CN106513005A - A preparing method of an iron-based composite oxide catalyst - Google Patents
A preparing method of an iron-based composite oxide catalyst Download PDFInfo
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- CN106513005A CN106513005A CN201610950981.5A CN201610950981A CN106513005A CN 106513005 A CN106513005 A CN 106513005A CN 201610950981 A CN201610950981 A CN 201610950981A CN 106513005 A CN106513005 A CN 106513005A
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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
- B01D53/8621—Removing nitrogen compounds
- B01D53/8625—Nitrogen oxides
- B01D53/8628—Processes characterised by a specific catalyst
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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
- 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
- B01J23/84—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 arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/85—Chromium, molybdenum or tungsten
- B01J23/888—Tungsten
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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
A preparing method of an iron-based composite oxide catalyst is provided. The method includes 1) dissolving a soluble iron salt, a soluble cerium salt and a soluble tungsten salt into water and performing magnetic stirring at room temperature to dissolve the salts to obtain a solution, 2) adding a certain amount of a complexing agent into the solution, and performing magnetic stirring at room temperature for 8-12 min to obtain a liquid mixture, 3) adding the liquid mixture into a microwave testing table, and performing microwave treatment at a certain power for a certain period of time to obtain gel, and 4) adding the gel into a muffle furnace and calcinating and activating the gel at 300-600 DEG C for 3-6 h to obtain the iron-based composite oxide catalyst. According to the method, microwave radiation is adopted as assistant so that preparation time is short, energy consumption is low, raw materials are easily available, the cost is reduced, and the method can be used for industrial production. The prepared iron-based composite oxide catalyst has characteristics of a wide denitration temperature window, and good middle- and low-temperature denitration activity. Nontoxic components are adopted so that the method is free of harm to human body health and ecological environment.
Description
Technical field
The invention belongs to catalyst and its preparing technical field, and in particular to a kind of system of iron-based composite oxide catalysts
Preparation Method.
Background technology
The flue gas of the coal-fired fixed source emission such as thermal power plant contains a large amount of nitrogen oxides, oxysulfide and carbon dioxide etc. and gives up
Gas, wherein, nitrogen oxides can cause the great environmental problems such as acid rain, photochemical fog, depletion of the ozone layer and greenhouse effect, right
Ecological environment and human health cause huge harm.
At present, mainly have for the technology of purification of nitrogen oxides in the fire coal stationary source tail flue gas such as thermal power plant：Low nitrogen oxygen
Compound combustion technology ,/advanced reburning technology, SNCR technology and SCR technology etc. are fired again, its
Middle SCR technology is considered as the nitrogen oxides for being most possibly applied to remove coal-fired stationary source tail flue gas
Technology.SCR technology core is catalyst, and which is mainly under catalyst action, using NH3Reducing agent is by nitrogen
Oxide is reduced into N2And H2O.At present, the widest denitrifying catalyst with selective catalytic reduction of commercial Application is V2O5-WO3
(MoO3)/TiO2, but there is denitration activity temperature window narrow (300～400 DEG C) in which, and active component vanadium is poisonous, be easy to run off, poison
Environment, easily cause secondary pollution, easily make SO2It is oxidized to SO3The shortcomings of.
Compared with vanadium tungsten titanium catalyst series, ferrum-based catalyst has that environment is nontoxic, anti-H2O and SO2Poison ability strong, de-
Nitre low cost and other advantages, and compared with expensive vanadium tungsten titanium catalyst series, ferrum-based catalyst will undoubtedly be more suitable for application
In the removing of the nitrogen oxides of China's coal fired thermal power plant discharge, but the denitration temperature window of single ferriferous oxide catalyst is inclined
Height, preparation technology are not mature enough and time-consuming longer, are unfavorable for being widely used in commercial production, therefore, exploitation is a kind of nontoxic, honest and clean
Valency, the preparation side with the catalytic-reduction denitrified activity of high selectivity and the iron-based composite oxide catalysts of wide denitration temperature window
Method, with important environment and social meaning.
