CN104548904A - Technology for liquid-phase complexing absorption of NO with iron-based chelate - Google Patents
Technology for liquid-phase complexing absorption of NO with iron-based chelate Download PDFInfo
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- CN104548904A CN104548904A CN201310483742.XA CN201310483742A CN104548904A CN 104548904 A CN104548904 A CN 104548904A CN 201310483742 A CN201310483742 A CN 201310483742A CN 104548904 A CN104548904 A CN 104548904A
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02C—CAPTURE, STORAGE, SEQUESTRATION OR DISPOSAL OF GREENHOUSE GASES [GHG]
- Y02C20/00—Capture or disposal of greenhouse gases
- Y02C20/10—Capture or disposal of greenhouse gases of nitrous oxide (N2O)
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Abstract
The invention relates to a technology for liquid-phase complexing absorption of NO with an iron-based chelate. A chelate (Fe<2+>TEA) solution is used for removing NO in industrial and combustion tail gas, the NO which is absorbed through complexing and enters the liquid phase is converted into ammonia with a cathode electrolysis method, and meanwhile, Fe<3+>TEA produced by oxidizing Fe<2+>TEA is reduced to the Fe<2+>TEA.
Description
Art
The present invention relates to the administering method of NOx pollutant in industrial smoke.
Background technology
Nitrogen oxide (NO
x) be one of major pollutants causing atmosphere pollution, and SO
2the same, be the atmosphere pollution forming acid rain and acid mist, and cause the environmental problem such as soil acidification, water resource pollution, have significant damage to ecological environment and health.The harm of NOx is also embodied in the destruction to atmospheric environment, and NO can significantly as fluorochlorohydrocarbon damage the ozone layer, simultaneously NO and N
2o is also greenhouse gases, and in addition, NO and hydrocarbons chemical reaction can occur under the effect of sunlight, cause photochemical pollution.
Flue-gas denitration process is divided into wet method and Dry denitration technology by absorbent is different with removing product state.Dry denitration technology as SCR method, SNCR method, active carbon adsorption and electron beam irradiation method etc. also exist that range of application is narrow, smoke processing system is complicated respectively, Construction and operation costly, waste catalyst forms the shortcomings such as secondary pollution, power consumption are large; And wet denitration technology alternatively, often SO can be realized
2remove with while NOx, there is the advantages such as flue gas managing technique flow process is short, equipment is simple.But 95% is NO in the NOx pollutant in flue gas, extremely difficult water-soluble (when 50 DEG C, the solubility of NO in water is 38mg/L, is SO
2and NO
2less than 1/1000), therefore conventional soda liquor absorption technique is substantially invalid to NO.There are some researches show, the transition metal such as iron, cobalt, nickel can form the complex compound (bibliography: Ind. Eng. Chem. Process Des. Dev. 1978,17,321-324 of π-sour ligand with NO; Ind. Eng. Chem. Process Des. Dev. 1985,24,149-152), and after these transition metal and some part form chelate, greatly can promote the formation of metal and NO complex compound, and wherein with the complexing fastest (bibliography: Ind. Eng. Chem. Res. 1987,26,2016-2019) of ferrous chelate compound and NO.Ferrous chelate forms nitrosyl complex and complexing NO(bibliography: Ind. Eng. Chem. Fundam. 1984,23,60-64).In follow-up research, it is found that two class parts and ferrous iron can complexing NO: class be aminocarboxylic acids parts fast after forming chelate, as ethylenediamine tetra-acetic acid (EDTA), two pentaacetic acids (DTPA), NTA (NTA) etc.Such as, the chelate Fe that formed of EDTA and Fe (II)
2+-EDTA can by the quick complexing NO of following formula:
Another kind of is the sulfydryl class part containing SH-, as cysteine (CySH), glutathione (GSH), dimercaptopropane base sulfonate (DMPS) etc.Such as, DMPS and ferrous chelate Fe
2+-(DMPS)
2following formula complexing NO(bibliography is pressed: Nature, 1994,369:139-141 with NO):
The performance of different parts on ferrous chelate compound complexing NO has remarkable impact.First kind aminocarboxylic acids ferrous chelate compound has complexing NO ability faster, but the ferrous iron in chelate is very easily by the impact of oxygen, the ferrous iron in ferrous chelate compound can be caused to be oxidized to ferric iron rapidly, lose the ability (bibliography: Ind. Eng. Chem. Res. of complexing NO, 1987,26:1468-1472, Ind. Eng. Chem. Res., 1993,32:2580-2594).Although people once attempted the methods such as bioanalysis regeneration, catalytic regeneration, reducing agent regeneration, totally regenerated difficulty, be difficult to commercial Application.In addition, this kind of part itself is also easily oxidized, makes ferrous chelate compound loss amount large.In order to improve the antioxygen property of ferrous chelate compound, it is found that Equations of The Second Kind part, namely containing the propylhomoserin of SH-or the ferrous huge legendary turtle compound (bibliography: Ind. Eng. Chem. Res., 1988,27:2156-2161 of peptide; Environ. Prog. 1997,16:301-306), due to the effect of SH-group, it can stablize the ferrous ion in alkaline solution, the iron ion that oxidation generates can be reduced into ferrous ion.But this kind of part is also in the laboratory research stage, some problems need to solve, and such as, such complexes absorption is at absorption NO and reduction Fe
3+time, the continuous oxidized needs of sulfhydryl compound reduce in time, and this type of chelate synthesis technique is complicated simultaneously, expensive, commercial Application difficulty.
