CN111097269A - Method and device for simultaneously removing SOx and NOx in flue gas and producing compound fertilizer - Google Patents
Method and device for simultaneously removing SOx and NOx in flue gas and producing compound fertilizer Download PDFInfo
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- CN111097269A CN111097269A CN201911409763.0A CN201911409763A CN111097269A CN 111097269 A CN111097269 A CN 111097269A CN 201911409763 A CN201911409763 A CN 201911409763A CN 111097269 A CN111097269 A CN 111097269A
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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
- B01D53/60—Simultaneously removing sulfur oxides and nitrogen oxides
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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
- B01D53/77—Liquid phase processes
- B01D53/78—Liquid phase processes with gas-liquid contact
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- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05G—MIXTURES OF FERTILISERS COVERED INDIVIDUALLY BY DIFFERENT SUBCLASSES OF CLASS C05; MIXTURES OF ONE OR MORE FERTILISERS WITH MATERIALS NOT HAVING A SPECIFIC FERTILISING ACTIVITY, e.g. PESTICIDES, SOIL-CONDITIONERS, WETTING AGENTS; FERTILISERS CHARACTERISED BY THEIR FORM
- C05G1/00—Mixtures of fertilisers belonging individually to different subclasses of C05
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2251/00—Reactants
- B01D2251/10—Oxidants
- B01D2251/104—Ozone
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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
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/20—Air quality improvement or preservation, e.g. vehicle emission control or emission reduction by using catalytic converters
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Abstract
The invention relates to a method and a device for simultaneously removing SOx and NOx in flue gas and producing a compound fertilizer. The system has low investment and operation cost, high removal efficiency of SOx and NOx, no secondary pollution and good economic benefit of waste gas treatment, and all removal products are recycled to prepare fertilizer.
Description
Technical Field
The invention belongs to the field of nitrogen and sulfur oxide removal methods and devices, and particularly relates to a method and a device for simultaneously removing SOx and NOx in flue gas and producing a compound fertilizer.
Background
Heating plant, thermal power plant and oil refinerySOx and NOx emitted by the combustion of fossil fuels from stationary and mobile combustion sources, such as transportation vehicles, are major pollutants of the atmosphere. Over the past decades, the power generation of the energy sector has relied heavily on fossil fuels, and the use of fossil fuels will continue to increase in the coming decades. Although natural gas may be a good alternative to fossil fuels, it has long been an important fuel in the future as a cheap and stable fossil fuel due to variable prices. The flue gas of a plant using fossil fuel contains 87% of SOx and 67% of NOx, and is mainly SO2NO and NO2Wherein NO accounts for 90-95% of NOx. These toxic gases pose serious threats to humans and the environment, such as acid rain, photochemical smog, ozone layer destruction, and the resulting human respiratory problems of asthma, bronchitis, emphysema and inflammation, and also form a large amount of aerosol, resulting in hazy weather.
In the past decades, in order to mitigate the effects of these toxic gases on the environment and human health, extensive attention has been paid to the problem of emission of smoke pollutants, and a great deal of research has been conducted. The SOx and NOx treatment methods can be generally classified into a recoverable method and a non-recoverable method according to the manner of subsequent treatment of the absorbent. The recoverable method mainly comprises a wet flue gas desulfurization technology (WFGD), the unrecoverable method mainly comprises a selective catalytic reduction technology (SCR), and the two technologies are the most mature and widely applied. Generally, recyclable processes are preferred over non-recyclable processes from cost and waste disposal considerations.
CN 105233647A discloses a method for desulfurization and denitrification of an ammonium sulfide solution, but the method is easy to generate sublimation and volatilization of sulfur and pollute the environment; there are also documents that use ammonia to absorb tail gas, but ammonia escape easily occurs, and the environment is polluted. The ammonia fertilizer has low value.
Disclosure of Invention
The invention aims to solve the technical problem of providing a method and a device for simultaneously removing SOx and NOx in flue gas and producing a compound fertilizer, solving the problem of secondary pollution and improving the value of absorption liquid.
The invention relates to a method for treating SOx and NOx waste gas, which comprises the following steps:
(1) mixing water, yellow phosphorus and a potassium source to obtain oxidation absorption reaction liquid;
(2) and introducing SOx and/or NOx gas into the oxidation absorption reaction liquid for reaction to remove SOx and NOx and generate the ammonium-phosphorus-potassium fertilizer NPK.
