CN106732539B - For being catalyzed the compound non-noble metal oxide catalyst and its preparation method and application of burning toluene - Google Patents
For being catalyzed the compound non-noble metal oxide catalyst and its preparation method and application of burning toluene Download PDFInfo
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/16—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
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- B01J23/34—Manganese
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/002—Mixed oxides other than spinels, e.g. perovskite
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- F23—COMBUSTION APPARATUS; COMBUSTION PROCESSES
- F23G—CREMATION FURNACES; CONSUMING WASTE PRODUCTS BY COMBUSTION
- F23G7/00—Incinerators or other apparatus for consuming industrial waste, e.g. chemicals
- F23G7/06—Incinerators or other apparatus for consuming industrial waste, e.g. chemicals of waste gases or noxious gases, e.g. exhaust gases
- F23G7/07—Incinerators or other apparatus for consuming industrial waste, e.g. chemicals of waste gases or noxious gases, e.g. exhaust gases in which combustion takes place in the presence of catalytic material
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2523/00—Constitutive chemical elements of heterogeneous catalysts
Abstract
The present invention provides a kind of for being catalyzed the compound non-noble metal oxide catalyst of burning toluene, and the catalyst is with TiO2For carrier, to be supported on TiO2On compound non-noble metal oxide be active component, the structural formula of the compound non-noble metal oxide are as follows: Sn1‑xMnxO2, x satisfaction: the quality of 0.05≤x≤0.5, the compound non-noble metal oxide accounts for the 10%~30% of catalyst quality.The present invention also provides a kind of methods for preparing above-mentioned catalyst, and the method for carrying out catalysis burning to toluene using the catalyst.Catalyst of the present invention is compound non-noble metal oxide catalyst, can fast and efficiently eliminate the toluene in industrial tail gas.
Description
Technical field
The invention belongs to catalyst technical fields, and in particular to a kind of for being catalyzed the compound base metal of burning toluene
Oxide catalyst and its preparation method and application.
Background technique
Toluene is a kind of volatile organic matter, has greatly harm to ecological environment and human health, it is generated extensively
In production processes such as petrochemical industry, printing, pharmacy.In recent years, China has put into effect multi-section regulation power-assisted volatile organic matter successively
(VOCs) it administers, is broadly divided into two major classes commonly used in the catalyst of toluene catalytic combustion: noble metal such as Pt, Pd, Rh etc., and
Non-noble metal oxide such as calcium nutrition, hexa-aluminate, metal composite oxide etc..Wherein, although noble metal catalyst have compared with
Good low temperature active, but its easy-sintering, it is expensive the problems such as seriously constrain the industrial application of noble metal catalyst.Therefore,
Develop it is a kind of for be catalyzed burning toluene non-precious metal catalyst have important economy and environmental benefit.
In non-noble metal oxide material, although the stability of perocskite type and hexa-aluminate catalyzer has compared with noble metal
It is improved, but its usual low temperature active is lower, therefore is reacted commonly used in the methane catalytic combustion of high concentration.Transition metal oxide
Such as copper oxide, manganese oxide are often applied to toluene catalytic combustion field, there is outstanding catalytic activity in cold stage.
Summary of the invention
It is a kind of for being catalyzed combustion technical problem to be solved by the present invention lies in view of the above shortcomings of the prior art, providing
Burn the compound non-noble metal oxide catalyst of toluene.The catalyst can fast and efficiently eliminate the first in industrial tail gas
Benzene.
In order to solve the above technical problems, the technical solution adopted by the present invention is that: it is a kind of for being catalyzed the compound of burning toluene
Type non-noble metal oxide catalyst, which is characterized in that the catalyst is with TiO2For carrier, to be supported on TiO2On it is compound
Non-noble metal oxide is active component, the structural formula of the compound non-noble metal oxide are as follows: Sn1-xMnxO2, x satisfaction:
The quality of 0.05≤x≤0.5, the compound non-noble metal oxide accounts for the 10%~30% of catalyst quality.