The present invention is open a kind of cheland promoting ferrous complexing NO efficiency, and uses the method for ferrous chelate compound complexed absorption NO of this cheland, to overcome the defect in prior art, realizes low cost and administers nitrogen oxides pollution.
Summary of the invention
The present invention is open a kind of cheland promoting ferrous complexing NO efficiency: triethanolamine (TEA), and uses triethanolamine and ferrous chelate as absorbent, the method for complexed absorption NO.The method may be used for the NO pollution control of the industrial process such as nitric acid industry, nonferrous industry, nitrated operation, and the high-efficient purification that in combustion product gases, NOx pollutes.
The method first ferrous salt and triethanolamine is formed ferrous triethanolamine chelate (Fe at reactant aqueous solution
2+tEA), then add highly basic (as NaOH, KOH etc.) and regulate pH to alkalescence, obtain the complex solution that can be used for NO absorption.The ferrous chela agent contained in this complexed absorption liquid in the offgas aerobic is deposited in case, also very fast with the complex reaction speed of NO, all can obtain higher NO absorption rate in bubbling reactor, counter current contacting formula reactor.After solution absorbs the decline of NO speed, use electrolysis to regenerate ferrous chelating liquid, on the one hand, make to be oxidized into Fe
3+the chelating agent of TEA is reduced to Fe
2+tEA, the NO that another aspect complexing enters solution is reduced to NH
4 +, the solution after regeneration is reused after ammonia removal in the basic conditions.The general principle that whole process relates to is as follows:
1) ferrous ion and the triethanolamine aqueous solution form chelate, and course of reaction is as follows:
2) ferrous triethanolamine chelating agent (Fe
2+tEA) complexed absorption NO in the basic conditions, its course of reaction is as follows:
3) in absorbent use procedure, complexes absorption Fe
2+ferrous iron in TEA can by the O in gas
2the ferric iron that is oxidized to, generates Fe
3+tEA, thus lose complexing NO ability.Course of reaction is as follows
Fe
3+tEA can be reduced by the method for electrolysis, and regenerative response is as follows:
4) from after the NO gas phase is entered liquid phase by complexing, under the effect of electrolysis, obtain electronics, can NH be converted to
4 +, when concentration accumulation reaches a timing, in the basic conditions can by stripping.Course of reaction is as follows:
The technical scheme realizing the object of the invention in turn includes the following steps:
(1) preparation of complex solution: ferrous salt, triethanolamine are dissolved in aqueous.After placing a period of time, add a certain amount of highly basic and regulate solution basicity, finally obtain the complexed absorption liquid of NO.
The ferrous salt chatted can be ferrous sulfate, in frerrous chloride, ferrous nitrate any one, or several combination, preferential recommendation ferrous sulfate.
Described highly basic, can be in NaOH, KOH any one, or two kinds of combinations, preferential recommendation NaOH.
With Fe in described complexed absorption liquid
2+the chelate concentration of meter is 0.01 ~ 0.3mol/L, and recommended density is: 0.05 ~ 0.15mol/L, and strong base concentrations is 0.5 ~ 2mol/L.
Described standing time is 0.5 ~ 3 hour.
