CN109529860A - A kind of X-Sn-Zr reducing catalyst and its preparation method and application - Google Patents
A kind of X-Sn-Zr reducing catalyst and its preparation method and application Download PDFInfo
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- CN109529860A CN109529860A CN201811474227.4A CN201811474227A CN109529860A CN 109529860 A CN109529860 A CN 109529860A CN 201811474227 A CN201811474227 A CN 201811474227A CN 109529860 A CN109529860 A CN 109529860A
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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
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/835—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with germanium, tin or lead
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
- B01D53/86—Catalytic processes
- B01D53/8603—Removing sulfur compounds
- B01D53/8609—Sulfur oxides
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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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2258/00—Sources of waste gases
- B01D2258/02—Other waste gases
- B01D2258/0283—Flue gases
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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
- B01J2523/00—Constitutive chemical elements of heterogeneous catalysts
Abstract
The invention discloses a kind of X-Sn-Zr reducing catalyst and its preparation method and application, the structures of the catalyst are as follows: XnOm‑SnO2‑ZrO2；Wherein, X includes: Cu and its metal of the same clan or Fe；Wherein, n:m=1:1 or 2:3；The catalyst is used for SO2It is reduced to elemental sulfur, X in the catalystnOmQuality account for the 5%~20% of catalyst gross mass.Catalyst of the invention can pass through N2, CO and SO2Mixed gas presulfurization after at 300~500 DEG C catalytic desulfurization is carried out to the mixed gas containing oxygen and sulfur dioxide, desulfuration efficiency is high.
Description
Technical field
The present invention relates to a kind of ternary metal oxides, and in particular to a kind of X-Sn-Zr reducing catalyst and its preparation side
Method and purposes.
Background technique
With the continuous intensification of countries in the world process of industrialization, SO2Pollution has been more than that smoke contamination becomes atmospheric environment
First big pollutant.Flue gas desulfurization (Flue gas desulfurization, FGD) is different from other desulfurization methods, is the world
The sulfur method of upper unique large-scale commercial application, is control of acid rain and SO2The maximally efficient and main technology of pollution
Means.
Flue gas desulfurization is all paid much attention in countries in the world, tens of kinds of effective desulfurization technologies has been developed, wherein extensively
The flue gas desulfurization technique of general use has:
(1) lime/lime stone-wet process has many advantages, such as applicable coal is wide, raw material is cheap and easy to get, desulfurization degree is high, accounts for
According to the maximum market share, but investment and operating cost are big, and operation and maintenance amount is big, and is easy to produce white cigarette, causes secondary dirt
Dye；
(2) rotating spraying semidry method (LSD), investment and operating cost are also slightly below wet process, and product is calcium sulfite
(CaSO3), but desulfurization degree is low compared with wet process；
(3) in-furnace calcium spraying humidification activation method (LIFAC), for desulfurization degree up to 70%-80%, project cost is lower, but produces
Object is calcium sulfite (CaSO3), easily cause ash erosion；
(4) flue gas desulfurization with seawater method, simple process, system is reliable for operation, and the high operating cost of desulfurization degree is low, and desulphurization system needs
It is arranged by the sea and ocean temperature is lower, dissolved oxygen (OC) is higher；
(5) ammonia type flue gas desulfurizing, usually to synthesize ammonia as raw material, product is sulphur ammonia etc., need neighbouring synthesis ammonia factory and
Chemical fertilizer factory；
(6) simple wet the Technology of Integrating Desulfurization, desulfurization degree is low, the lower raw material of cost be industrial alkali waste and caustic soda,
Need to close on the factory for thering is spent lye to discharge, after neutralization, waste water need to be discharged into sewage plant and be handled.
Desulphurization catalyst surface is active, can accelerate desulfurization, currently used to have: manganese oxide (MnO), zinc oxide
(ZnO), iron oxide (Fe3O4) etc..Metal oxide desulfurization is that a kind of dry desulfurizing process not will cause without sewage and spent acid
Pollution, but current metal oxide desulfuration efficiency is too low, it is difficult to it promotes.
