CN114262041A - Supercritical water oxidation tail gas recovery method and system - Google Patents
Supercritical water oxidation tail gas recovery method and system Download PDFInfo
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Abstract
The invention discloses a supercritical water oxidation tail gas recovery method, which is characterized in that non-oxygen impurity gases in tail gas are removed by adopting technologies such as pressure swing adsorption and the like to realize oxygen concentration or purification, so that recovery of excessive oxygen in supercritical water oxidation is realized, and reaction heat and a byproduct carbon dioxide product are recovered at the same time. Compared with the prior art, the oxygen is directly discharged after being recycled, so that the operating cost of the supercritical water oxidation technology is high, and carbon emission is increased due to carbon dioxide discharge, therefore, the recycling of the oxygen and the reaction heat greatly reduces the operating cost, and the recycling of the carbon dioxide greatly reduces the carbon emission.
Description
Technical Field
The invention belongs to the technical field of supercritical water oxidation treatment of sewage containing organic solid waste, organic hazardous waste, radioactive organic waste and the like, and particularly relates to an oxygen recovery system after supercritical water oxidation reaction, which is used for greatly reducing the operating cost of supercritical water oxidation so as to realize energy conservation and consumption reduction of the whole device.
Background
The supercritical water oxidation technology is widely applied to industries such as nuclear power, military industry, chemical industry, petroleum, municipal industry, pharmacy, food and the like, and is used for treating toxic, harmful and difficultly-degradable organic wastes (particularly dangerous wastes and solid wastes). The supercritical water oxidation technology for treating organic waste has the technical characteristics of high oxidation efficiency and high reaction speed, and almost completely mineralizes organic matters, so that hazardous waste, solid waste and other organic wastes are subjected to harmless treatment.
The supercritical water oxidation process has high operation cost, mainly has high raw material consumption cost caused by oxygen consumption, and most of students have paid high attention to supercritical physical properties, materials and the like of the supercritical water oxidation, but have paid little attention to an exhaust gas recovery system. With the development of new materials and supercritical technologies, the self excellent characteristics of the rapid and complete oxidation reaction of supercritical water oxidation are more and more shown, and the industrial demonstration application of the technology is generated, so that a tail gas recovery system has to be considered to reduce the operation cost, and conditions are created for the economic feasibility of the technology. The novel process for recovering the supercritical water oxidation tail gas aims to improve the economy of the supercritical water oxidation technology.
Disclosure of Invention
The invention aims at the reaction tail gas (mainly CO) of the existing supercritical water oxidation technology2、H2O and excess O2Etc.), the oxygen is concentrated or purified for recovery, and the reaction heat is recovered to achieve system energy saving. In the supercritical water oxidation process, nonmetallic elements such as S and P possibly contained in the sewage are generally oxidized into SO4 2-And PO4 3-Etc. (S in the course of supercritical water oxidation reactionX-+O2→SO4 2-；Py-+O2→PO4 3-) The waste water contains a small amount of N element, and a small amount of N is generated by oxidation2The tail gas treatment is to recover excessive oxygen and remove other impurity gases, mainly to remove a large amount of CO2(Prior Art TailThe gas is not treated, so the energy consumption is high and the CO is removed2Other impurities such as P and S are removed in the salt elimination, and the tail gas does not contain O2The valuable recovery is possible, the radioactive elements are filtered and then emptied), the pressure swing adsorption technology (PSA) is adopted to adsorb the carbon dioxide gas, the basic working principle of the pressure swing adsorption is to utilize the adsorption agent to have different adsorption capacities, adsorption speeds and adsorption forces to the adsorbate under different partial pressures, and to have the characteristic of selective adsorption to each component of the separated gas