(2) complexed absorption NO: complexed absorption liquid can carry out the reaction of the NO removed in waste gas in conventional gas-liquid reactor, and not having particular/special requirement to reactor types, can be bubble tower, plate column, packed tower or other forms of gas-liquid reactor.
NO concentration range of the present invention is 10 ~ 1500ppm, O
2concentration be 0 ~ 15%.
Absorption operation pressure is normal pressure, and temperature range is 10 ~ 80 DEG C, and recommended temperature is 20 ~ 50 DEG C.
(3) regeneration of complexes absorption: the cathode can that the absorbent solution after step (2) is absorbed NO is sent in electrolytic cell is reacted, Fe
3+fe in TEA
3+obtain electronics, reduction becomes Fe
2+, Fe simultaneously
3+in TEA (NO), NO and water one react and generate NH
4 +.Be NaOH or the KOH solution of concentration 0.1 ~ 2mol/L in anode slot.Separated by amberplex between anode slot and cathode can.
Described electric tank cathode material can be the materials such as stainless steel, graphite, silver, nickel, platinum, and recommendation cathode electrode material is stainless steel.
Decomposition voltage is 1.1 ~ 3.0V, and recommendation voltage is 1.2 ~ 1.5V, and temperature range is 15 ~ 45 DEG C, and operating pressure is normal pressure.
The present invention is by adopting Fe
2+-TEA makees absorbent, under alkaline aqueous environment, and the NO pollutant in complexed absorption gas, and be converted to NH by electrolytic reduction by by the NO of complexing
4 +, make the Fe3+ reduction being oxidized to three valence states for ferrous simultaneously, thus regenerates active absorbent components Fe
2+-TEA.When ammonia be accumulated to a certain amount of after, send ammonia still to remove.
The present invention, compared with other techniques, has following characteristics.
1. the present invention adopts triethanolamine and the absorbent of ferrous chelate as NO in complexed absorption flue gas, and relative to the ferrous chelate compound of aminocarboxylic acids part and sulfydryl class part, it has higher absorption rate.
2. the speed impact of oxygen on the complexed absorption NO of triethanolamine ferrous chelate compound is comparatively little.
3. use the renewable oxidized absorbent of method of electrolysis, and make to be converted to NH by the NO of complexing
4 +, realize the regeneration of ferrous chelating absorbent solution and recycle, being easy to realize commercial Application.
4. with TEA as the part of ferrous iron, cheap, be easy to get, safe, nontoxic.
Accompanying drawing explanation
Fig. 1 is a kind of flow chart of the present invention.
Symbol description:
In accompanying drawing: 1-contains the waste gas of NO, 2-ferrous sulfate, 3-triethanolamine, 4-NaOH, 5-water, waste gas after 6-purification, 7-mixing channel, 8-NO absorption reactor thermally, 9-electric tank cathode groove, 10-anode electrolytic cell groove, 11-dc source, 12-deamination device, 13-ammonia.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is further elaborated, but protection scope of the present invention is not limited in this.
Below in conjunction with specific embodiment, the present invention is further elaborated, but protection scope of the present invention is not limited in this.
Embodiment 1:
The experiment that complex solution absorbs NO is 5cm at diameter, carries out in the bubbling reactor of high 25cm, wherein:
Green vitriol (FeSO in complex solution
47H
2o) molar concentration is 0.19mol/L, and the molar concentration of triethanolamine is the molar concentration of 0.25mol/L, NaOH is 0.9mol/L, complex solution cumulative volume 400mL.
Simulated exhaust forms: the flow of nitrogen is 1.35L/min, and nitric oxide production flow is 1.3mL/min, at normal temperatures NO and N
2after mixing in mixing channel, obtain NO entrance concentration by being 128ppm by apparatus measures.Gas is passed in bubbling reactor, and complex solution absorbs NO in bubbling reactor, and after stablizing a period of time, record the 20ppm of NO outlet, denitration efficiency is 84.38%.
Embodiment 2:
The experiment that complex solution absorbs NO is 5cm at diameter, carries out in high 25cm bubbling reactor, wherein:
Green vitriol (FeSO in complex solution
47H
2o) molar concentration is 0.19mol/L, and the molar concentration of triethanolamine is the molar concentration of 0.25mol/L, NaOH is 0.9mol/L, complex solution cumulative volume 400mL.