The mass ratio of the water, the yellow phosphorus and the potassium source in the step (1) is 70-95: 1-30: 4-29.
The potassium source in the step (1) is potassium chloride.
And (3) the gas flow rate in the step (2) is 0.3-0.6 ml/min.
The reaction in the step (2) is a stirring reaction, the reaction temperature is 50-60 ℃, and the stirring speed is 1000-1200 rpm.
And (3) carrying out real-time monitoring in the reaction process in the step (2) through an online flue gas analyzer, an online pH monitor and an online temperature monitor.
The SOx and NOx waste gas treatment device comprises an oxidation absorption reactor 6, wherein a heater 8 is arranged outside the oxidation absorption reactor 6, a stirrer 7 is arranged inside the oxidation absorption reactor 6, and an online pH monitor 9, an online temperature monitor 10 and an online flue gas analyzer 13 are arranged inside the oxidation absorption reactor; the bottom of the oxidation absorption reactor 6 is provided with an absorption liquid outlet and is connected with an NPK compound fertilizer production system 14; the oxidation absorption reactor 6 is connected with the gas buffer tank 5; the top of the gas buffer tank 5 is provided with a flue gas inlet and a buffer gas outlet, flue gas enters the gas buffer tank 5 through the flue gas inlet, and the buffer gas outlet is connected with an oxidation absorption reactor 6.
The device is also provided with a demister 11 and a dust remover 12, wherein the demister 11 is connected with the oxidation absorption reactor 6, and the dust remover 12 is connected with an online flue gas analyzer 13.
A waste liquid storage tank 15 and an NPK compound fertilizer storage tank are arranged outside the NPK compound fertilizer production system 14; the gas buffer tank 5 is connected with the gas steel cylinders 1 and 2.
Specifically, an oxidation absorption reaction liquid is injected into an oxidation absorption reactor 6, gas in a gas steel cylinder is introduced into a gas buffer tank 5, fully mixed flue gas is introduced into the oxidation absorption reactor 6, the temperature of the oxidation absorption reaction liquid is adjusted by a heater 8, the pH of the oxidation absorption reaction liquid is monitored by an online pH monitor 9, the temperature is controlled by an online temperature monitor 10, gas escaping from the oxidation absorption reactor is measured by an online flue gas analyzer 13, SOx and NOx in the flue gas are fully oxidized and absorbed in the oxidation absorption reactor to form raw slurry of the NPK compound fertilizer, and then the raw slurry enters an NPK compound fertilizer production system 14.
SOx and NOx are sulfur oxides and nitrogen oxides, respectively.
The system of the invention utilizes yellow phosphorus and potassium chloride to prepare the oxidation absorption liquid, and the yellow phosphorus oxidizes NO into NO2And other high valence NOx. After the oxidation absorption reaction is finished, PO is formed4And P2O5The solid particles contain other elements required by the compound fertilizer in the oxidation absorption liquid.