The content of the invention
To solve the above problems, following technical scheme is present invention employs：
The preparation method of a kind of iron-based composite oxide catalysts that the present invention is provided, it is characterised in that including following step
Suddenly：Step 1, will be soluble ferric iron salt, solubility cerium salt, solubility tungsten salt soluble in water, and under room temperature, magnetic agitation dissolving, obtains molten
Liquid；Step 2, adds a certain amount of chelating agent in solution, and under room temperature, magnetic agitation 8～12 minutes, obtain mixed liquor；Step 3,
Mixed liquor is positioned in microwave test platform, under certain power, microwave treatment for a period of time, obtains gel；Step 4, by gel
It is put in Muffle furnace, 3～6h of calcining and activating at 300～600 DEG C obtains iron-based composite oxide catalysts.
The preparation method of a kind of iron-based composite oxide catalysts that the present invention is provided, also with following technical characteristic：Its
In, the Ce elements in ferrum element, the solubility cerium salt and the tungsten in the solubility tungsten salt in the soluble ferric iron salt
The mol ratio of element is 0.6～1:0.05～0.2:0.025～0.2.
The preparation method of a kind of iron-based composite oxide catalysts that the present invention is provided, also with following technical characteristic：Can
Dissolubility iron salt is ferric nitrate, ferrous sulfate, ferrous chloride, any one in iron sulfate；Solubility cerium salt is cerous nitrate, nitric acid
Any one in sub- cerium, cerous sulfate, cerous sulfate；Solubility tungsten salt is ammonium tungstate, any one in ammonium metatungstate.
The preparation method of a kind of iron-based composite oxide catalysts that the present invention is provided, also with following technical characteristic：Its
In, in step 2, chelating agent is citric acid.
The preparation method of a kind of iron-based composite oxide catalysts that the present invention is provided, also with following technical characteristic：Network
The mol ratio of the cation in mixture and solution is 0.25～2.
Invention effect and effect
The preparation method of a kind of iron-based composite oxide catalysts provided according to the present invention, in the method, to solution
It is middle to add a certain amount of chelating agent and be sufficiently stirred for obtaining mixed liquor, by mixed liquor microwave treatment for a period of time, obtain gel.By
In complex reaction being carried out using microwave radiation auxiliary complex-former in this process, substantially reduce the response time, so when preparing
Between it is short, and energy consumption is low, and raw material is easy to get, and reduces cost, it is easy to industrialized production.
Specific embodiment
In order that technological means, creation characteristic, reached purpose and effect that the present invention is realized are easy to understand, it is real below
Apply example to be specifically addressed the preparation method of the iron-based composite oxides of the present invention.
【Embodiment one】
A kind of preparation method of iron-based composite oxide catalysts that the present embodiment is provided, comprises the following steps：
Step 1, will be ferric nitrate, cerous nitrate and ammonium metatungstate soluble in water, and magnetic agitation 10 minutes under room temperature obtain molten
Liquid.Wherein, the mol ratio of the wolfram element in the ferrum element in ferric nitrate, the Ce elements in cerous nitrate and ammonium metatungstate is
0.9:0.05:0.05。
Step 2, adds a certain amount of citric acid in the solution for obtaining, and controls citric acid and the cation (Fe in solution3 +、Ce3+、W6+) mol ratio be 0.5, and continuing magnetic force stir 10 minutes, obtain mixed liquor.
Step 3, the mixed liquor for obtaining is positioned in microwave experiment platform, microwave treatment 10 minutes under the power of 210W,
Obtain gel.
Step 4, the gel for obtaining is put in Muffle furnace, the calcining and activating 5h in 500 DEG C of air, and iron-based composite oxygen is obtained
Compound catalyst.Obtained iron-based composite oxide catalysts are ground, sieved, it is standby to take 40～60 mesh, become iron-based and be combined
Oxide catalyst A.
Iron-based composite oxide catalysts A manufactured in the present embodiment, investigates NH on homemade micro fixed-bed reactor3
The reactivity of selective catalyst reduction of nitrogen oxides, compares 60000h in air speed-1[NO]=[NH3Under the conditions of]=1000ppm,
Iron-based composite oxide catalysts A has good NH3Selective-catalytic-reduction denitrified performance, it is in 225～425 DEG C of activity
The transformation efficiency of the oxides of nitrogen higher than 90% can be obtained in temperature window.