Above-mentioned is a kind of for being catalyzed the compound non-noble metal oxide catalyst of burning toluene, which is characterized in that institute
State x=0.2.
Above-mentioned is a kind of for being catalyzed the compound non-noble metal oxide catalyst of burning toluene, described compound non-expensive
The quality of metal oxide accounts for the 20% of catalyst quality.
In addition, the present invention also provides a kind of methods for preparing above-mentioned catalyst, which is characterized in that this method includes following
Step:
Step 1: by Mn (CH3COO)2·4H2O and SnCl4It is dissolved in deionized water, is added after sonic oscillation 0.5h
TiO2Powder obtains suspension after mixing evenly；
Step 2: being stirred to suspension described in step 1, and ammonium hydroxide is added dropwise in whipping process, makes suspension
PH value is adjusted to 8~10, is precipitated after filtering；
Step 3: precipitating described in step 2 is placed in baking oven, under conditions of temperature is 120 DEG C dry 12h~
24h；
Step 4: the precipitating after will be dry in step 3 is placed in Muffle furnace, with 5 DEG C/min~7 DEG C/min heating speed
Heat preservation 4h~8h carries out calcination process after rate is warming up to 650 DEG C, obtains the compound base metal oxygen for being catalyzed burning toluene
Compound catalyst.
In addition to this, the present invention also provides it is a kind of using above-mentioned catalyst to toluene carry out catalysis burning method,
It is characterized in that, this method are as follows: Catalyst packing in reactor and is warming up to 200 DEG C~300 DEG C, with 80000h after constant temperature-1
Mass space velocity mixed gas containing toluene is continually fed into reactor, make toluene the urging in catalyst in mixed gas
Change lower combustion decomposition, generates carbon dioxide and water.
Above-mentioned method, which is characterized in that the ingredient of the mixed gas presses volume percentage are as follows: toluene 0.5%, O2
20%, surplus N2。
Above-mentioned method, which is characterized in that the form for being loaded on the catalyst in reactor is particulate form, and granularity is 60 mesh
~100 mesh.
Compared with the prior art, the present invention has the following advantages:
1, catalyst of the present invention is with TiO2For carrier, to be supported on TiO2On Sn1-xMnxO2(0.05≤x≤0.5) is compound
Type non-noble metal oxide is active component.Wherein, Sn oxide has good thermal stability, in other hydrocarbon class catalysis combustions
It burns in reaction and shows higher activity.Mn oxide has active oxygen species, TiO2It, can be with stronger surface acidity
Absorption toluene type organic well.Thus the catalyst being combined can fast and efficiently eliminate the first in industrial tail gas
Benzene.
2, catalytic component of the present invention is non-noble metal oxide, cost can be made to substantially reduce, raw material is both selected from
In the non-noble metal oxide that rich reserves are easy to get, and show than common Pd/Al2O3The higher catalysis of noble metal catalyst is lived
Property, there is extremely strong commercial application prospect.
3, catalyst preparation and methods for using them of the present invention is simple, is easy to repeat, pollution-free, is conducive to industrialized popularization and answers
With.Catalyst of the present invention has excellent low temperature active and thermal stability.
Invention is further described in detail with reference to the accompanying drawings and examples.
Detailed description of the invention
Fig. 1 is the toluene catalytic combustion curve comparison figure of 1 catalyst of 1-5 of embodiment of the present invention catalyst and comparative example.
Fig. 2 is the graph of pore diameter distribution of 1 catalyst of the embodiment of the present invention.
Fig. 3 is that the SEM of 1 catalyst of the embodiment of the present invention schemes.
Specific embodiment
Embodiment 1
A kind of compound non-noble metal oxide catalyst for carrying out being catalyzed burning to toluene is present embodiments provided,
The catalyst is with TiO2For carrier, to be supported on TiO2On compound non-noble metal oxide be active component, it is described compound
The structural formula of non-noble metal oxide are as follows: Sn0.8Mn0.2O2, the quality of the compound non-noble metal oxide accounts for catalyst matter
20%, TiO of amount2Quality account for the 80% of catalyst quality.