The main chemical reaction principle of the system is as follows:
(1) the reaction of yellow phosphorus and oxygen generates ozone
P4+O2→P4O+O
P4O+nO2→P4O10+ mO (m means m oxygen atoms)
O+O2→O3
(2) Ozone oxidizes NO to NO2 and other higher-valence NOx
NO+O3→NO2+O2
NO+O→NO2
NO+NO2→N2O3
NO2+NO2→N2O4
NO2+O3→NO3+O2
NO+NO3→2NO2
NO2+NO3→N2O5
(3) NO2 and other higher NOx are absorbed by water to form nitric and nitrous acids
2NO2+H2O→HNO3+HNO2
N2O3+H2O→2HNO2
N2O4+H2O→HNO3+HNO2
N2O5+H2O→2HNO3
2HNO2+O2→2HNO3
(4) The main reaction of potassium chloride with nitric acid and sulfuric acid
KCL+HNO3→KNO3+HCL
KCL+H2SO4→K2SO4+2HCL
Description of the main reactions: p4 and O2The reaction of (3) can take place either in the liquid phase or in the gas phase. The reaction in the liquid phase is affected by parameters such as liquid to gas ratio, reactor design, temperature, and all that may alter the dispersion of dissolved phosphorus. In addition, all additives which may alter the dielectric constant of the medium may also have an effect. And for reactions in the gas phase, O2Is reacted with P4 released from the emulsion at elevated temperature. Under the thermal equilibrium conditions of 1atm of pressure and 55℃ of temperature, P4The concentration is close to 420ppm, so the P of the WFGD unit4The emulsion temperature and concentration were the same as those of NO (500ppm) in the flue gas. P4And O2To O3The reaction rate of the oxygen atom and the oxygen atom is almost equal, and the oxygen atom in the smoke is usually the2Higher, so this is the predominant reaction after addition of yellow phosphorus. O is3The main reaction with NO is the formation of the more soluble NO2But will be subjected to oxygen atoms O or O3Influence of, NO produced2Reaction with NO to form N2O3Or dimerized to N2O4。NO2And other intermediates can be reacted directly with water to form nitrous acid andnitric acid. Finally, for denitration alone, KCl will form KNO with nitric acid3For desulfurization and denitrification, KCl can generate KNO with nitric acid and sulfuric acid3And K2SO4. KNO3 is a source of potassium in fertilizer, including 44% K2O and 36.5% potassium, such as with KNO3And K2SO4The fertilizer contains 50-52% of K2O and 41.5-43.2% K.
The invention utilizes yellow phosphorus and KCl to prepare oxidation absorption reaction liquid and inject the oxidation absorption reaction liquid into an oxidation absorption reactor. Introducing the flue gas into a gas mixing tank, and introducing the fully mixed flue gas into an oxidation absorption reactor. The temperature of the oxidation absorption reaction liquid is adjusted by a heater, the temperature is controlled and monitored by an online temperature monitor, and the pH of the oxidation absorption reaction liquid is monitored by an online pH monitor. Thereby controlling the temperature and pH of the oxidation absorption reaction solution. SOx and NOx in the flue gas are fully oxidized and absorbed in the oxidation absorption reactor to form raw slurry of the NPK compound fertilizer. The gas escaping from the oxidation absorption reactor is measured by an on-line flue gas analyzer. The contents of the NPK raw slurry were measured by ion chromatography, and it was confirmed that all the contents of the NPK compound fertilizer were contained.
Advantageous effects
(1) The method utilizes the yellow phosphorus to produce O3As a high-efficiency oxidant, the cost is low, and other oxidant sources are not needed.
(2) High removal efficiency was obtained, with SOx removal efficiency of 100% and NOx removal efficiency exceeding 90%.
(3) Because large-scale energy consumption equipment is not needed, the method has low energy consumption.
(4) The final solid precipitate is easily separated by filtration, which is a rich source of phosphorus compounds.
(5) The final absorption solution is a valuable byproduct of the NPK fertilizer.
(6) The chemical reagent used is low in price, and the removal effect is good, so that the desulfurization and denitrification technology is high in cost benefit.
(7) Simple process and equipment and easy operation.
Drawings
FIG. 1 is a schematic diagram of a system for simultaneously removing SOx and NOx from flue gas and producing a nitrogen phosphorus potassium (NPK) compound fertilizer in accordance with the present invention; 1SO2 steel cylinder; 2NO steel cylinder; 3, a flow meter; 4, a flow meter; 5, a gas buffer tank; 6 oxidizing and absorbing reactor; 7, a stirrer; 8, a heater; 9 an online pH monitor; 10 an online temperature monitor; 11 a demister; 12 a dust remover; 13 an on-line flue gas analyzer; 14NPK compound fertilizer production equipment; 15 a waste liquid storage tank; 16; NPK compound fertilizer storage tank.
Detailed Description
The invention will be further illustrated with reference to the following specific examples. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention. Further, it should be understood that various changes or modifications of the present invention may be made by those skilled in the art after reading the teaching of the present invention, and such equivalents may fall within the scope of the present invention as defined in the appended claims.