【Embodiment two】
A kind of preparation method of iron-based composite oxide catalysts that the present embodiment is provided, preparation method and one phase of embodiment
Together, the mol ratio of the wolfram element in the ferrum element in ferric nitrate, the Ce elements in cerous nitrate and ammonium metatungstate is changed to
0.85:0.1:0.05, iron-based composite oxide catalysts B is obtained.
Iron-based composite oxide catalysts B manufactured in the present embodiment, investigates NH on homemade micro fixed-bed reactor3
The reactivity of selective catalyst reduction of nitrogen oxides, compares 60000h in air speed-1[NO]=[NH3Under the conditions of]=1000ppm,
Iron-based composite oxide catalysts B has good NH3Selective-catalytic-reduction denitrified performance, it is in 225～400 DEG C of activity
The transformation efficiency of the oxides of nitrogen higher than 90% can be obtained in temperature window.
【Embodiment three】
A kind of preparation method of iron-based composite oxide catalysts that the present embodiment is provided, preparation method and one phase of embodiment
Together, the mol ratio of the wolfram element in the ferrum element in ferric nitrate, the Ce elements in cerous nitrate and ammonium metatungstate is changed to
0.8:0.15:0.05, iron-based composite oxide catalysts C is obtained.
Iron-based composite oxide catalysts C manufactured in the present embodiment, investigates NH on homemade micro fixed-bed reactor3
The reactivity of selective catalyst reduction of nitrogen oxides, compares 60000h in air speed-1[NO]=[NH3Under the conditions of]=1000ppm,
Iron-based composite oxide catalysts C has good NH3Selective-catalytic-reduction denitrified performance, it is in 250～400 DEG C of activity
The transformation efficiency of the oxides of nitrogen higher than 90% can be obtained in temperature window.
【Example IV】
A kind of preparation method of iron-based composite oxide catalysts that the present embodiment is provided, preparation method and one phase of embodiment
Together, the mol ratio of wolfram element in the ferrum element in ferric nitrate, the Ce elements in cerous nitrate and ammonium metatungstate is changed to into 0.75:
0.2:0.05, iron-based composite oxide catalysts D is obtained.
Iron-based composite oxide catalysts D manufactured in the present embodiment, investigates NH on homemade micro fixed-bed reactor3
The reactivity of selective catalyst reduction of nitrogen oxides, compares 60000h in air speed-1[NO]=[NH3Under the conditions of]=1000ppm,
Iron-based composite oxide catalysts D has good NH3Selective-catalytic-reduction denitrified performance, it is in 225～375 DEG C of activity
The transformation efficiency of the oxides of nitrogen higher than 90% can be obtained in temperature window.
【Embodiment five】
A kind of preparation method of iron-based composite oxide catalysts that the present embodiment is provided, preparation method and one phase of embodiment
Together, the mol ratio of wolfram element in the ferrum element in ferric nitrate, the Ce elements in cerous nitrate and ammonium metatungstate is changed to
0.875:0.1:0.025, iron-based composite oxide catalysts E is obtained.
Iron-based composite oxide catalysts E manufactured in the present embodiment, investigates NH on homemade micro fixed-bed reactor3
The reactivity of selective catalyst reduction of nitrogen oxides, compares 60000h in air speed-1[NO]=[NH3Under the conditions of]=1000ppm,
Iron-based composite oxide catalysts E has good NH3Selective-catalytic-reduction denitrified performance, it is in 250～375 DEG C of activity
The transformation efficiency of the oxides of nitrogen higher than 90% can be obtained in temperature window.
【Embodiment six】
A kind of preparation method of iron-based composite oxide catalysts that the present embodiment is provided, preparation method and one phase of embodiment
Together, the mol ratio of wolfram element in the ferrum element in ferric nitrate, the Ce elements in cerous nitrate and ammonium metatungstate is changed to
0.825:0.1:0.075, iron-based composite oxide catalysts F is obtained.
