CN105854541A - Method for reducing and removing nitrogen oxide by adsorption-oxidation and liquid phase absorption - Google Patents

Method for reducing and removing nitrogen oxide by adsorption-oxidation and liquid phase absorption Download PDF

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Publication number
CN105854541A
CN105854541A CN201610338798.XA CN201610338798A CN105854541A CN 105854541 A CN105854541 A CN 105854541A CN 201610338798 A CN201610338798 A CN 201610338798A CN 105854541 A CN105854541 A CN 105854541A
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nitrogen
molecular sieve
nitrogen oxides
gas
nitrogen oxide
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CN201610338798.XA
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Inventor
张光旭
张国孟
王战科
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Wuhan University of Technology WUT
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Wuhan University of Technology WUT
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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
    • B01D53/46—Removing components of defined structure
    • B01D53/54—Nitrogen compounds
    • B01D53/56—Nitrogen oxides
    • 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
    • B01D53/02—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 by adsorption, e.g. preparative gas chromatography
    • B01D53/04—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 by adsorption, e.g. preparative gas chromatography with stationary adsorbents
    • 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
    • B01D53/02—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 by adsorption, e.g. preparative gas chromatography
    • B01D53/04—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 by adsorption, e.g. preparative gas chromatography with stationary adsorbents
    • B01D53/0407—Constructional details of adsorbing systems
    • B01D53/0438—Cooling or heating systems
    • 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
    • B01D53/46—Removing components of defined structure
    • B01D53/54—Nitrogen compounds
    • B01D53/56—Nitrogen oxides
    • B01D53/565—Nitrogen oxides by treating the gases with solids
    • 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
    • B01D53/77—Liquid phase processes
    • B01D53/78—Liquid phase processes with gas-liquid contact
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2253/00—Adsorbents used in seperation treatment of gases and vapours
    • B01D2253/10—Inorganic adsorbents
    • B01D2253/106—Silica or silicates
    • B01D2253/108—Zeolites
    • B01D2253/1085—Zeolites characterized by a silicon-aluminium ratio
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2259/00—Type of treatment
    • B01D2259/40—Further details for adsorption processes and devices
    • B01D2259/40083—Regeneration of adsorbents in processes other than pressure or temperature swing adsorption
    • B01D2259/40088—Regeneration of adsorbents in processes other than pressure or temperature swing adsorption by heating

Abstract

The invention discloses a method for reducing and removing nitrogen oxide by adsorption-oxidation and liquid phase absorption. The method comprises the following steps: (1) letting exhaust gas containing nitrogen oxide to pass through a fixed bed reactor filled with a molecular sieve to oxidize part of the nitrogen oxide and adsorb the nitrogen oxide on the molecular sieve; (2) stopping feeding the exhaust gas, feeding carrier gas (air or nitrogen), and performing heating desorption on a bed layer of the molecular sieve in a WF-01 differential integral reactor; (3) absorbing desorbed gas with a sodium sulfite in a filler tower, to finally reduce the gas into nitrogen. According to the method disclosed by the invention, efficient and low-cost removal of the nitrogen oxide is realized; desorbed nitrogen dioxide is 80 percent or higher of the total volume of the desorbed nitrogen oxide; after the gas is absorbed and reduced with the sodium sulfite solution, the denitrification rate can be up to 80 percent or higher.