Example 1
The device of the invention is as follows: the device comprises an oxidation absorption reactor 6, wherein a heater 8 is arranged outside the oxidation absorption reactor 6, a stirrer 7 is arranged inside the oxidation absorption reactor 6, and an online pH monitor 9, an online temperature monitor 10 and an online flue gas analyzer 13 are arranged; the bottom of the oxidation absorption reactor 6 is provided with an absorption liquid outlet and is connected with an NPK compound fertilizer production system 14; the oxidation absorption reactor 6 is connected with the gas buffer tank 5; the top of the gas buffer tank 5 is provided with a flue gas inlet and a buffer gas outlet, flue gas enters the gas buffer tank 5 through the flue gas inlet, and the buffer gas outlet is connected with an oxidation absorption reactor 6.
In the specific reaction process: the prepared oxidation absorption reaction liquid is injected into an oxidation absorption reactor 6, gas in a gas steel cylinder is introduced into a gas buffer tank 5, fully mixed flue gas is introduced into the oxidation absorption reactor 6, the temperature of the oxidation absorption reaction liquid is adjusted by a heater 8, the pH of the oxidation absorption reaction liquid is monitored by an online pH monitor 9, the temperature is controlled by an online temperature monitor 10, gas escaping from the oxidation absorption reactor is measured by an online flue gas analyzer 13, SOx and NOx in the flue gas are oxidized by ozone generated by the reaction of P4 and oxygen in the oxidation absorption reactor and are absorbed by water to generate phosphate, sulfate and nitrate, and further raw slurry (liquid fertilizer) of the NPK compound fertilizer is formed, and then the raw slurry enters an NPK compound fertilizer evaporation and crystallization production system 14 to generate solid compound fertilizer.
Example 2
(1) Preparing 1L of fresh deionized water, injecting the deionized water into a 1L Brinell flask, adding 95 percent, 1 percent and 4 percent of water, yellow phosphorus and potassium source KCL by mass percent respectively to prepare oxidation absorption reaction liquid, and arranging a pH meter and a thermometer in the flask and sealing the flask. The temperature of the emulsion was controlled at 55 ℃ and the stirring speed of the stirrer was 1083 rpm, and the gas entering the flask and the gas escaping after the reaction were measured by a smoke analyzer.
(2) The flow rate of gas into the flask was controlled to be 0.3 to 0.6 ml/min and the NO concentration was 500 ppm.
In the present embodiment, the NOx removal rate is greater than 90%. The final reaction product is the main component of the NPK compound fertilizer (potassium sulfate, potassium nitrate and potassium chloride in the mass ratio of 1: 1: 4) determined by an ion chromatograph, a Raman spectrometer (RAMAN) and an X-ray diffraction analyzer (XRD).
Example 3
(1) Preparing 1L of fresh deionized water, injecting into 1L of Buchner flask, adding water, yellow phosphorus, and KCO as potassium source3The contents of the reaction solution were 70%, 10% and 20% by mass, respectively, to prepare an oxidation absorption reaction solution, and a pH meter and a thermometer were installed in the flask and sealed. The temperature of the emulsion was controlled at 55 ℃ and the stirring speed of the stirrer was 1083 rpm, and the gas entering the flask and the gas escaping after the reaction were measured by a smoke analyzer.
(2) The flow rate of gas into the flask was controlled to be 0.3 to 0.6 ml/min, the concentration of NO was 500ppm, and SO was added2The concentration was 2700 ppm.
In this example, the NOx removal rate was higher than 90%, SO2The removal rate of (2) was 100%. The final reaction product is the main component of the NPK compound fertilizer (the mass ratio of potassium sulfate, potassium nitrate and potassium chloride is 1: 1: 20) through the measurement of an ion chromatograph, a Raman spectrometer (RAMAN) and an X-ray diffraction analyzer (XRD).
Claims (10)
1. A method of treating an SOx, NOx exhaust gas comprising:
(1) mixing water, yellow phosphorus and a potassium source to obtain oxidation absorption reaction liquid;
(2) and introducing SOx and/or NOx gas into the oxidation absorption reaction liquid for reaction to remove SOx and NOx and generate the ammonium-phosphorus-potassium fertilizer NPK.
2. The method according to claim 1, wherein the mass ratio of the water, the yellow phosphorus and the potassium source in the step (1) is 70-95: 1-30: 4-29.
3. The method of claim 1, wherein the potassium source in step (1) is one or more of potassium chloride, potassium carbonate, potassium sulfate, potassium hydroxide, and potassium fertilizers containing the potassium chloride, the potassium carbonate, the potassium sulfate, the potassium hydroxide and the potassium fertilizers.