Summary of the invention
The object of the present invention is to provide a kind of X-Sn-Zr reducing catalyst and its preparation method and application, the catalyst solutions
The problem of existing conventional wet desulfurization of having determined easily causes secondary pollution, can be realized catalytic desulfurization, will not generate sewage, and desulfurization
It is high-efficient.
In order to achieve the above object, the present invention provides a kind of X-Sn-Zr reducing catalyst, the structures of the catalyst are as follows:
XnOm-SnO2-ZrO2；Wherein, X includes: Cu and its metal of the same clan or Fe；Wherein, n:m=1:1 or 2:3；The catalyst is used for
By SO2It is reduced to elemental sulfur, X in the catalystnOmQuality account for the 5%~20% of catalyst gross mass.
Preferably, the X-ray diffractogram of the catalyst has diffraction maximum at 2 θ=26,33,37,51,53,62,65.
Preferably, the X-Sn-Zr reducing catalyst is by by raw material SnCl4、ZrO(NO3)2And Xa(NO3)bAqueous solution exist
It is obtained under neutrallty condition；Wherein, a:b=1:2 or 1:3.
Preferably, the SnCl4With ZrO (NO3)2Mass ratio be 3:1.
Preferably, the aqueous solution is adjusted to neutrality by ammonium hydroxide.
The present invention also provides the preparation methods of the X-Sn-Zr reducing catalyst described in one kind, and this method includes:
(1) it weighs raw material: weighing SnCl4、ZrO(NO3)2And Xa(NO3)b, raw material is soluble in water；
(2) adjusting aqueous solution of raw material is neutrality, is stirred under different aging temperatures, is filtered, and is dried, and roasting, tabletting is to make
Obtain the catalyst of different meshes.
Preferably, in step (1), the SnCl4With ZrO (NO3)2Mass ratio be 3:1.
Preferably, in step (2), use ammonium hydroxide adjust aqueous solution pH value be 7, the aging temperature for 20 DEG C~
80℃。
Preferably, in step (2), the reaction solution is sealed using film, and several holes are set on film, in different agings
At a temperature of stir.
The present invention also provides the purposes of the X-Sn-Zr reducing catalyst described in one kind, which is used
In catalytic desulfurization, pass through N2, CO and SO2Mixed gas presulfurization after at 300~500 DEG C to containing oxygen and sulfur dioxide
Mixed gas carries out catalytic desulfurization.
It is easy to solve existing conventional wet desulfurization for X-Sn-Zr reducing catalyst of the invention and its preparation method and application
The problem of causing secondary pollution has the advantage that
X-Sn-Zr reducing catalyst of the invention can carry out catalytic desulfurization at 300~500 DEG C, and desulfuration efficiency is high；
X-Sn-Zr reducing catalyst of the invention can carry out catalysis reduction under the conditions of oxygen-containing, by SO2It is reduced to elemental sulfur；
The present invention uses mixed gas presulfurization, to regulate and control the status of overall reaction shared by two kinds of mechanism.Known experiment knot
Demonstration is real, and in oxygen-free environment, redox mechanism is dominant, and there is no need to carry out presulfurization to catalyst.And the present invention relates to
And be it is oxygen-containing under the conditions of catalysis reduction, redox mechanism is since Lacking oxygen is by O in flue gas in the case of this2Occupy and by
Inhibit, therefore is regulated and controled by mixed gas presulfurization to strengthen status of the COS intermediate mechanism in catalytic process；
Catalyst of the invention, the load capacity of X element influence the structure of catalyst, and what heteroatomic addition changed is catalysis
Agent electric conductivity reduces forbidden bandwidth, so that outer-shell electron is easier to move to conduction band from valence band to form electron hole, in turn
Its catalytic performance is influenced, so to control XnOmElement mass fraction is between 5%-20%；
Catalyst using plasma irradiation of the invention can be such that catalytic activity acquisition effectively restores, and the transformation that relents
The recovery to catalytic activity is handled without too big effect.
Detailed description of the invention
Fig. 1 is the X-ray diffractogram of Cu-Sn-Zr reducing catalyst of the present invention.
Specific embodiment
The technical scheme in the embodiments of the invention will be clearly and completely described below, it is clear that described implementation
Example is only a part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, this field is common
Technical staff's every other embodiment obtained without making creative work belongs to the model that the present invention protects
It encloses.