mixture under certain pressure (to adsorb H in turn)2O (steam), CO2、CO、CH4、O2、N2And H2) Removing impurity components (except for O) from raw material gas by pressure adsorption2Except for impurities), the adsorbent is regenerated by desorbing the impurities under reduced pressure. Therefore, the purpose of continuously separating the gas mixture can be achieved by using a plurality of adsorption beds and cyclically changing the pressure of each combined adsorption bed. These gas components (in turn H)2O (steam), CO2、CO、CH4、O2、N2And H2) The adsorption capacity and adsorption capacity on the physical adsorbent are sequentially weakened and reduced under certain temperature and pressure. When the shift gas passes through the adsorbent bed, the preceding component is preferentially adsorbed and displaced by the adsorbent even though the latter component has been adsorbed by the former component (the order of adsorption being H in turn)2O (steam), CO2、CO、CH4、O2、N2And H2). Hardly adsorbable component CH4、O2、N2And H2The gas is less adsorbed and discharged from the outlet end of the adsorption tower as a gas from which carbon dioxide is removed. When the pressure of the adsorption bed is reduced, the adsorbed gas such as carbon dioxide is desorbed, and the adsorbent is regenerated. The supercritical water oxidation tail gas is mainly H2O (gas), CO2、O2(50-80%) and N2(small amount), etc., and high concentration O can be obtained on the high pressure side after pressure swing adsorption2(more than 95%) and N2Desorption of gas CO2Can be recovered as a by-product, and the present invention can recover the excess O not participating in the reaction2Thereby supercritical water can be mixedIn oxidation reaction O2The consumption is reduced, the total cost consumed by the device is saved by about 15%, meanwhile, the benefit of the recovery of the purified carbon dioxide accounts for about 5-10% of the operation cost, the cost can be saved by more than 20% in total, and the energy conservation and consumption reduction are greatly realized.
The supercritical water oxidation reactor is designed to have the pressure of 26-35 MPa (G) and the temperature of 450-700 ℃, and is provided with an organic sewage inlet reaching a certain temperature (300-450 ℃) and pressure (26-35 MPa (G)), an oxygen inlet reaching a certain pressure (26-35 MPa (G)), a vapor phase outlet, a salt discharge port and an emergency discharge port after supercritical water oxidation. Supercritical water, oxygen and organic sewage which reach certain temperature (above 500 ℃) and pressure (26-35 MPa (G)) are reacted in a reactor in a homogeneous way, organic matters can be almost completely decomposed within 4-30 s, and water, carbon dioxide and a very small amount of N are generated2(determined by the nitrogen content of the raw material), salts (organic non-hydrocarbon impurities), and the like. The supercritical water oxidation reactor is provided with an emergency discharge pipeline for overtemperature (temperature high alarm) and overpressure (pressure high alarm), and when the reactor is over-temperature and overpressure, the temperature and the pressure are reduced and released through the emergency discharge pipeline, and organic waste is collected and recycled to be subjected to supercritical water oxidation reaction again. And a vapor phase removing treatment system after reaction.
Based on the operation steps of the supercritical water oxidation tail gas recovery system for sewage such as organic solid waste, organic hazardous waste, radioactive organic waste and the like, the method comprises the following steps:
step a: starting the supercritical water oxidation reactor, and conveying the organic sewage and oxygen which reach the reaction condition to the supercritical water oxidation reactor;
step b: the reaction vapor phase flows out of the supercritical water oxidation reactor and exchanges heat with the organic sewage coil heat exchanger through the reaction vapor phase to recover heat of the reaction vapor phase;
step c: further recovering waste heat of the high-pressure reaction vapor phase at about 200 ℃ by using a steam drum;
step d: reducing the pressure of a reaction vapor phase with high-pressure reaction and proper temperature to the operating pressure (about 2.0MPa (G)) of a PSA tower by using a backpressure valve, entering the PSA tower for adsorption, purifying gas to a subsequent system, removing desorbed gas to a carbon dioxide recovery system, and producing a byproduct, namely carbon dioxide for delivery;
step e: the purified gas is pressurized to 26-30 MPa (G) by a booster and enters a reaction system for recycling.