Description

A kind of adsorption and oxidation combines the method for liquid phase scrubbing reduction removing nitrogen oxides
Technical field
The present invention relates to the process of various production process nitrogen oxides in effluent, particularly a kind of adsorption and oxidation combines liquid phase scrubbing also Nitrogen oxides in former removing flue gas so that it is the method being reduced to nitrogen.
Background technology
Nitrogen oxides is one of primary pollution source causing atmospheric pollution, and its discharge not only can cause acid rain, photochemical fog, also Can damage the ozone layer, bring serious harm to natural environment and human being's production, life；Therefore flue gas has to pass through de-before discharging Nitre processes.
Use the main selective catalysis reduction of gas denitrifying technology and the non-selective catalytic reduction two kinds of comparative maturity at present.Non- Selective-catalytic-reduction denitrified effect is poor, and denitration rate is typically about 40%；Use the most promising the widest denitrating technique at present For SCR (SCR) technology.But the method there is problems in that engineering cost is extremely expensive, operating cost is also The highest, floor space is big；Course of reaction ammonia amount need to accurately control, and is susceptible to ammonia leakage；Reaction temperature height and temperature window Mouth is narrow；Time in flue gas containing sulfur dioxide, have a strong impact on the service life of catalyst.
Nitric oxide total amount accounts for more than the 90% of nitrogen oxides in effluent cumulative volume, and it is water insoluble, and direct liquid phase scrubbing is difficult. In recent years, relevant employing oxidant such as NaClO2、H2O2、ClO2、O3Deng being directly two by the oxidation of nitric oxide in flue gas Nitrogen oxide is in conjunction with the research of liquid phase scrubbing.Research finds, when nitrogen dioxide accounts for 50% left side of nitrogen oxides in effluent total amount Time right, sodium alkali assimilation effect is preferable, and when nitrogen dioxide proportion is higher, liquid-phase reduction is more favourable.But all things considered, Institute's development approach all fails fully up to expectations at present, and such as restricted application, reaction condition requirement is high, device is loaded down with trivial details, energy and material consumption Conversion ratio higher, nitrogen oxides is low.Researcher is still exploring more preferably nitrogen oxides treatment method both at home and abroad.
Summary of the invention
The technical problem to be solved is: overcome deficiency of the prior art, it is provided that a kind of adsorption and oxidation combines liquid phase and inhales Receive the method that reduction removes the nitrogen oxides in flue gas.
The present invention solves its technical problem and uses following technical scheme:
The adsorption and oxidation that the present invention provides combines the method for liquid phase scrubbing reduction removing nitrogen oxides, specifically uses and includes following step Rapid method:
(1) by the flue gas containing nitrogen oxides by being filled with the fixed bed reactors of molecular sieve, nitrogen oxides partial oxidation is made also Absorption is over a molecular sieve；
(2) stop being passed through flue gas, be passed through nitrogen or air, in WF-01 type integral calculus reactor, molecular sieve added Thermal desorption；
(3) gas being desorbed out absorbs with sodium sulfite solution in packed tower and is reduced to nitrogen.
In said method, fixed bed reactors used are internal diameter 10～14mm, can packed height be 16～20cm quartz glass Pipe.
In said method, molecular sieve used be silica alumina ratio be the one in the H-ZSM-5 type molecular sieve of 25～500, particle diameter is 12～32 Mesh.
In said method, the reaction temperature of described activating pretreatment molecular sieve is 500～550 DEG C, and the time is 2～3h.
In said method, during absorption, flue gas tolerance is 6L/min, and nitrogen oxides volumetric concentration is 0.1%～0.15%.
In said method, the adsorptive pressure of nitric oxide adsorption is normal pressure, and adsorption temp is 10 DEG C～30 DEG C.
