CN107175118A - The preparation method of iron-based heteropoly compound and the application that NO is removed in heterogeneous Fenton-like system - Google Patents
The preparation method of iron-based heteropoly compound and the application that NO is removed in heterogeneous Fenton-like system Download PDFInfo
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- CN107175118A CN107175118A CN201710320416.5A CN201710320416A CN107175118A CN 107175118 A CN107175118 A CN 107175118A CN 201710320416 A CN201710320416 A CN 201710320416A CN 107175118 A CN107175118 A CN 107175118A
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- iron
- heteropoly compound
- absorbing liquid
- based heteropoly
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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
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/14—Phosphorus; Compounds thereof
- B01J27/186—Phosphorus; Compounds thereof with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J27/188—Phosphorus; Compounds thereof with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium with chromium, molybdenum, tungsten or polonium
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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
- B01D—SEPARATION
- B01D2257/00—Components to be removed
- B01D2257/40—Nitrogen compounds
- B01D2257/404—Nitrogen oxides other than dinitrogen oxide
-
- 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
Abstract
NO application is removed the invention discloses a kind of preparation method of iron-based heteropoly compound and in heterogeneous Fenton-like system, the iron-based heteropoly compound is prepared by coprecipitation, comprised the following steps：Ferric chloride hexahydrate and aspartic acid are dissolved in deionized water under a, stirring, soluble complex is formed；Salkowski's solution is added dropwise in above-mentioned soluble complex under b, stirring, precipitation is formed；C, filtering, washing, drying, grinding obtain powdered iron-based heteropoly compound.The iron-based heteropoly compound and hydrogen peroxide H prepared is utilized in spouting induction flotation2O2NO in absorbing liquid removing flue gas.Easily, gas cleaning removing process is simply easily operated for the preparation method of iron-based heteropoly compound in the inventive method, and removal efficiency is high, the increase of system operation pH scopes, and small to equipment corrosion in use, post catalyst reaction is easily recycled separation.Reaction product is environmentally friendly, easy to utilize with stronger economy.
Description
Technical field
The invention belongs to flue gases purification field, and in particular to a kind of preparation method of iron-based heteropoly compound and
NO application is removed in heterogeneous Fenton-like system
Background technology
NOxExcessive emissions a series of serious environment such as acid rain, city photochemical fog, haze weather can be caused to ask
Topic.Therefore removing is as the excessive NO produced by combustion of fossil fuelxIt is a urgent problem to be solved.For increasingly serious
NOxExcessive emissions problem, China has put into effect a series of strict standard policies.Thermal power plant air pollution emission standard GB
13223-2011, it is desirable to which existing coal-burning power plant performed nitrogen oxides 100mg/m from 1 day July in 20143Pollutant emission
Standard.
At present, denitration mainly uses SCR (SCR) in coal-fired flue-gas, the use of metal oxide is catalysis
Agent, NH3NOx is reduced to N as reducing agent2, although denitration efficiency can reach 70%-90%, but face higher
The problems such as catalyst cost, the escaping of ammonia and catalyst poisoning.Compared with catalytic reduction technique, oxidative absorption method has preferable
Gas cleaning effect, key be the NO of indissoluble being oxidized to NO2, then with water or alkaline solution absorption.Oxidative absorption method
Removal efficiency is high, product recoverable and can realize simultaneous SO_2 and NO removal demercuration, is many in a kind of promising flue gas
Pollutant Collaborative Control technology.Hydrogen peroxide (the H in various oxidants2O2) have cheap, oxidation product is harmless
Oxygen and water, advantages of environment protection are more suitable for commercial Application.
(catalyst is Fe to traditional Fenton2+) and homogeneous Fenton-like (catalyst be other water miscible ions, such as Fe3 +, Cu2+) homogeneous system of method in acid condition must could maintain solution after higher removal efficiency, reaction to need alkali
In liquid and could discharge, catalyst recovery difficulty, it is difficult to large-scale application.Solid catalyst is prepared by different process, is used for
Catalyzing and decomposing H2O2Produce the hydroxyl radical free radical with strong oxidation, referred to as heterogeneous Fenton-like reaction.This method master
It is used for the removing of Organic Pollutants In Water, studies seldom in coal-fired plant flue gas processing.At present, iron system solid catalysis
The research of agent is the most extensive, can be immobilized on carrier or prepare oxide.(Polyoxometalates is abbreviated as heteropoly acid
POMs) stability is good, environmentally safe, is the green catalyst that a class has high catalytic activity, available for homogeneous and non-equal
Phase reaction.Therefore, preparing new iron-based heteropoly compound is used for the NO in heterogeneous Fenton-like system in removing coal-fired flue-gas
With larger research and application prospect.