The present embodiment prepare the method for the catalyst the following steps are included:
Step 1: taking a range is the clean beaker of 500mL, 300mL deionized water is added, is then weighed by design requirement
Mn (the CH of metering3COO)2·4H2O and SnCl4, later by Mn (CH3COO)2·4H2O and SnCl4It is added in beaker, stirring makes
The two is completely dissolved in deionized water, then places the beaker sonic oscillation 0.5h in ultrasonator, backward beaker in
TiO is added2Powder obtains suspension after mixing evenly；
Step 2: being stirred to suspension described in step 1, and industrial ammonia is added dropwise in whipping process, and uses pH
Reagent detects the pH value of suspension, and until the pH value of suspension is adjusted to 9, filtering is precipitated；
Step 3: precipitating described in step 2 is placed in baking oven, dry 18h under conditions of temperature is 120 DEG C；
Step 4: the precipitating after will be dry in step 3 is placed in Muffle furnace, it is warming up to the heating rate of 6 DEG C/min
6h is kept the temperature after 650 DEG C and carries out calcination process, obtains the compound non-noble metal oxide catalyst for toluene catalytic combustion.
The pore-size distribution testing result of the present embodiment catalyst is shown in Fig. 2, and the duct of the catalyst belongs to mesoporous as shown in Figure 2
Structure, this structure are conducive to the diffusion transport of reactant, to improve the activity of catalyst.The SEM of the present embodiment catalyst
Testing result is shown in Fig. 3, and the particle of the catalyst is uniform as shown in Figure 3, and granularity is small, this is conducive to the specific surface for improving catalyst
Product, to improve contact site of the catalyst with reactant, improves the activity of catalyst.
Embodiment 2
A kind of compound non-noble metal oxide catalyst for carrying out being catalyzed burning to toluene is present embodiments provided,
The catalyst is with TiO2For carrier, to be supported on TiO2On compound non-noble metal oxide be active component, it is described compound
The structural formula of non-noble metal oxide are as follows: Sn0.7Mn0.3O2, the quality of the compound non-noble metal oxide accounts for catalyst matter
25%, TiO of amount2Quality account for the 75% of catalyst quality.
The present embodiment prepare the method for the catalyst the following steps are included:
Step 1: taking a range is the clean beaker of 500mL, 300mL deionized water is added, is then weighed by design requirement
Mn (the CH of metering3COO)2·4H2O and SnCl4, later by Mn (CH3COO)2·4H2O and SnCl4It is added in beaker, stirring makes
The two is completely dissolved in deionized water, then places the beaker sonic oscillation 0.5h in ultrasonator, backward beaker in
TiO is added2Powder obtains suspension after mixing evenly；
Step 2: being stirred to suspension described in step 1, and industrial ammonia is added dropwise in whipping process, and uses pH
Reagent detects the pH value of suspension, and until the pH value of suspension is adjusted to 8.5, filtering is precipitated；
Step 3: precipitating described in step 2 is placed in baking oven, dry 16h under conditions of temperature is 120 DEG C；
Step 4: the precipitating after will be dry in step 3 is placed in Muffle furnace, it is warming up to the heating rate of 6 DEG C/min
5h is kept the temperature after 650 DEG C and carries out calcination process, obtains the compound non-noble metal oxide catalyst for toluene catalytic combustion.
Embodiment 3
A kind of compound non-noble metal oxide catalyst for carrying out being catalyzed burning to toluene is present embodiments provided,
The catalyst is with TiO2For carrier, to be supported on TiO2On compound non-noble metal oxide be active component, it is described compound
The structural formula of non-noble metal oxide are as follows: Sn0.6Mn0.4O2, the quality of the compound non-noble metal oxide accounts for catalyst matter
20%, TiO of amount2Quality account for the 80% of catalyst quality.