And d, controlling by two or more PSA towers and a programmable valve to realize frequent automatic switching operation and complete the repeated cycle of adsorption-desorption-reabsorption so as to realize continuous adsorption of tail gas and continuous discharge of purified gas, namely: one column (such as a PSA-1 column) is in an adsorption process, a PSA-2 column or a PSA-3 column is in a desorption or desorption completion waiting state, when the adsorption of the PSA-1 column is saturated, the operation is switched to the adsorption of the PSA-2 column, the desorption of the PSA-1 column, the adsorption of the PSA-2 column, the adsorption of the PSA-3 column, the desorption of the PSA-2 column, the adsorption of the PSA-3 column is saturated, the adsorption of the PSA-1 column after the desorption is completed continues, and the desorption of the PSA-3 column is the operation example of a three-column cycle.
Compared with the prior art, the invention has the beneficial effects that:
(1) the tail gas recovery system mainly recovers oxygen, so that the oxygen consumption is greatly reduced, the oxygen consumption cost of the system without tail gas recovery accounts for about 50% of the total operation cost, and the oxygen consumption cost after tail gas recovery accounts for about 35% of the total operation cost, so that the operation cost is greatly reduced;
(2) by-product CO2Not only improves the economic benefit of the device, but also reduces CO2The discharge plays an important role in environmental protection of the device and resource utilization of pollutants. By-product CO2The recovery and increase benefit of the method accounts for about 5-10% of the operation cost;
(3) PSA pressure swing adsorption Process, O2The purified gas is medium pressure, compared with other decarburization technologies, the method is low pressure operation, and a subsequent reaction system O2Is high pressure, the PSA pressure swing adsorption process is more suitable for recovering oxygen in supercritical water oxidation tail gas and is more beneficial to O2Energy-saving recovery;
(4) for supercritical water oxidation of radioactive materials, O with low radioactive dose is added2The waste water is recycled and reused, but not discharged into the atmosphere, so that the environment is protected;
(5) the coil pipe type heat exchanger and the steam drum for reacting the vapor phase and the raw material organic sewage are used for recovering the waste heat of the high-temperature high-pressure reaction vapor phase discharged from the supercritical water oxidation reactor, thereby being beneficial to reducing the energy consumption of the device.
Description of the drawings:
FIG. 1 is a flow chart of a supercritical water oxidation tail gas recovery process provided by the implementation of the invention;
wherein, 1-supercritical water oxidation reactor, 11-organic sewage inlet, 12-oxygen inlet, 13-emergency discharge outlet, 14-vapor phase outlet after reaction, and 15-salt outlet after reaction; 2-reaction vapor phase-organic sewage raw material heat exchanger, 21-reaction vapor phase inlet, 22-reaction vapor phase outlet, 23-organic sewage inlet; 24-an organic sewage outlet; 3 a-a shell and tube heat exchanger of a steam drum, 3 b-a steam generator of the steam drum, 31-a reaction vapor phase inlet, 32-a vapor-liquid mixed outlet, 33-a boiler water inlet and 34-a low-pressure steam outlet; 4-a gas-liquid separator, 41-a gas-liquid mixing inlet, 42-a gas phase outlet and 43-a pure water outlet; 5-PSA-1 column, 51 a-vapor phase inlet, 52 a-purified gas outlet, 53 a-desorbed gas outlet; 6-PSA-2 column, 61 a-vapor phase inlet, 62 a-purified gas outlet, 63 a-stripping gas outlet; 7-gas booster, 71-gas inlet, 72-gas outlet.
The specific implementation mode is as follows:
the present invention will be described in more detail with reference to the accompanying drawings and embodiments.