The content of the invention
Present invention aim to address the above-mentioned problems in the prior art, there is provided a kind of iron-based heteropoly compound
Preparation method and the compound remove the application of NO in flue gas in heterogeneous Fenton-like system.
The technical scheme is that：
A kind of preparation method of iron-based heteropoly compound, comprises the following steps：
Ferric chloride hexahydrate and aspartic acid are dissolved in deionized water under a, stirring, soluble complex is formed.
Salkowski's solution is added dropwise in above-mentioned soluble complex under b, stirring, precipitation is formed.
C, filtering, washing, drying, grinding obtain powdered iron-based heteropoly compound.
Wherein, in step a, the concentration of iron chloride and aspartic acid is 0.04mol/L, mixing time 1h.
In stepb：The concentration of phosphotungstic acid is 0.015mol/L, is added dropwise under stirring, 100mL time for adding is
1h, continues to stir 2h after dripping, forms precipitation.
Step c is specially：0.22um membrane filtration suspensions, deionized water washing, 40 DEG C of vacuum drying 12h are ground
To powdered iron-based heteropoly compound.
Iron-based heteropoly compound prepared by the above method removes the application side of NO in flue gas in heterogeneous Fenton-like system
Method, by the flue gas containing NO by spouting induction flotation, contains in the reactor and contains in absorbing liquid, the absorbing liquid
Hydrogen peroxide and the iron-based heteropoly compound, wherein concentration of hydrogen peroxide 4-5mol/L, iron-based heteropoly compound addition 5-
6g/L.The concentration that flue gas enters NO before and after bubbling reactor is recorded with flue gas analyzer, the removing effect for obtaining NO is calculated
Rate.
Further, the flue gas flow rate 200-400mL/min, NO initial concentrations are less than 1250mg/m3。
Further, the initial pH value of the absorbing liquid is 45-70 DEG C of temperature in 2-6, the spouting induction flotation.
Hydrogen peroxide is the oxidant in absorbing liquid, and hydroxyl radical free radical isoreactivity material is produced in the presence of catalyst,
NO in flue gas is oxidized to NO2.The specific mechanism of action includes iron-based heteropoly compound surfaceWith
Redox reaction, and catalyst and H2O2Between hydrogen bond harsh chemical suction-operated.
In the non-equal Fenton-like system of iron-based heteropoly compound of the present invention, H2O2Pass through in catalyst surfaceRedox reaction produce oxidative free radical.Reaction mechanism is as follows：
≡Fe3++H2O2→≡Fe2++H++·OOH
≡Fe2++H2O2→≡Fe3++OH-+·OH
≡Fe3++·OOH→≡Fe2++H++O2
≡Fe2++·OOH+H+→≡Fe3++H2O2
Iron-based heteropoly compound prepared by the present invention has higher catalytic activity, its reason than general iron-based material
It isRedox reaction can also produce oxidative free radical.Reaction mechanism is as follows：
≡POM-+H2O2+H+→≡POM+H2O+·OH
≡POM-+O2→≡POM+O2 ·-
≡POM-+O2 ·-+2H+→≡POM+H2O2
Another reason of high catalytic activity is that the iron-based heteropoly compound prepared includes organic ligand amino acid, energy
Pass through Hydrogen Binding Adsorption H2O2, the local H of increase catalyst surface2O2Concentration, reduces H2O2The electron density of middle O -- O bond, favorably
H2O2Decompose and produce hydroxyl radical free radical.
The present invention is directed to the problem of NO removings are difficult in coal-fired flue-gas, proposes that a kind of wet oxidation absorbs flue gases purification.
The technology is that the miscellaneous many chemical combination of a certain amount of iron-based are added in the spouting induction flotation equipped with a certain amount of hydrogen peroxide absorbing liquid
What thing was implemented, experiment shows, in 45-70 DEG C of reaction temperature, pH value is 2-6, and flue gas flow rate 200-400mL/min, NO is initially dense
Degree is less than 1250mg/m3, removal efficiency can reach 90%.The present invention has removal efficiency high, and investment and operating cost are low, if
Standby simple, stable, catalyst is easily recycled, and valuable byproduct can be reclaimed, the features such as easy to utilize.
Brief description of the drawings
Fig. 1 is the examination of infrared spectrum figure of iron-based heteropoly compound of the present invention, wherein H3PW12O40Represent phosphotungstic acid,
FeASpPW represents the iron-based heteropoly compound prepared, it was demonstrated that there is heteropoly acid structure in the iron-based heteropoly compound.