The present embodiment prepare the method for the catalyst the following steps are included:
Step 1: taking a range is the clean beaker of 500mL, 300mL deionized water is added, is then weighed by design requirement
Mn (the CH of metering3COO)2·4H2O and SnCl4, later by Mn (CH3COO)2·4H2O and SnCl4It is added in beaker, stirring makes
The two is completely dissolved in deionized water, then places the beaker sonic oscillation 0.5h in ultrasonator, backward beaker in
TiO is added2Powder obtains suspension after mixing evenly；
Step 2: being stirred to suspension described in step 1, and industrial ammonia is added dropwise in whipping process, and uses pH
Reagent detects the pH value of suspension, and until the pH value of suspension is adjusted to 8, filtering is precipitated；
Step 3: precipitating described in step 2 is placed in baking oven, dry 12h under conditions of temperature is 120 DEG C；
Step 4: the precipitating after will be dry in step 3 is placed in Muffle furnace, it is warming up to the heating rate of 5 DEG C/min
8h is kept the temperature after 650 DEG C and carries out calcination process, obtains the compound non-noble metal oxide catalyst for toluene catalytic combustion.
Embodiment 4
A kind of compound non-noble metal oxide catalyst for carrying out being catalyzed burning to toluene is present embodiments provided,
The catalyst is with TiO2For carrier, to be supported on TiO2On compound non-noble metal oxide be active component, it is described compound
The structural formula of non-noble metal oxide are as follows: Sn0.5Mn0.5O2, the quality of the compound non-noble metal oxide accounts for catalyst matter
20%, TiO of amount2Quality account for the 80% of catalyst quality.
The present embodiment prepare the method for the catalyst the following steps are included:
Step 1: taking a range is the clean beaker of 500mL, 300mL deionized water is added, is then weighed by design requirement
Mn (the CH of metering3COO)2·4H2O and SnCl4, later by Mn (CH3COO)2·4H2O and SnCl4It is added in beaker, stirring makes
The two is completely dissolved in deionized water, then places the beaker sonic oscillation 0.5h in ultrasonator, backward beaker in
TiO is added2Powder obtains suspension after mixing evenly；
Step 2: being stirred to suspension described in step 1, and industrial ammonia is added dropwise in whipping process, and uses pH
Reagent detects the pH value of suspension, and until the pH value of suspension is adjusted to 10, filtering is precipitated；
Step 3: precipitating described in step 2 is placed in baking oven, dried for 24 hours under conditions of temperature is 120 DEG C；
Step 4: the precipitating after will be dry in step 3 is placed in Muffle furnace, it is warming up to the heating rate of 7 DEG C/min
4h is kept the temperature after 650 DEG C and carries out calcination process, obtains the compound non-noble metal oxide catalyst for toluene catalytic combustion.
Embodiment 5
A kind of compound non-noble metal oxide catalyst for carrying out being catalyzed burning to toluene is present embodiments provided,
The catalyst is with TiO2For carrier, to be supported on TiO2On compound non-noble metal oxide be active component, it is described compound
The structural formula of non-noble metal oxide are as follows: Sn0.9Mn0.1O2, the quality of the compound non-noble metal oxide accounts for catalyst matter
20%, TiO of amount2Quality account for the 80% of catalyst quality.
The present embodiment prepare the method for the catalyst the following steps are included:
Step 1: taking a range is the clean beaker of 500mL, 300mL deionized water is added, is then weighed by design requirement
Mn (the CH of metering3COO)2·4H2O and SnCl4, later by Mn (CH3COO)2·4H2O and SnCl4It is added in beaker, stirring makes
The two is completely dissolved in deionized water, then places the beaker sonic oscillation 0.5h in ultrasonator, backward beaker in
TiO is added2Powder obtains suspension after mixing evenly；
Step 2: being stirred to suspension described in step 1, and industrial ammonia is added dropwise in whipping process, and uses pH
Reagent detects the pH value of suspension, and until the pH value of suspension is adjusted to 8, filtering is precipitated；
Step 3: precipitating described in step 2 is placed in baking oven, dry 12h under conditions of temperature is 120 DEG C；
Step 4: the precipitating after will be dry in step 3 is placed in Muffle furnace, it is warming up to the heating rate of 5 DEG C/min
8h is kept the temperature after 650 DEG C and carries out calcination process, obtains the compound non-noble metal oxide catalyst for toluene catalytic combustion.