In said method, under being passed through nitrogen or air conditions, adsorb saturated after molecular sieve WF-01 type integral calculus react Device regenerates in 450～550 DEG C.
In said method, the molar concentration of sodium sulfite used is 0.03～0.07mol/L, and temperature is 6～12 DEG C.
In said method, when liquid-phase reduction, the volumetric concentration of nitrogen oxides is 0.07%～0.19%, and the time of staying of gas is 0.4～0.7s, the liquid-gas ratio of packed tower is 9～15L/m3, filler is glass spring filler.
In said method, the nitrogen oxides being desorbed out is reduced to conversion ratio >=80% of nitrogen.
The present invention compared with prior art has a following main advantage:
(1) the high efficiency, low cost removing of nitrogen oxides is achieved.
First make the waste gas containing nitrogen oxides by being filled with in the fixed bed reactors of adsorbent, make nitrogen oxides partial oxidation also It is adsorbed on adsorbent；Nitrogen oxide absorbent to a certain extent after, heat adsorbent bed desorption, desorption gas out Body enters in reduction tower and reduces, and nitrogen oxides is reduced to nitrogen and directly discharges, it is achieved thereby that the high efficiency, low cost of nitrogen oxides Removing.Use can be continued cycling through after reacted adsorbent desorption.
(2) consumption of material and the generation of garbage are decreased.
Reprocess after making nitrogen oxides enrichment, reducing the air inflow of directly process, reducing follow-up equipment size, if combining soda Method desulfurization is used together, then may utilize by-product sodium sulfite that desulfurization produces for denitration, decreases the consumption of material and discarded The generation of thing.
(3) practical:
Can be widely applied to the removing of nitrogen oxides in industrial tail gas, flue gas, absorption and liquid phase scrubbing reduction process are all often Carry out under normal temperature and pressure, it is to avoid traditional handicraft couple, because of what wet desulphurization cooling caused, the energy consumption increasing brought with SCR method denitrating technique Adding, adsorbent low cost and energy regeneration cycle, whole process energy and material consumption is low, and nitrogen oxides is reduced to the conversion ratio of nitrogen can Reach more than 80%.There is good economy and environmental benefit.
Detailed description of the invention
Below in conjunction with embodiment, the invention will be further described, only for technology design and the feature of the explanation present invention, but does not constitutes Any limitation of the invention.
Embodiment 1:
(1) H-ZSM-5 molecular sieve being pulverized, sieved, obtaining particle diameter is 12～32 mesh particulate molecular sieve, horse at 500 DEG C Stove is not dried 2h, is then placed in equipped with the drying basin of silica gel is cooled to room temperature；
(2) taking 3g silica alumina ratio is that 25H-ZSM-5 molecular sieve is placed in fixed bed reactors, will be containing nitrogen oxides (volumetric concentration Be 0.1%～0.15%) and the mixed gas (total flow 6L/min) of oxygen (volumetric concentration is 20.8%) by adsorbent bed, At 10 DEG C～30 DEG C, absorption reaches saturated；
(3) molecular sieve after saturated absorption is warmed up to 500 DEG C in WF-01 type integral calculus reactor and carries out desorption and regeneration, In desorption gas, nitrogen dioxide accounts for the 82% of nitric oxide and nitrogen dioxide volume total amount；
(4) with nitrogen or air as carrier gas, controlling import nitrogen oxides volumetric concentration is 0.126%, and oxidizability is 82%, stops Time is 0.5s, and temperature is 10 DEG C, and liquid-gas ratio is 12L/m3, when sodium sulfite solution molar concentration is 0.0525mol/L, by cigarette Edema caused by disorder of QI analyzer records final nitrogen oxides and is reduced to the conversion ratio of nitrogen is 80%.
Embodiment 2:
With embodiment 1, sodium sulfite solution molar concentration is 0.07mol/L, and other conditions are constant, records final nitrogen oxides also Originally be the conversion ratio of nitrogen be 82%.
Embodiment 3:
(1) H-ZSM-5 molecular sieve being pulverized, sieved, obtaining particle diameter is 12～32 mesh particulate molecular sieve, at 500 DEG C Muffle furnace is dried 2h, is then placed in equipped with the drying basin of silica gel is cooled to room temperature；
(2) taking 3g silica alumina ratio is that 150H-ZSM-5 molecular sieve is placed in fixed bed reactors, will (volume is dense containing nitrogen oxides Degree 0.1%～0.15%) and oxygen (volumetric concentration 20.8%) mixed gas (total flow 6L/min) pass through adsorbent bed, At 10 DEG C～30 DEG C, absorption reaches saturated；
(3) molecular sieve after saturated absorption is warmed up to 500 DEG C in WF-01 type integral calculus reactor and carries out desorption and regeneration, In desorption gas, nitrogen dioxide accounts for the 84% of nitric oxide and nitrogen dioxide volume total amount；
(4) being 0.035mol/L in sodium sulfite molar concentration, import nitrogen oxides degree is about 83%, and temperature is 6 DEG C, The time of staying is 0.5s, and liquid-gas ratio is 12L/m3, when nitrogen oxides volumetric concentration is 0.1%, flue gas analyzer record final nitrogen oxygen It is 80% that compound is reduced to the conversion ratio of nitrogen.
Case study on implementation 4
With embodiment 3, nitrogen oxides volumetric concentration is 0.07%, and other conditions are constant, records final nitrogen oxides and is reduced to nitrogen Conversion ratio be 87%.
Embodiment 5:
(1) H-ZSM-5 molecular sieve being pulverized, sieved, obtaining particle diameter is 12～32 mesh particulate molecular sieve, horse at 500 DEG C Not stove is dried 2h, is then placed in equipped with being cooled to room temperature in the drying basin of silica gel；
(2) taking 3g silica alumina ratio is that 300H-ZSM-5 molecular sieve is placed in fixed bed reactors, will (volume is dense containing nitrogen oxides Degree is 0.1%～0.15%) and the mixed gas (total flow 6L/min) of oxygen (volumetric concentration is 20.8%) pass through adsorbent bed Layer, at 10 DEG C～30 DEG C, absorption reaches saturated；
(3) molecular sieve after saturated absorption is warmed up to 500 DEG C in WF-01 type integral calculus reactor and carries out desorption and regeneration, In desorption gas, nitrogen dioxide accounts for the 82% of nitric oxide and nitrogen dioxide volume total amount；
(4) being 0.035mol/L in sodium sulfite molar concentration, import nitrogen oxides volumetric concentration is 0.186%, and oxidizability is 80% Left and right, temperature is 10 DEG C, and the time of staying is 0.4s, and liquid-gas ratio is 9.2L/m3Time, flue gas analyzer record final nitrogen oxides The conversion ratio being reduced to nitrogen is 73%.
Embodiment 6
With embodiment 5, liquid-gas ratio is 11.5L/m3, other conditions are constant, record final nitrogen oxides and are reduced to the conversion ratio of nitrogen It is 74%.
Embodiment 7:
(1) H-ZSM-5 molecular sieve being pulverized, sieved, obtaining particle diameter is 12～32 mesh particulate molecular sieve, horse at 500 DEG C Not stove is dried 2h, is then placed in equipped with being cooled to room temperature in the drying basin of silica gel；
(2) take the H-ZSM-5 molecular sieve that 3g silica alumina ratio is 25 and be placed in fixed bed, will (volumetric concentration be containing nitrogen oxides 0.1%～0.15%) and the mixed gas (total flow 6L/min) of oxygen (volumetric concentration is 20.8%) is by adsorbent bed, At 10 DEG C～30 DEG C, absorption reaches saturated；
(3) molecular sieve after saturated absorption is warmed up to 500 DEG C in WF-01 type integral calculus reactor and carries out desorption and regeneration, In desorption gas, nitrogen dioxide accounts for the 80% of nitric oxide and nitrogen dioxide volume total amount；
(4) being 0.0525mol/L in sodium sulfite molar concentration, import nitrogen oxides volumetric concentration is 0.126%, and oxidizability is 80% Left and right, temperature is 7 DEG C, and liquid-gas ratio is 12L/m3, when the time of staying is 0.4s, flue gas analyzer record final nitrogen oxides also Originally be the conversion ratio of nitrogen be 75%.
Embodiment 8
With embodiment 7, the gas time of staying in packed tower is 0.6s, and other conditions are constant, records the reduction of final nitrogen oxides Conversion ratio for nitrogen is 80%.