Iron-based composite oxide catalysts F manufactured in the present embodiment, investigates NH on homemade micro fixed-bed reactor3
The reactivity of selective catalyst reduction of nitrogen oxides, compares 60000h in air speed-1[NO]=[NH3Under the conditions of]=1000ppm,
Iron-based composite oxide catalysts F has good NH3Selective-catalytic-reduction denitrified performance, it is in 275～400 DEG C of activity
The transformation efficiency of the oxides of nitrogen higher than 90% can be obtained in temperature window.
【Embodiment seven】
A kind of preparation method of iron-based composite oxide catalysts that the present embodiment is provided, preparation method and one phase of embodiment
Together, the mol ratio of the wolfram element in the ferrum element in ferric nitrate, the Ce elements in cerous nitrate and ammonium metatungstate is changed to
0.8:0.1:0.1, iron-based composite oxide catalysts G is obtained.
Iron-based composite oxide catalysts G manufactured in the present embodiment, investigates NH on homemade micro fixed-bed reactor3
The reactivity of selective catalyst reduction of nitrogen oxides, compares 60000h in air speed-1[NO]=[NH3Under the conditions of]=1000ppm,
Iron-based composite oxide catalysts G has good NH3Selective-catalytic-reduction denitrified performance, it is in 275～450 DEG C of activity
The transformation efficiency of the oxides of nitrogen higher than 90% can be obtained in temperature window.
【Embodiment eight】
A kind of preparation method of iron-based composite oxide catalysts that the present embodiment is provided, preparation method and one phase of embodiment
Together, the mol ratio of the wolfram element in the ferrum element in ferric nitrate, the Ce elements in cerous nitrate and ammonium metatungstate is changed to
0.85:0.1:0.05, control citric acid and the cation (Fe in solution3+、Ce3+、W6+) mol ratio be 0.25, be obtained iron-based
Composite oxide catalysts H.
Iron-based composite oxide catalysts H manufactured in the present embodiment, investigates NH on homemade micro fixed-bed reactor3
The reactivity of selective catalyst reduction of nitrogen oxides, compares 60000h in air speed-1[NO]=[NH3Under the conditions of]=1000ppm,
Iron-based composite oxide catalysts H has good NH3Selective-catalytic-reduction denitrified performance, it is in 350～400 DEG C of activity
The transformation efficiency of the oxides of nitrogen higher than 90% can be obtained in temperature window.
【Embodiment nine】
A kind of preparation method of iron-based composite oxide catalysts that the present embodiment is provided, preparation method and one phase of embodiment
Together, the mol ratio of the wolfram element in the ferrum element in ferric nitrate, the Ce elements in cerous nitrate and ammonium metatungstate is changed to
0.85:0.1:0.05, control citric acid and the cation (Fe in solution3+、Ce3+、W6+) mol ratio be 1, be obtained iron-based be combined
Oxide catalyst I.
Iron-based composite oxide catalysts I manufactured in the present embodiment, investigates NH on homemade micro fixed-bed reactor3
The reactivity of selective catalyst reduction of nitrogen oxides, compares 60000h in air speed-1[NO]=[NH3Under the conditions of]=1000ppm,
Iron-based composite oxide catalysts I has good NH3Selective-catalytic-reduction denitrified performance, it is in 250～400 DEG C of activity
The transformation efficiency of the oxides of nitrogen higher than 90% can be obtained in temperature window.
Iron-based composite oxide catalysts A～I that embodiment one to embodiment nine is prepared carries out apparent magnetism survey
Examination, specific experiment step are as follows：
Step 1, iron-based composite oxide catalysts A～I is ground, screening, takes 80～120 mesh respectively as catalyst sample
Product.
Step 2, catalyst sample is placed in the beaker equipped with 50ml deionized waters, at normal temperatures 10 points of magnetic agitation
Clock.
Step 3, Magnet is placed on the outside of beaker, carries out apparent magnetism absorption test.
Apparent magnetism test result shows：Iron-based composite oxide catalysts A～I is respectively provided with ferromagnetism.