Embodiment 6
A kind of compound non-noble metal oxide catalyst for carrying out being catalyzed burning to toluene is present embodiments provided,
The catalyst is with TiO2For carrier, to be supported on TiO2On compound non-noble metal oxide be active component, it is described compound
The structural formula of non-noble metal oxide are as follows: Sn0.95Mn0.05O2, the quality of the compound non-noble metal oxide accounts for catalyst matter
20%, TiO of amount2Quality account for the 80% of catalyst quality.
The present embodiment prepare the method for the catalyst the following steps are included:
Step 1: taking a range is the clean beaker of 500mL, 300mL deionized water is added, is then weighed by design requirement
Mn (the CH of metering3COO)2·4H2O and SnCl4, later by Mn (CH3COO)2·4H2O and SnCl4It is added in beaker, stirring makes
The two is completely dissolved in deionized water, then places the beaker sonic oscillation 0.5h in ultrasonator, backward beaker in
TiO is added2Powder obtains suspension after mixing evenly；
Step 2: being stirred to suspension described in step 1, and industrial ammonia is added dropwise in whipping process, and uses pH
Reagent detects the pH value of suspension, and until the pH value of suspension is adjusted to 8, filtering is precipitated；
Step 3: precipitating described in step 2 is placed in baking oven, dry 12h under conditions of temperature is 120 DEG C；
Step 4: the precipitating after will be dry in step 3 is placed in Muffle furnace, it is warming up to the heating rate of 5 DEG C/min
8h is kept the temperature after 650 DEG C and carries out calcination process, obtains the compound non-noble metal oxide catalyst for toluene catalytic combustion.
Comparative example 1
The catalyst that this comparative example provides is Pd/Al2O3Noble metal catalyst, the noble metal catalyst is using purchase or certainly
The method of system obtains, wherein homemade method is equivalent impregnation method, detailed process are as follows: weigh the Pd (NO of palladium 18.46%3)3Solution
0.5291g, in weighed Pd (NO3)33mL deionization is added in solution, by the Pd (NO after dilution3)3Solution is added drop-wise to 4.1g
γ-Al2O3On powder, after ultrasonic 10min, stand for 24 hours, 80 DEG C of dry 12h in air dry oven, later in Muffle furnace
With the heating rate of 5 DEG C/min from room temperature to 500 DEG C, and in 500 DEG C of roasting 4h, Pd/Al is obtained2O3Powder takes one
50mL deionization is added in the clean beaker of 100mL, and ultrasonic 10min is stood for 24 hours, 80 DEG C of dry 12h in air dry oven, it
Afterwards in Muffle furnace with the heating rate of 5 DEG C/min from room temperature to 500 DEG C, and in 500 DEG C of roasting 4h, obtain Pd/Al2O3
Catalyst.
Catalyst prepared by the embodiment of the present invention 1 to 5 and comparative example 1 is subjected to catalysis burning toluene application test, tool
Body tests process are as follows: embodiment 1 to 5 and 1 catalyst of comparative example are respectively prepared to the particulate form of 60~100 mesh of granularity, loaded
It is then 80000h with mass space velocity in reactor-1It is passed through to reactor containing CH4The mixed gas of ingredient carries out catalysis combustion
Burn experiment.The mixed gas composition is (volume content): toluene 0.5%；O220%；Remaining is N2.Temperature be 200 DEG C~
Under conditions of 300 DEG C, every conversion ratio of 30 DEG C of records, each temperature spot stops 30min, catalyst activity is made to reach steady
Fixed, toluene concentration is detected using gas chromatograph, detect curve graph is as shown in Figure 1.The Sn of the embodiment of the present invention1- xMnxO2/TiO2O composite metallic oxide catalyst and comparative example Pd/Al2O3Starting combustion in catalyst in relation to toluene catalytic combustion
Burn temperature (the temperature T that conversion ratio is 10%10) data be listed in Table 1 below.