Simulated exhaust forms: the flow of nitrogen is 1.35L/min, and nitric oxide production flow is 3.0mL/min, at normal temperatures NO and N
2after mixing in mixing channel, obtain NO entrance concentration by being 309ppm by apparatus measures.Gas is passed in bubbling reactor, and complex solution absorbs NO in bubbling reactor, and after stablizing a period of time, record the 65ppm of NO outlet, denitration efficiency is 78.96%.
Embodiment 3:
The experiment that complex solution absorbs NO is 5cm at diameter, carries out in high 25cm bubbling reactor, wherein:
Green vitriol (FeSO in complex solution
47H
2o) molar concentration is 0.15mol/L, and the molar concentration of triethanolamine is the molar concentration of 0.2mol/L, NaOH is 2.0mol/L, complex solution cumulative volume 400mL.
Simulated exhaust forms: the flow of nitrogen is 1.35L/min, and nitric oxide production flow is 1.1mL/min, and the flow of oxygen is 100mL/min, at normal temperatures NO and N
2after mixing in mixing channel, obtain NO entrance concentration by being 108ppm by apparatus measures.Gas is passed in bubbling reactor, and complex solution absorbs NO in bubbling reactor, and after stablizing a period of time, record the 48ppm of NO outlet, denitration efficiency is 55.56%.
Embodiment 4:
After ferrous chelating agent in example 3 reacts a period of time in aerobic situation, after denitration efficiency reduces to 30.28%, the cathode can that reaction solution now passes in electrolytic cell being reacted, looping back bubbling reactor by completing the ferrous chelating agent after electrode reaction.Gas composition is: the flow of nitrogen is 1.35L/min, and nitric oxide production flow is 1.1mL/min, absorbs in bubbling reactor to NO, records NO concentration and is down to 30ppm by 108ppm, and denitration efficiency is 72.22%.
Find out that ferrous chelate compound liquid phase similar with other removes compared with NO by above-mentioned example, this Technical expression has gone out very high denitration efficiency.
Claims (7)
1. the technique of an iron-based chelate liquid complexing absorption NO, it is characterized in that carrying out as follows: (1) ferrous salt and part thereof are dissolved in aqueous, allow it place, react a period of time generation iron-based chelate, add a certain amount of highly basic again and regulate solution basicity, finally obtain can be used for the complexed absorption liquid that NO removes; (2) this complexed absorption liquid carries out the reaction of the NO removed in waste gas in conventional gas-liquid reactor, and reactor types can be bubble tower, plate column, packed tower or other forms of gas-liquid reactor; (3), by step (2), the cathode can completed in the solution feeding electrolytic cell after NO absorption is carried out cell reaction, then is born the iron-based chelate for complexed absorption NO; Be NaOH or the KOH solution of concentration 0.1 ~ 2mol/L in anode slot; Separated by amberplex between anode slot and cathode can.
2. iron-based chelate liquid complexing according to claim 1 absorbs the technique of NO, it is characterized in that: the part of iron-based chelate is triethanolamine (TEA); Iron-based chelate for complexing NO is Fe
2+tEA.
3. iron-based chelate liquid complexing according to claim 1 absorbs the technique of NO, it is characterized in that: ferrous salt is ferrous sulfate, a kind of in frerrous chloride, ferrous nitrate, or several combination; With Fe in complexed absorption liquid
2+the chelate concentration of meter is 0.01 ~ 0.3mol/L.
4. iron-based chelate liquid complexing according to claim 1 absorbs the technique of NO, it is characterized in that: highly basic is a kind of in NaOH, potassium hydroxide, or two kinds of combinations; In complexed absorption liquid, concentration of lye is 0.5 ~ 2mol/L.
5. iron-based chelate liquid complexing according to claim 1 absorbs the technique of NO, and it is characterized in that: absorption operation pressure is normal pressure, temperature range is 10 ~ 80 DEG C, and NO concentration range is 10 ~ 1500ppm, O
2concentration be 0 ~ 15%.
6. iron-based chelate liquid complexing according to claim 1 absorbs the technique of NO, and it is characterized in that: absorbing liquid is electrolytic regeneration in cathode can, decomposition voltage is 1.1 ~ 3.0V, temperature 15 ~ 45 DEG C, atmospheric operation.