Example 1
FIG. 1 is a flow chart of a process for recovering supercritical water oxidation treatment tail gas of sewage such as organic solid waste, organic hazardous waste, radioactive organic waste and the like, wherein a supercritical water oxidation treatment tail gas system comprises a supercritical water oxidation reactor 1, a reaction vapor phase-organic sewage raw material heat exchanger 2, a steam drum 3, a vapor-liquid separator 4, a PSA-1 tower 5, a PSA-2 tower 6, a gas booster 7, and pipelines and valves belonging to the gas booster 7.
The supercritical water oxidation reactor 1 is respectively provided with an organic sewage inlet 11, an oxygen inlet 12, a vapor phase outlet 14 after reaction, a salt discharge outlet 15 after reaction and an emergency discharge outlet 13 with over-temperature and over-pressure; the organic sewage reaching the supercritical condition enters the reactor through the organic sewage inlet 11, and is subjected to a homogeneous, rapid and complete oxidation reaction in the reactor 1 with the oxygen entering through the oxygen inlet 12 to generate supercritical water, salt, carbon dioxide and the like. Among the products of the supercritical water oxidation reaction, vapor phase (gas such as gaseous water and carbon dioxide) is discharged out of the reactor 1 through a vapor phase outlet 14, salt is discharged out of the reactor 1 through a salt discharge outlet 15, and an emergency discharge outlet 13 is used for realizing pressure relief and temperature reduction of a reaction system.
A reaction vapor phase-organic sewage raw material heat exchanger 2, the heat exchanger 2 is arranged for recovering the heat of the high-temperature reaction vapor phase as the primary heating of the raw material organic sewage so as to reduce the load of the secondary electric heating of the raw material sewage as much as possible. Raw materials feeding heater need heat to supercritical temperature among the supercritical water oxidation unit, adopts the one-level heating to utilize the high temperature material after the reaction as the one-level heating heat source of raw materials organic sewage and carries out the one-level heating to be furnished with second grade electric heater in order to realize that raw materials organic sewage feeding temperature reaches supercritical temperature, the one-level heater is exactly heat exchanger 2, thereby realizes the energy-conserving first step of device.
In the embodiment, the reaction vapor phase-organic sewage raw material heat exchanger 2 adopts a coil type heat exchanger, so that the heat exchange area is large, the occupied area is small, and meanwhile, the structure of the device is easy to eliminate the thermal stress generated by high temperature. The reaction vapor phase-organic sewage raw material heat exchanger 2 is provided with a reaction vapor phase inlet 21, a reaction vapor phase outlet 22, a jacket organic sewage inlet 23 and a jacket organic sewage outlet 24. The high-pressure high-temperature reaction vapor phase transmitted from the vapor phase outlet 14 after the reaction enters a reaction vapor phase inlet 21, a coil of a coil heat exchanger is arranged, the high-pressure low-temperature organic sewage enters a jacket from a jacket organic sewage inlet 23, primary heat exchange is carried out on the high-pressure high-temperature reaction vapor phase in the jacket, and then the high-pressure high-temperature reaction vapor phase is discharged from a jacket organic sewage outlet 24 (only heat exchange is carried out in the jacket).
The outlet of the vapor phase treatment system (namely the reaction vapor phase outlet 22 of the reaction vapor phase-organic sewage heat exchanger 2) is connected with a steam drum 3 to further recover the reaction vapor phase waste heat, and the low-level energy recovery is realized by adopting the steam drum to produce low-pressure exhaust steam because the temperature is about 200 ℃ after the heat exchange is carried out by the reaction vapor phase-organic sewage heat exchanger 2. The steam drum is combined by a tube type heat exchanger 3a and a steam generator 3b (the lower part of the steam drum 3 is the tube type heat exchanger 3a, the upper part is the steam generator 3b), a reaction vapor phase passes through a tube side of the tube type heat exchanger, and boiler water passes through a shell side of the tube type heat exchanger. The steam drum 3 is provided with a reaction vapor phase inlet 31, a gas-liquid mixture outlet 32, a boiler water inlet 33 and a low-pressure steam outlet 34. The high-pressure gas pressure is reduced to be slightly higher than the PSA adsorption pressure through the gas backpressure valve I, the obtained gas-liquid mixed solution enters the gas-liquid separator 4 for separation, the gas-liquid separator 4 is provided with a gas-liquid mixed solution inlet 41, a gas phase outlet 42 and a pure water outlet 43, and pure water is conveyed to a pure water membrane filtration system through a pump.