The laboratory NO oxidative absorption schematic devices that Fig. 2 uses for the present invention, wherein：1、N2Steel cylinder；2nd, NO steel cylinders；
3、SO2Steel cylinder；4th, flowmeter；5th, gas cylinder is mixed；6th, bubbling reactor；7th, constant-temperature heating magnetic stirring apparatus；8th, drying tower；9th, cigarette
Qi leel analyzer；10th, triple valve.
Embodiment
Below in conjunction with specific embodiment, the invention will be further described.
Embodiment 1
The absorbing liquid of this example is 100mL, concentration of hydrogen peroxide 4mol/L, iron-based heteropoly compound 5g/L, initial pH value
Adjust to 5.5.The absorbing liquid configured is placed in spouting induction flotation, temperature 50 C in reactor.It is by flue gas flow
0.4L/min, NO concentration are 614mg/m3Flue gas be passed through in the bubbling reactor filled with above-mentioned absorbing liquid, can obtain
92.76% denitration efficiency.
Embodiment 2
The absorbing liquid of this example is 100mL, concentration of hydrogen peroxide 4mol/L, iron-based heteropoly compound 5g/L, initial pH value
Adjust to 5.The absorbing liquid configured is placed in spouting induction flotation, temperature 50 C in reactor.Flow is 0.4L/
Min, NO concentration are 920mg/m3Flue gas be passed through in the bubbling reactor filled with above-mentioned absorbing liquid, can obtain 90.14% it is de-
Nitre efficiency.
Embodiment 3
The absorbing liquid of this example is 100mL, concentration of hydrogen peroxide 4mol/L, iron-based heteropoly compound 5g/L, initial pH value
Adjust to 5.The absorbing liquid configured is placed in spouting induction flotation, temperature 50 C in reactor.Flow is 0.2L/
Min, NO concentration are 1227mg/m3Flue gas be passed through in the bubbling reactor filled with above-mentioned absorbing liquid, can obtain 93.33%
Denitration efficiency.
Embodiment 4
The absorbing liquid of this example is 100mL, concentration of hydrogen peroxide 4mol/L, iron-based heteropoly compound 5g/L, initial pH value
Adjust to 2.The absorbing liquid configured is placed in spouting induction flotation, temperature 50 C in reactor.Flow is 0.4L/
Min, NO concentration are 614mg/m3Flue gas be passed through in the bubbling reactor filled with above-mentioned absorbing liquid, can obtain 94.66% it is de-
Nitre efficiency.
Embodiment 5
The absorbing liquid of this example is 100mL, concentration of hydrogen peroxide 4mol/L, iron-based heteropoly compound 5g/L, initial pH value
Adjust to 4.The absorbing liquid configured is placed in spouting induction flotation, temperature 50 C in reactor.Flow is 0.4L/
Min, NO concentration are 614mg/m3Flue gas be passed through in the bubbling reactor filled with above-mentioned absorbing liquid, can obtain 88.98% it is de-
Nitre efficiency.
Embodiment 6
The absorbing liquid of this example is 100mL, concentration of hydrogen peroxide 4mol/L, iron-based heteropoly compound 5g/L, initial pH value
Adjust to 6.The absorbing liquid configured is placed in spouting induction flotation, temperature 50 C in reactor.Flow is 0.4L/
Min, NO concentration are 614mg/m3Flue gas be passed through in the bubbling reactor filled with above-mentioned absorbing liquid, can obtain 89.03% it is de-
Nitre efficiency.
Embodiment 7
The absorbing liquid of this example is 100mL, concentration of hydrogen peroxide 4mol/L, iron-based heteropoly compound 5g/L, initial pH value
Adjust to 5.5.The absorbing liquid configured is placed in spouting induction flotation, temperature 45 C in reactor.Flow is 0.4L/
Min, NO concentration are 614mg/m3Flue gas be passed through in the bubbling reactor filled with above-mentioned absorbing liquid, can obtain 90.15% it is de-
Nitre efficiency.
Embodiment 8
The absorbing liquid of this example is 100mL, concentration of hydrogen peroxide 4mol/L, iron-based heteropoly compound 5g/L, initial pH value
Adjust to 5.5.The absorbing liquid configured is placed in spouting induction flotation, 55 DEG C of temperature in reactor.Flow is 0.4L/
Min, NO concentration are 614mg/m3Flue gas be passed through in the bubbling reactor filled with above-mentioned absorbing liquid, can obtain 92.54% it is de-
Nitre efficiency.