A kind of X-Sn-Zr reducing catalyst, as shown in Figure 1, being the X-ray diffraction of Cu-Sn-Zr reducing catalyst of the present invention
Figure, characterization result have SnO at 2 θ=26,33,37,51,53,62,652Diffraction maximum, the structure of the catalyst are as follows: XnOm-
SnO2-ZrO2；Wherein, X includes: Cu and its metal of the same clan or Fe；Wherein, n:m=1:1 or 2:3；The catalyst is used for SO2
It is reduced to elemental sulfur, X in the catalystnOmQuality account for the 5%~20% of catalyst gross mass.
The metal of the same clan can be Ag or Au, better catalytic activity, but the cost is relatively high.When X is Cu and its gold of the same clan
When category, the structure of the catalyst are as follows: XO-SnO2-ZrO2；When X is Fe, the structure of the catalyst are as follows: Fe2O3-SnO2-ZrO2。
Catalyst of the invention, catalyst are reused 5 times, catalytic activity are lost after 1 hour every time, experiments have shown that alternating temperature
With transformation processing to the recovery of catalytic activity without too big effect, it is effective that using plasma irradiation can be such that catalytic activity obtains
Restore.
Catalyst of the invention, the load capacity of X element influence the structure of catalyst.What heteroatomic addition changed is catalysis
Agent electric conductivity reduces forbidden bandwidth, so that outer-shell electron is easier to move to conduction band from valence band to form electron hole, in turn
Its catalytic performance is influenced, so to control XnOmElement mass fraction is between 5%-20%.
Further, the X-Sn-Zr reducing catalyst is by by raw material SnCl4、ZrO(NO3)2And Xa(NO3)bAqueous solution
It obtains in neutral conditions；Wherein, a:b=1:2 or 1:3.
Further, SnCl4With ZrO (NO3)2Mass ratio be 3:1.Xa(NO3)bAdditive amount according to XnOmQuality account for
Catalyst gross mass and SnCl4With ZrO (NO3)2Mass Calculation.
Further, aqueous solution is adjusted to neutrality by ammonium hydroxide.
A kind of preparation method of above-mentioned X-Sn-Zr reducing catalyst, this method includes:
(1) it weighs raw material: weighing SnCl4、ZrO(NO3)2And Xa(NO3)b, raw material is soluble in water；
(2) adjusting aqueous solution of raw material is neutrality, is stirred under different aging temperatures, is filtered, and is dried, and roasting, tabletting is to make
Obtain the catalyst of different meshes.
Further, in step (1), SnCl4With ZrO (NO3)2Mass ratio be 3:1.
Further, in step (2), use ammonium hydroxide adjust aqueous solution pH value be 7, aging temperature be 20 DEG C~80
℃.Aging temperature can be 20 DEG C, 30 DEG C, 40 DEG C, 50 DEG C, 60 DEG C, 70 DEG C or 80 DEG C.
Aging temperature influences the crystal structure of catalyst, and then influences its reactivity, the catalyst prepared at 20 DEG C
Catalytic efficiency is 71%, and the catalytic efficiency of the catalyst prepared at 40 DEG C is 75%, the catalysis effect of the catalyst prepared at 60 DEG C
Rate is that the catalytic efficiency of the catalyst prepared at 72%80 DEG C is 69%, therefore optimal aging temperature should be 40 DEG C.
Further, in step (2), reaction solution is sealed using film, and several holes are set on film, in different aging temperature
The lower stirring of degree.Ammonium hydroxide volatilizees in order to prevent, thus pH value when changing co-precipitation, so sealed using film.
Further, in step (2), drying temperature is 100~300 DEG C.600 are raised to from room temperature temperature programming when roasting
DEG C, and in 600 DEG C of 4 hours of holding, maturing temperature is too low can not to be made metallic element aoxidize and form cellular structure, too Gao Zehui
Cause sintering of catalyst.
Further, in step (2), finished catalyst is 30~50 mesh.