The embodiment is provided with two pressure swing adsorption towers, namely a PSA-1 tower 5 and a PSA-2 tower 6, and is provided with a program control valve to realize automatic frequent switching and continuous operation of adsorption-desorption-adsorption-desorption of the two towers so as to ensure that the tail gas treatment system safely and stably continuously operates, and the gas is sequentially H2O (steam), CO2、CO、CH4、O2、N2And H2The adsorption capacity and adsorption capacity on the physical adsorbent are reduced and decreased in turn at a certain temperature and pressure, and O2As poorly adsorbed gas, is present in the purge gas, thus at medium pressure, followed by O2The reaction under high pressure is more beneficial to energy-saving recovery.
After opening the valve IIa and IIIa of the vapor phase inlet line 51a, the vapor phase with proper temperature and pressure from the gas-liquid separator 4 enters the PSA-1 tower 5 through the vapor phase outlet 42 to start adsorption, after the PSA-1 tower 5 is saturated in adsorption, the vapor phase inlet valve IIb and the vapor phase outlet valve IIIb of the PSA-2 tower 6 are opened first, then the valve IIIa and the valve IIa are closed, the valves on the vapor phase inlet line of the PSA tower are seamlessly switched and butted to realize continuous operation, at this time, the desorption gas valve IVa of the PSA-1 tower 5 is opened to start desorption, and the adsorbed vapor and CO are desorbed2Gas desorption to CO2Recovery system makes the dry ice as the byproduct, and two at least towers of PSA system are in order to realize continuous steady operation, and according to desorption time and absorption time difference, set up two above PSA towers, because PSA tower pressurizing and pressure release frequency are higher, this PSA tower belongs to tired equipment, and the many towers of PSA can realize full process automation through the program-controlled valve. The pressure of the purified gas after being pressurized by the compressor 7 reaches 26-30 MPa (G), and the purified gas enters the reactor through the reactor oxygen pipeline 12.
Based on the operation steps of the supercritical water oxidation tail gas recovery system for sewage such as organic solid waste, organic hazardous waste, radioactive organic waste and the like, the method comprises the following steps:
step (1): starting the supercritical water oxidation reactor, and conveying the organic sewage and oxygen which reach the reaction condition to the supercritical water oxidation reactor 1;
step (2): the reaction vapor phase flows out of the supercritical water oxidation reactor and exchanges heat with the organic sewage raw material heat exchanger 2 to recover the heat of the reaction vapor phase;
and (3): the high-pressure reaction vapor phase at about 200 ℃ is further recycled by adopting a steam drum 3;
and (4): reducing the pressure of a reaction vapor phase with high-pressure reaction and proper temperature to the operating pressure (about 2.0MPa (G)) of a PSA tower by using a backpressure valve, entering the PSA tower for adsorption, purifying gas to a subsequent system, removing desorbed gas to a carbon dioxide recovery system, and producing a byproduct, namely carbon dioxide for delivery;
and (5): the purified gas is pressurized to 26-30 MPa (G) by a booster and enters a reaction system for recycling.
And (4) controlling by adopting two or more PSA towers and a programmable valve to realize frequent automatic switching operation, and completing the repeated cycle of adsorption-desorption-reabsorption so as to realize continuous adsorption of tail gas and continuous discharge of purified gas, namely: one column (such as a PSA-1 column) is in an adsorption process, a PSA-2 column or a PSA-3 column is in a desorption or desorption completion waiting state, when the adsorption of the PSA-1 column is saturated, the operation is switched to the adsorption of the PSA-2 column, the desorption of the PSA-1 column, the adsorption of the PSA-2 column, the adsorption of the PSA-3 column, the desorption of the PSA-2 column, the adsorption of the PSA-3 column is saturated, the adsorption of the PSA-1 column after the desorption is completed continues, and the desorption of the PSA-3 column is the operation example of a three-column cycle.