Embodiment 9
The absorbing liquid of this example is 100mL, concentration of hydrogen peroxide 4mol/L, iron-based heteropoly compound 5g/L, initial pH value
Adjust to 5.5.The absorbing liquid configured is placed in spouting induction flotation, temperature 60 C in reactor.Flow is 0.4L/
Min, NO concentration are 614mg/m3Flue gas be passed through in the bubbling reactor filled with above-mentioned absorbing liquid, can obtain 92.13% it is de-
Nitre efficiency.
Embodiment 10
The absorbing liquid of this example is 100mL, concentration of hydrogen peroxide 4mol/L, iron-based heteropoly compound 5g/L, initial pH value
Adjust to 5.5.The absorbing liquid configured is placed in spouting induction flotation, temperature 70 C in reactor.Flow is 0.4L/
Min, NO concentration are 614mg/m3Flue gas be passed through in the bubbling reactor filled with above-mentioned absorbing liquid, can obtain 92.39% it is de-
Nitre efficiency.
Embodiment 11
The absorbing liquid of this example is 100mL, concentration of hydrogen peroxide 5mol/L, iron-based heteropoly compound 5g/L, initial pH value
Adjust to 5.5.The absorbing liquid configured is placed in spouting induction flotation, temperature 50 C in reactor.Flow is 0.4L/
Min, NO concentration are 614mg/m3Flue gas be passed through in the bubbling reactor filled with above-mentioned absorbing liquid, can obtain 92.76% it is de-
Nitre efficiency.
Embodiment 12
The absorbing liquid of this example is 100mL, concentration of hydrogen peroxide 4mol/L, iron-based heteropoly compound 6g/L, initial pH value
Adjust to 5.5.The absorbing liquid configured is placed in spouting induction flotation, temperature 50 C in reactor.Flow is 0.4L/
Min, NO concentration are 614mg/m3Flue gas be passed through in the bubbling reactor filled with above-mentioned absorbing liquid, can obtain 91.21% it is de-
Nitre efficiency.
Technical scheme is described in detail above-described embodiment.It is apparent that the present invention is not limited being retouched
The embodiment stated.Based on the embodiment in the present invention, those skilled in the art can also make a variety of changes accordingly, but
It is any to be equal or similar change belongs to the scope of protection of the invention with of the invention.
Claims (7)
1. a kind of preparation method of iron-based heteropoly compound, it is characterised in that comprise the steps：
Ferric chloride hexahydrate and aspartic acid are dissolved in deionized water under a, stirring, soluble complex is formed；
Salkowski's solution is added dropwise in above-mentioned soluble complex under b, stirring, precipitation is formed；
C, filtering, washing, drying, grinding obtain powdered iron-based heteropoly compound.
2. method according to claim 1, it is characterised in that in step a, the concentration of the iron chloride and aspartic acid is
0.04mol/L, mixing time 1h.
3. method according to claim 1, it is characterised in that in step b：The concentration of the phosphotungstic acid is 0.015mol/L,
100mL time for adding is 1h, continues to stir 2h after dripping.
4. method according to claim 1, it is characterised in that filtered in step c using 0.22um filter membranes, 40 DEG C of vacuum
Dry 12h.
5. the iron-based heteropoly compound that according to claim 1 prepared by method removes NO's in heterogeneous Fenton-like system
Application process, it is characterised in that by the flue gas containing NO by spouting induction flotation, contains absorbing liquid in the reactor,
Contain hydrogen peroxide and the iron-based heteropoly compound in the absorbing liquid, wherein concentration of hydrogen peroxide 4-5mol/L, iron-based is miscellaneous
Many compound addition 5-6g/L.
6. method according to claim 5, it is characterised in that the flue gas flow rate 200-400mL/min, NO initial concentrations are low
In 1250mg/m3。
7. method according to claim 5, it is characterised in that the initial pH value of the absorbing liquid is 2-6, the JBR
45-70 DEG C of reactor temperature.
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| CN201710320416.5A CN107175118A (en) | 2017-05-09 | 2017-05-09 | The preparation method of iron-based heteropoly compound and the application that NO is removed in heterogeneous Fenton-like system |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111905547A (en) * | 2019-05-07 | 2020-11-10 | 山东师范大学 | Method for oxidizing low-concentration NO in gas by using hydrogen peroxide |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111905547A (en) * | 2019-05-07 | 2020-11-10 | 山东师范大学 | Method for oxidizing low-concentration NO in gas by using hydrogen peroxide |
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