A kind of purposes of above-mentioned X-Sn-Zr reducing catalyst, the X-Sn-Zr reducing catalyst are used for catalytic desulfurization, pass through
N2, CO and SO2Mixed gas presulfurization after the mixed gas containing oxygen and sulfur dioxide is catalyzed at 300~500 DEG C
Desulfurization.For example, electrolytic aluminum smoke desulfurization.
Further, N2, CO and SO2Volume ratio are as follows: 100~500:0.1~1:0.05~0.5.
Catalyst of the invention is to restore SO using CO2Reproducibility catalyst, product is S, catalysis reduction followed
Basic principle be redox mechanism and COS intermediate mechanism:
[redox mechanism]
MO-catalysts+2CO→M[]-catalysts+2CO2
M[]-catalysts+SO2→MO-catalysts+1/n Sn
[]: Lacking oxygen
[COS intermediate mechanism]
MO-catalysts+COS→MS-catalysts+CO2
MS-catalysts+CO→MSx-1-catalysts+COS
SO2+2COS→1/n Sn+2CO2。
The present invention uses mixed gas presulfurization, to regulate and control the status of overall reaction shared by two kinds of mechanism.Known experiment knot
Demonstration is real, and in oxygen-free environment, redox mechanism is dominant, and there is no need to carry out presulfurization to catalyst.And the present invention relates to
And be it is oxygen-containing under the conditions of catalysis reduction, redox mechanism is since Lacking oxygen is by O in the case of this2(in such as electrolytic aluminum smoke
O2) occupy and be suppressed, therefore regulated and controled by mixed gas presulfurization to strengthen COS intermediate mechanism in catalytic process
Status.
Embodiment 1
A kind of Cu-Sn-Zr reducing catalyst that Cu load capacity is 5%, the preparation process of the catalyst are as follows:
(1) raw material is weighed: 7.012g SnCl4、2.31gZrO(NO3)2、0.657gCu(NO3)2·3H2O is dissolved in 100mL
Distilled water in；
(2) adjusting the solution ph with ammonium hydroxide is 7, then is sealed with freshness protection package, and 20 or so are then pricked on freshness protection package
Hole filters under stirring in six hours of aging in draught cupboard at a temperature of 40 DEG C, is put in baking oven in 100~300 DEG C of temperature
Degree is lower to be dried 12 hours, and Muffle furnace roasting is placed into, and is raised to 600 DEG C from room temperature temperature programming, and in 600 DEG C of 4 hours of holding,
By the catalyst tabletting after roasting, the Cu load capacity for obtaining 30~50 mesh is respectively 5% catalyst.
Embodiment 2
Cu load capacity is respectively 10% and 20% Cu-Sn-Zr reducing catalyst, and preparation process and embodiment 1 are basic
Cu (NO that is identical, only adding3)2·3H2The amount of O is different.
Table 1 is the SO of the Cu-Sn-Zr catalyst of Example 1 and Example 2 of the present invention preparation2Conversion ratio table
Note: SO2Conversion ratio=1- exports SO2Concentration/entrance SO2Concentration
Embodiment 3
With SnCl4、ZrO(NO3)2、Fe(NO3)3·9H2O is raw material, according to iron load capacity be 5%, 10%, 20% point
It does not prepare, preparation process of the detailed process with Cu-Sn-Zr catalyst.
Table 2 is the SO of Fe-Sn-Zr catalyst prepared by comparative example 12Conversion ratio table
Note: SO2Conversion ratio=1- exports SO2Concentration/entrance SO2Concentration
Comparative example 1
(1) CuO-LaCoO for being 10% containing CuO is prepared3Catalyst
Preparation step is essentially identical with embodiment 1, specific as follows:
Weigh 7.485g La (NO3)3·6H2O、2.14g Co(NO3)2·6H2O、1.27g Cu(NO3)2·3H2O is dissolved in
In 100ml distilled water；Adjusting the solution ph with ammonium hydroxide is 7, then is sealed with freshness protection package, and 20 or so are then pricked on freshness protection package
Hole, under stirring, six hours of aging at a temperature of 40 DEG C, obtain the catalyst of 40 DEG C of aging temperatures, filter, be put in baking
It is dried 12 hours in case, places into Muffle furnace and roast four hours, by tabletting after roasting, obtain the CuO- for being 10% containing CuO
LaCoO3Catalyst.