4. The method as claimed in claim 1, wherein the gas flow rate in step (2) is 0.3-0.6 ml/min.
5. The method as claimed in claim 1, wherein the reaction in step (2) is a stirring reaction, the reaction temperature is 50-60 ℃, and the stirring rate is 1000-1200 rpm.
6. The method of claim 1, wherein the reaction process in step (2) is monitored in real time by an online flue gas analyzer, an online pH monitor and an online temperature monitor.
7. The device for treating the SOx and NOx waste gas is characterized by comprising an oxidation absorption reactor (6), wherein a heater (8) is arranged outside the oxidation absorption reactor (6), a stirrer (7) is arranged inside the oxidation absorption reactor, and an online pH monitor (9), an online temperature monitor (10) and an online flue gas analyzer (13) are arranged inside the oxidation absorption reactor; the bottom of the oxidation absorption reactor (6) is provided with an absorption liquid outlet and is connected with an NPK compound fertilizer production system (14); the oxidation absorption reactor (6) is connected with the gas buffer tank (5); the top of the gas buffer tank (5) is provided with a flue gas inlet and a buffer gas outlet, the flue gas enters the gas buffer tank (5) through the flue gas inlet, and the buffer gas outlet is connected with an oxidation absorption reactor (6).
8. The apparatus according to claim 7, wherein the apparatus is further provided with a demister (11) and a dust collector (12), wherein the demister (11) is connected to the oxidation absorption reactor (6), and the dust collector (12) is connected to the on-line flue gas analyzer (13).
9. The apparatus of claim 7, wherein the NPK compound fertilizer production system (14) is externally provided with a waste liquid storage tank (15) and an NPK compound fertilizer storage tank; the gas buffer tank (5) is connected with the gas steel cylinders (1) and (2).
10. The apparatus according to claim 7, wherein the oxidizing absorption reaction solution is injected into the oxidizing absorption reactor (6), the gas in the gas cylinder is introduced into the gas buffer tank (5), the well-mixed flue gas is introduced into the oxidizing absorption reactor (6), the temperature of the oxidizing absorption reaction solution is adjusted by the heater (8), the pH of the oxidizing absorption reaction solution is monitored by the online pH monitor (9), the temperature is controlled by the online temperature monitor (10), the gas escaping from the oxidizing absorption reactor is measured by the online flue gas analyzer (13), SOx and NOx in the flue gas are fully oxidized and absorbed in the oxidizing absorption reactor to form the raw slurry of the NPK compound fertilizer, and then the raw slurry enters the NPK compound fertilizer production system (14).
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116510497A (en) * | 2023-06-26 | 2023-08-01 | 昆明理工大学 | Method and system for removing sulfur, phosphorus and nitrogen oxides in yellow phosphorus tail gas boiler by using phosphorus ore powder |
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| CN101307289A (en) * | 2008-02-14 | 2008-11-19 | 朱洪 | Biological culturing method and device for reducing discharge of waste gases |
| CN102247750A (en) * | 2011-07-11 | 2011-11-23 | 华东理工大学 | Device and method for simultaneously desulfurizing and denitrifying flue gas by ozone catalytic oxidation process |
| CN105236551A (en) * | 2015-09-30 | 2016-01-13 | 山东大学 | Soil fast-filter bed system for purifying bioreactor tail gas |
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Patent Citations (3)
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| CN101307289A (en) * | 2008-02-14 | 2008-11-19 | 朱洪 | Biological culturing method and device for reducing discharge of waste gases |
| CN102247750A (en) * | 2011-07-11 | 2011-11-23 | 华东理工大学 | Device and method for simultaneously desulfurizing and denitrifying flue gas by ozone catalytic oxidation process |
| CN105236551A (en) * | 2015-09-30 | 2016-01-13 | 山东大学 | Soil fast-filter bed system for purifying bioreactor tail gas |
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| Title |
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| 杨加强: "黄磷复合矿浆脱除烟气NOx的研究", 《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》 * |
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| CN116510497A (en) * | 2023-06-26 | 2023-08-01 | 昆明理工大学 | Method and system for removing sulfur, phosphorus and nitrogen oxides in yellow phosphorus tail gas boiler by using phosphorus ore powder |
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