7. iron-based chelate liquid complexing according to claim 1 absorbs the technique of NO, it is characterized in that: electrolytic tank electrode material is a kind of in stainless steel, graphite, silver, nickel, platinum, or two kinds of combinations.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105854527A (en) * | 2016-04-18 | 2016-08-17 | 青岛海德威科技有限公司 | Waste-gas denitration device and method |
| CN106237791A (en) * | 2016-09-06 | 2016-12-21 | 中南大学 | The method that nitrogen resource is reclaimed in the efficient complexed absorption of a kind of NO/electro-catalysis reduction |
| CN108793104A (en) * | 2017-04-28 | 2018-11-13 | 北京阳光欣禾科技有限公司 | A kind of nitric oxide phase transfer catalyzed methods |
| CN110756170A (en) * | 2019-11-12 | 2020-02-07 | 常熟理工学院 | Preparation method of expanded perlite sulfur-carrying modified patina adsorbent |
| CN114014281A (en) * | 2022-01-05 | 2022-02-08 | 浙江陶特容器科技股份有限公司 | Preparation method of high-purity nitric oxide and application of high-purity nitric oxide in semiconductor manufacturing process |
| CN114870819A (en) * | 2022-05-17 | 2022-08-09 | 桂林理工大学 | Aerobic atmosphere synthesis method of Fe (II) -MOF-74 material with NO adsorption performance |
| CN115676850A (en) * | 2022-10-11 | 2023-02-03 | 电子科技大学 | Method for synthesizing ammonia by Fe (II) EDTA-assisted photocatalysis of NO |
| CN115715915A (en) * | 2022-11-11 | 2023-02-28 | 大连理工大学 | Denitration method for selectively converting nitric oxide into ammonium nitrate by membraneless paired electrolysis |
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Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105854527A (en) * | 2016-04-18 | 2016-08-17 | 青岛海德威科技有限公司 | Waste-gas denitration device and method |
| CN105854527B (en) * | 2016-04-18 | 2019-05-07 | 海德威科技集团(青岛)有限公司 | A kind of exhaust gas denitration device and method |
| CN106237791B (en) * | 2016-09-06 | 2019-07-23 | 中南大学 | A kind of method of the efficient complexed absorption of NO/electro-catalysis reduction recycling nitrogen resource |
| CN106237791A (en) * | 2016-09-06 | 2016-12-21 | 中南大学 | The method that nitrogen resource is reclaimed in the efficient complexed absorption of a kind of NO/electro-catalysis reduction |
| CN108793104B (en) * | 2017-04-28 | 2021-01-08 | 北京阳光欣禾科技有限公司 | Nitric oxide phase transfer catalysis method |
| CN108793104A (en) * | 2017-04-28 | 2018-11-13 | 北京阳光欣禾科技有限公司 | A kind of nitric oxide phase transfer catalyzed methods |
| CN110756170A (en) * | 2019-11-12 | 2020-02-07 | 常熟理工学院 | Preparation method of expanded perlite sulfur-carrying modified patina adsorbent |
| CN110756170B (en) * | 2019-11-12 | 2021-10-29 | 常熟理工学院 | Preparation method of expanded perlite sulfur-carrying modified patina adsorbent |
| CN114014281A (en) * | 2022-01-05 | 2022-02-08 | 浙江陶特容器科技股份有限公司 | Preparation method of high-purity nitric oxide and application of high-purity nitric oxide in semiconductor manufacturing process |
| CN114014281B (en) * | 2022-01-05 | 2022-06-21 | 宿州伊维特新材料有限公司 | Preparation method of high-purity nitric oxide and application of high-purity nitric oxide in semiconductor manufacturing process |
| CN114870819A (en) * | 2022-05-17 | 2022-08-09 | 桂林理工大学 | Aerobic atmosphere synthesis method of Fe (II) -MOF-74 material with NO adsorption performance |
| CN114870819B (en) * | 2022-05-17 | 2023-08-11 | 桂林理工大学 | Aerobic atmosphere synthesis method of Fe (II) -MOF-74 material with NO adsorption performance |
| CN115676850A (en) * | 2022-10-11 | 2023-02-03 | 电子科技大学 | Method for synthesizing ammonia by Fe (II) EDTA-assisted photocatalysis of NO |
| CN115715915A (en) * | 2022-11-11 | 2023-02-28 | 大连理工大学 | Denitration method for selectively converting nitric oxide into ammonium nitrate by membraneless paired electrolysis |
| CN115715915B (en) * | 2022-11-11 | 2024-08-13 | 大连理工大学 | Denitration method for selectively converting nitric oxide into ammonium nitrate by membraneless paired electrolysis |
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