(2) CuO-LaCoO for being 10% containing CuO3The SO of catalyst2Conversion ratio
Table 3 is the Cu-LaCoO of comparative example 13The SO of catalyst2Conversion ratio table
Note: SO2Conversion ratio=1- exports SO2Concentration/entrance SO2Concentration
The preparation of comparative example 2 contains SnO2For 10% Sn-LaCoO3Catalyst
Containing SnO2For 10% Sn-LaCoO3The preparation method of catalyst and essentially identical, the original only added of comparative example
Expect different.
Table 4 is the Sn-LaCoO of comparative example 23The SO of catalyst2Conversion ratio table
Note: SO2Conversion ratio=1- exports SO2Concentration/entrance SO2Concentration
The activity of the Cu-Sn-Zr catalyst of Example 1 and Example 2 of the present invention preparation is compared with comparative example 1 and comparative example 2
Activity is good, and SO can be catalyzed under the conditions of oxygen containing2Desulfurization.
In conclusion X-Sn-Zr reducing catalyst of the invention has reduction, N can be passed through2, CO and SO2It is mixed
In 300~500 DEG C of progress catalytic desulfurizations after conjunction gas presulfurization, desulfuration efficiency is high.
It is discussed in detail although the contents of the present invention have passed through above preferred embodiment, but it should be appreciated that above-mentioned
Description is not considered as limitation of the present invention.After those skilled in the art have read above content, for of the invention
A variety of modifications and substitutions all will be apparent.Therefore, protection scope of the present invention should be limited to the appended claims.
Claims (9)
1. a kind of X-Sn-Zr reducing catalyst, which is characterized in that the structure of the catalyst are as follows: XnOm-SnO2-ZrO2；Wherein, X packet
Contain: Cu and its metal of the same clan or Fe；Wherein, n:m=1:1 or 2:3；
The catalyst is used for SO2It is reduced to elemental sulfur, X in the catalystnOmQuality account for catalyst gross mass 5%~
20%.
2. X-Sn-Zr reducing catalyst according to claim 1, which is characterized in that the X-ray diffractogram of the catalyst exists
There are diffraction maximum in 2 θ=26 at 33,37,51,53,62,65.
3. X-Sn-Zr reducing catalyst according to claim 1, which is characterized in that the X-Sn-Zr reducing catalyst passes through
By raw material SnCl4、ZrO(NO3)2And Xa(NO3)bAqueous solution obtain in neutral conditions；Wherein, a:b=1:2 or 1:3.
4. X-Sn-Zr reducing catalyst according to claim 3, which is characterized in that the aqueous solution is adjusted by ammonium hydroxide
To neutrality.
5. a kind of preparation method of the X-Sn-Zr reducing catalyst as described in any one of claim 1-4, feature exist
In this method includes:
(1) it weighs raw material: weighing SnCl4、ZrO(NO3)2And Xa(NO3)b, raw material is soluble in water；
(2) adjusting aqueous solution of raw material is neutrality, is stirred under different aging temperatures, is filtered, and is dried, roasting, and tabletting is to be made not
With the catalyst of mesh number.
6. the preparation method of X-Sn-Zr reducing catalyst according to claim 5, which is characterized in that in step (1),
The SnCl4With ZrO (NO3)2Mass ratio be 3:1.
7. the preparation method of X-Sn-Zr reducing catalyst according to claim 5, which is characterized in that in step (2),
Use ammonium hydroxide adjust aqueous solution pH value be 7, the aging temperature be 20 DEG C~80 DEG C.
8. the preparation method of X-Sn-Zr reducing catalyst according to claim 5, which is characterized in that in step (2),
The reaction solution is sealed using film, and several holes are set on film, is stirred under different aging temperatures.
9. a kind of purposes of the X-Sn-Zr reducing catalyst as described in any one of claim 1-4, which is characterized in that should
X-Sn-Zr reducing catalyst is used for catalytic desulfurization, passes through N2, CO and SO2Mixed gas presulfurization after at 300~500 DEG C to containing
There is the mixed gas of oxygen and sulfur dioxide to carry out catalytic desulfurization.
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