Embodiment is acted on and effect
The preparation method of a kind of iron-based composite oxide catalysts provided according to the present invention, in the method, to solution
It is middle to add a certain amount of chelating agent and be sufficiently stirred for obtaining mixed liquor, by mixed liquor microwave treatment for a period of time, obtain gel.By
In complex reaction being carried out using microwave radiation auxiliary citric acid in this process, substantially reduce the response time, so when preparing
Between it is short, and energy consumption is low, and raw material is easy to get, and reduces cost, it is easy to industrialized production.
Iron-based composite oxide catalysts obtained in embodiment one to embodiment nine have wider denitration temperature window 225
～450 DEG C, compare 60000h in air speed-1[NO]=[NH3Under the conditions of]=1000ppm, with good NH3Selective catalysis are also
Former denitration performance, and nontoxic component is adopted, health and ecological environment will not be worked the mischief.
Claims (5)
1. a kind of preparation method of iron-based composite oxide catalysts, it is characterised in that comprise the following steps：
Step 1, will be soluble ferric iron salt, solubility cerium salt, solubility tungsten salt soluble in water, and under room temperature, magnetic agitation dissolving, obtains
Solution；
Step 2, adds a certain amount of chelating agent in the solution, and under room temperature, magnetic agitation 8～12 minutes, obtain mixed liquor；
Step 3, the mixed liquor is positioned in microwave test platform, and under certain power, microwave treatment for a period of time, is coagulated
Glue；
Step 4, the gel is put in Muffle furnace, 3～6h of calcining and activating in 300～600 DEG C of air, obtains the iron-based
Composite oxide catalysts.
2. the preparation method of iron-based composite oxide catalysts according to claim 1, it is characterised in that：
Wherein, in the soluble ferric iron salt Ce elements and the solubility tungsten salt in ferrum element, the solubility cerium salt
In wolfram element mol ratio be 0.6～1:0.05～0.2:0.025～0.2.
3. the preparation method of iron-based composite oxide catalysts according to claim 1, it is characterised in that：
The soluble ferric iron salt is ferric nitrate, ferrous sulfate, ferrous chloride, any one in iron sulfate；
The solubility cerium salt is cerous nitrate, cerous nitrate, cerous sulfate, any one in cerous sulfate；
The solubility tungsten salt is ammonium tungstate, any one in ammonium metatungstate.
4. the preparation method of iron-based composite oxide catalysts according to claim 1, it is characterised in that：
Wherein, in step 2, the chelating agent is citric acid.
5. the preparation method of the iron-based composite oxide catalysts according to claim 1 or 4, it is characterised in that：
The mol ratio of the cation in the chelating agent and the solution is 0.25～2.
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| CN108479852A (en) * | 2018-05-14 | 2018-09-04 | 李俊霞 | A kind of preparation method of green denitrating catalyst |
| CN109046372A (en) * | 2018-09-14 | 2018-12-21 | 上海理工大学 | Iron-based composite oxidant SCR (Selective Catalytic Reduction) denitrating denitrating catalyst and its aqueous gel preparation method |
| CN109174112A (en) * | 2018-09-14 | 2019-01-11 | 上海理工大学 | Organic acid modified iron cerium tungsten composite oxidant SCR (Selective Catalytic Reduction) denitrating denitrating catalyst and preparation method |
| CN109897700A (en) * | 2019-02-19 | 2019-06-18 | 南京科技职业学院 | A kind of iron-based nano material and its application |
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| CN109046372A (en) * | 2018-09-14 | 2018-12-21 | 上海理工大学 | Iron-based composite oxidant SCR (Selective Catalytic Reduction) denitrating denitrating catalyst and its aqueous gel preparation method |
| CN109174112A (en) * | 2018-09-14 | 2019-01-11 | 上海理工大学 | Organic acid modified iron cerium tungsten composite oxidant SCR (Selective Catalytic Reduction) denitrating denitrating catalyst and preparation method |
| CN109897700A (en) * | 2019-02-19 | 2019-06-18 | 南京科技职业学院 | A kind of iron-based nano material and its application |
| CN109897700B (en) * | 2019-02-19 | 2020-11-03 | 南京科技职业学院 | Iron-based nano material and application thereof |
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