The temperature of initial combustion T of 1 embodiment of the present invention of table and comparative example catalyst10
It will be seen from figure 1 that Sn prepared by the present invention0.8Mn0.2O2Catalyst is shown than comparative example precious metals pd/γ-
Al2O3Catalyst (commercialized catalyst) higher conversion ratio.Simultaneously from table 1 it follows that composition metal prepared by the present invention
Oxide catalyst initiation temperature is equal to or lower than comparative example Pd/ γ-Al2O3Catalyst illustrates that the series base metal is urged
Agent activity with higher is expected to substitute commercialized precious metals pd/γ-Al2O3Catalyst.
The above is only presently preferred embodiments of the present invention, is not intended to limit the invention in any way.It is all according to invention skill
Art any simple modification, change and equivalence change substantially to the above embodiments, still fall within technical solution of the present invention
Protection scope in.
Claims (7)
1. it is a kind of for be catalyzed burning toluene compound non-noble metal oxide catalyst, which is characterized in that the catalyst with
TiO2For carrier, to be supported on TiO2On compound non-noble metal oxide be active component, the compound base metal oxygen
The structural formula of compound are as follows: Sn1-xMnxO2, x satisfaction: 0.05≤x≤0.5, the quality of the compound non-noble metal oxide, which accounts for, urges
The 10%~30% of agent quality.
2. it is according to claim 1 a kind of for being catalyzed the compound non-noble metal oxide catalyst of burning toluene,
It is characterized in that, the x=0.2.
3. according to claim 1 a kind of for being catalyzed the compound non-noble metal oxide catalyst of burning toluene, institute
The quality for stating compound non-noble metal oxide accounts for the 20% of catalyst quality.
4. a kind of method for preparing the catalyst as described in claim 1,2 or 3, which is characterized in that method includes the following steps:
Step 1: by Mn (CH3COO)2·4H2O and SnCl4It is dissolved in deionized water, TiO is added after sonic oscillation 0.5h2Powder
Body obtains suspension after mixing evenly；
Step 2: being stirred to suspension described in step 1, and ammonium hydroxide is added dropwise in whipping process, makes the pH value of suspension
8~10 are adjusted to, is precipitated after filtering；
Step 3: precipitating described in step 2 is placed in baking oven, the dry 12h~for 24 hours under conditions of temperature is 120 DEG C；
Step 4: the precipitating after will be dry in step 3 is placed in Muffle furnace, with 5 DEG C/min~7 DEG C/min heating rate liter
Temperature carries out calcination process to heat preservation 4h~8h after 650 DEG C, obtains the compound non-noble metal oxide for being catalyzed burning toluene
Catalyst.
5. a kind of method for carrying out catalysis burning to toluene using the catalyst as described in claim 1,2 or 3, which is characterized in that
This method are as follows: Catalyst packing in reactor and is warming up to 200 DEG C~300 DEG C, with 80000h after constant temperature-1Mass space velocity
It is continually fed into mixed gas containing toluene into reactor, so that the toluene in mixed gas is burnt under the catalysis of catalyst and divides
Solution generates carbon dioxide and water.
6. according to the method described in claim 5, it is characterized in that, the ingredient of the mixed gas presses volume percentage are as follows:
Toluene 0.5%, O220%, surplus N2。
7. according to the method described in claim 5, it is characterized in that, the form for the catalyst being loaded in reactor is particle
State, granularity are 60 mesh~100 mesh.
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| CN107930624B (en) * | 2017-11-30 | 2020-07-17 | 西安元创化工科技股份有限公司 | Composite catalyst for catalytic combustion of ethyl acetate and preparation method and application thereof |
| CN108080018B (en) * | 2017-12-20 | 2021-01-12 | 江汉大学 | Preparation method of modified manganese oxide molecular sieve catalyst for catalytic combustion of toluene |
| CN114602536B (en) * | 2020-12-03 | 2023-07-11 | 万华化学集团股份有限公司 | Preparation method of catalyst and method for reducing VOC content in polyether polyol |
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