtain catalyst carrier CZ4-Al2O3. Adding CZ4-Al catalyst carrier2O3Palladium nitrate was impregnated by an isometric impregnation method to a Pd content of 0.1%, dried after impregnation, and calcined at 450 ℃ for 2 hours to obtain a catalyst denoted as d (in weight percent: Pd 0.1%, cerium zirconium solid solution CZ4 accounting for 12%).
In order to examine the high-temperature stability of the catalyst, the catalysts prepared in examples 1-4 and comparative examples 1-4 were calcined in air at 1000 ℃ for 10h, accelerated aging was carried out, and the catalysts were respectively marked as A-old, B-old, C-old, D-old, a-old, B-old, C-old and D-old, and the catalytic combustion performance of the aged catalysts was evaluated, and the results are shown in Table 1.
The catalytic light-off and catalytic combustion effects of the catalyst are as follows.
TABLE 1 CATALYTIC LIGHTING TEMPERATURE SUMMARY TABLE FOR CATALYST
Table 2 percent gas volume of treated VOCs (%)
When volume calculation is carried out on tail gas content, N is not included2、O2And H2O。
As can be seen from the comparison of the data in tables 1-2, the catalyst disclosed by the invention can be ignited at normal temperature, realizes self-sustaining catalytic combustion, and has a good catalytic combustion effect. The catalyst of the comparative example has the catalytic light-off temperature close to 200 ℃ and has poor catalytic combustion effect. After the catalyst is aged for 5 hours at 1000 ℃, the light-off temperature and the catalytic combustion effect of the catalyst are not obviously reduced, but the catalyst of the comparative example is obviously reduced.
The preferred embodiments of the present invention have been described in detail, however, the present invention is not limited to the specific details of the above embodiments, and various simple modifications may be made to the technical solution of the present invention within the technical idea of the present invention, and these simple modifications are within the protective scope of the present invention.
It should be noted that the various technical features described in the above embodiments can be combined in any suitable manner without contradiction, and the invention is not described in any way for the possible combinations in order to avoid unnecessary repetition.
Claims (10)
1. A high-temperature resistant catalytic combustion catalyst for catalyzing and igniting VOCs to burn in a self-sustaining manner at normal temperature comprises a precious metal active component, an oxygen storage material cerium-zirconium solid solution and a carrier; the carrier contains Al2O3A carrier;
wherein, the content of the noble metal active component is 0.03 to 5 parts by weight, preferably 0.05 to 3 parts by weight, the content of the oxygen storage material cerium zirconium solid solution is 5 to 40 parts by weight, preferably 10 to 30 parts by weight, and the balance is a carrier, based on 100 parts by weight of the total weight of the catalyst.
2. The high-temperature-resistant catalytic combustion catalyst for normal-temperature catalytic ignition of self-sustaining combustion of VOCs according to claim 1, wherein: the noble metal active component is Pd and/or Pt.
3. The high-temperature-resistant catalytic combustion catalyst for normal-temperature catalytic ignition of self-sustaining combustion of VOCs according to claim 1, wherein:
the oxygen storage material cerium-zirconium solid solution is formed by performing a solid phase reaction at a high temperature of 500-1200 ℃ with a cerium-zirconium molar ratio (Ce/Zr) of 0.5-3.
4. The high-temperature-resistant catalytic combustion catalyst for normal-temperature catalytic ignition of self-sustaining combustion of VOCs according to claim 3, wherein: the oxygen storage material cerium zirconium solid solution is prepared by the following steps:
weighing cerium salt and zirconium salt according to the molar ratio of cerium to zirconium, and dissolving the cerium salt and the zirconium salt in water to prepare a mixed solution with the total solute concentration of 0.1-5 mol/L, preferably 0.2-2 mol/L; dropping the mixed solution into a precipitator under vigorous stirring until the pH value of the reaction solution is 9-11, continuing stirring after dropping, standing, washing, filtering, drying a filter cake, and then performing temperature programming to 500-1200 ℃ under flowing air, preferably roasting at 700-900 ℃ to prepare the cerium-zirconium solid solution;
the precipitant is selected from 0.1-10 wt%, preferably 1-5 wt% ammonia water.
5. The high-temperature-resistant catalytic combustion catalyst for normal-temperature catalytic ignition of self-sustaining combustion of VOCs according to claim 4, wherein:
the cerium salt is selected from cerium nitrate, cerium sulfate and cerium acetate;
the zirconium salt is selected from zirconyl nitrate, zirconium oxychloride, or zirconium tetrachloride.
6. The high-temperature-resistant catalytic combustion catalyst for normal-temperature catalytic ignition of self-sustaining combustion of VOCs according to claim 1, wherein:
the Al is2O3The specific surface of the carrier is 100-300 m2/g。
7. The method for preparing the high-temperature-resistant catalytic combustion catalyst for the self-sustained combustion of VOCs by normal-temperature catalytic ignition according to any one of claims 1 to 6, characterized by selecting from a wet forming method;
the wet forming method comprises the following steps:
mixing oxygen storage material cerium zirconium solid solution, auxiliary agent and Al2O3And kneading and extruding the carrier and a forming assistant for forming, drying at 80-120 ℃, roasting at 250-600 ℃ to prepare the catalyst carrier, impregnating the catalyst carrier with the required noble metal active component, drying at 80-120 ℃, and roasting at 250-600 ℃.
8. The method for preparing the high-temperature-resistant catalytic combustion catalyst for the self-sustaining combustion of the room-temperature catalytic ignition VOCs according to claim 7, wherein the method comprises the following steps:
the auxiliary agent is selected from sol; the sol is at least one selected from titanium sol, silica sol, water glass and silane.
9. The method for preparing the high-temperature-resistant catalytic combustion catalyst for the self-sustaining combustion of the room-temperature catalytic ignition VOCs according to claim 8, wherein the method comprises the following steps:
the dosage of the auxiliary agent is Al2O31-5% of the weight of the carrier.
10. Use of the high-temperature-resistant catalytic combustion catalyst for self-sustaining combustion of normal-temperature catalytic ignition VOCs according to any one of claims 1 to 6 or the catalyst prepared by the preparation method according to any one of claims 7 to 9 in normal-temperature catalytic ignition of VOCs streams.
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| CN111715240A (en) * | 2020-07-22 | 2020-09-29 | 无锡尚好蓝图环保科技有限公司 | Rare earth metal oxide catalyst for degrading VOCs at low temperature and preparation method thereof |
| CN114917925A (en) * | 2022-04-20 | 2022-08-19 | 山东亮剑环保新材料有限公司 | Composite VOCs catalyst and production method thereof |
| CN115624973A (en) * | 2022-09-20 | 2023-01-20 | 中国船舶重工集团公司第七一八研究所 | Sulfur poisoning resistant monolithic catalyst and preparation method and application thereof |
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| CN114917925A (en) * | 2022-04-20 | 2022-08-19 | 山东亮剑环保新材料有限公司 | Composite VOCs catalyst and production method thereof |
| CN115624973A (en) * | 2022-09-20 | 2023-01-20 | 中国船舶重工集团公司第七一八研究所 | Sulfur poisoning resistant monolithic catalyst and preparation method and application thereof |
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