Claims (10)

1. the method that adsorption and oxidation combines liquid phase scrubbing reduction removing nitrogen oxides, is characterized in that employing includes following step Rapid method:
(1) by the flue gas containing nitrogen oxides by being filled with the fixed bed reactors of molecular sieve, nitrogen oxides part oxygen is made Change and adsorb over a molecular sieve；
(2) stop being passed through flue gas, be passed through nitrogen or air, to mol sieve beds in WF-01 type integral calculus reactor Carry out adding thermal desorption；
(3) gas being desorbed out absorbs with sodium sulfite solution in packed tower and is reduced to nitrogen.
Method the most according to claim 1, it is characterised in that fixed bed reactors used are internal diameter 10～14mm, can Packed height is the quartz glass tube of 16～20cm.
Method the most according to claim 1, it is characterised in that molecular sieve used be silica alumina ratio be 25～500 One in H-ZSM-5 type molecular sieve, particle diameter is 12～32 mesh.
Method the most according to claim 1, it is characterised in that the reaction temperature of activating pretreatment molecular sieve is 500～550 DEG C, the time is 2～3h.
Method the most according to claim 1, it is characterised in that during absorption, flue gas tolerance is 6L/min, nitrogen oxides body Volume concentrations is 0.1%～0.15%.
Method the most according to claim 1, it is characterised in that the adsorptive pressure of nitric oxide adsorption is normal pressure, absorption Temperature is 10 DEG C～30 DEG C.
Method the most according to claim 1, is characterized in that under being passed through nitrogen or air conditions, adsorb saturated after point Son sieve regenerates in 450～550 DEG C in WF-01 type integral calculus reactor.
Method the most according to claim 1, it is characterised in that the molar concentration of sodium sulfite used is 0.03～0.07mol/L, temperature is 6～12 DEG C.
Method the most according to claim 1, is characterized in that when liquid-phase reduction, and the volumetric concentration of nitrogen oxides is 0.07%～0.19%, the time of staying of gas is 0.4～0.7s, and the liquid-gas ratio of packed tower is 9～15L/m3, filler is glass bullet Spring filler.
Method the most according to claim 1, it is characterised in that: the nitrogen oxides being desorbed out is reduced to the conversion of nitrogen Rate >=80%.
CN201610338798.XA 2016-05-20 2016-05-20 Method for reducing and removing nitrogen oxide by adsorption-oxidation and liquid phase absorption Pending CN105854541A (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109966917A (en) * 2019-04-22 2019-07-05 华能国际电力股份有限公司 A kind of electricity-saving type flue gas NO electrocatalytic oxidation system and method
US20210220772A1 (en) * 2019-10-29 2021-07-22 Huaneng Clean Energy Research Institute Flue gas low-temperature adsorption denitrification method
CN114471379A (en) * 2022-02-10 2022-05-13 万华化学集团股份有限公司 Trickle bed reactor with elastic filler and method for preparing 1, 3-cyclohexyldimethylamine by using trickle bed reactor
CN115350562A (en) * 2022-10-20 2022-11-18 格林斯达(北京)环保科技股份有限公司 Method for treating waste gas containing nitrogen oxide

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109966917A (en) * 2019-04-22 2019-07-05 华能国际电力股份有限公司 A kind of electricity-saving type flue gas NO electrocatalytic oxidation system and method
CN109966917B (en) * 2019-04-22 2023-09-26 华能国际电力股份有限公司 Electricity-saving type flue gas NO electrocatalytic oxidation system and method
US20210220772A1 (en) * 2019-10-29 2021-07-22 Huaneng Clean Energy Research Institute Flue gas low-temperature adsorption denitrification method
US11925898B2 (en) * 2019-10-29 2024-03-12 Huaneng Clean Energy Research Institute Flue gas low-temperature adsorption denitrification method
CN114471379A (en) * 2022-02-10 2022-05-13 万华化学集团股份有限公司 Trickle bed reactor with elastic filler and method for preparing 1, 3-cyclohexyldimethylamine by using trickle bed reactor
CN115350562A (en) * 2022-10-20 2022-11-18 格林斯达(北京)环保科技股份有限公司 Method for treating waste gas containing nitrogen oxide

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Application publication date: 20160817