The foregoing is considered as illustrative of the preferred embodiments of the invention and is not to be construed as limiting the invention in any way. Although the present invention has been described with reference to the preferred embodiments, it is not intended to be limited thereto. Therefore, any simple modification, equivalent change and modification made to the above embodiments according to the technical spirit of the present invention should fall within the protection scope of the technical scheme of the present invention, unless the technical spirit of the present invention departs from the content of the technical scheme of the present invention.
Claims (10)
1. A supercritical water oxidation tail gas recovery method, which is characterized in that,
step a: conveying supercritical organic sewage and oxygen into a supercritical water oxidation reactor, completely oxidizing the organic sewage in the reactor to generate water, carbon dioxide and salt, and discharging the salt;
step b: the high-temperature high-pressure reaction vapor phase obtained in the step a) flows into a reaction vapor phase-organic sewage raw material heat exchanger (2) to recover heat, and a high-pressure reaction vapor phase is obtained;
step c: exchanging heat between the high-pressure reaction steam phase obtained in the step b) and boiler water to obtain a gas-liquid mixture, depressurizing the gas-liquid mixture, performing gas-liquid separation, and filtering and recovering the obtained pure water;
step d: adsorbing the gas phase obtained after gas-liquid separation in the step c), and desorbing to obtain CO2Recovering, pressurizing other purified gas, and feeding into the reaction system for reuse.
2. The supercritical water oxidation tail gas recovery method of claim 1, wherein step d employs two or more PSA towers and a programmable valve control to realize frequent automatic switching operation, and complete repeated cycle of adsorption-desorption-re-adsorption-re-desorption to realize continuous adsorption of tail gas and continuous discharge of purified gas.
3. The supercritical water oxidation tail gas recovery method according to claim 1, wherein step d) is specifically: and c), reducing the pressure of the reaction vapor phase obtained in the step c) to the operating pressure of the PSA tower by using a backpressure valve, entering the PSA tower for adsorption, purifying the gas to a subsequent system, removing the desorbed gas to a carbon dioxide recovery system, and producing a byproduct, namely carbon dioxide, to leave a factory.
4. The supercritical water oxidation tail gas recovery method according to claim 1, characterized in that in step d), the pressure is increased to 26-30 MPa.
5. The system for recovering the supercritical water oxidation tail gas according to the claim 1 to 4 is characterized by comprising a supercritical water oxidation reactor (1), a reaction vapor phase-organic sewage raw material heat exchanger (2), a steam drum (3), a vapor-liquid separator (4), a PSA-1 tower (5), a PSA-2 tower (6), a gas booster (7) and necessary pipelines and valves thereof which are connected in sequence.
6. The supercritical water oxidation tail gas recovery system according to claim 5, wherein the supercritical water oxidation reactor (1) is provided with an organic sewage inlet (11), an oxygen inlet (12), a vapor phase outlet (14) after reaction and a salt discharge outlet (15) after reaction, respectively; organic sewage reaching the supercritical condition enters the reactor through the organic sewage inlet (11), and is subjected to homogeneous, rapid and complete oxidation reaction in the reactor (1) together with oxygen entering through the oxygen inlet (12), the generated vapor phase is discharged out of the supercritical water oxidation reactor (1) through the vapor phase outlet (14), and salt is discharged out of the supercritical water oxidation reactor (1) through the salt discharge outlet (15).
7. The supercritical water oxidation tail gas recovery system according to claim 6, characterized in that the supercritical water oxidation reactor (1) is further provided with an emergency discharge port (13) with super-temperature and super-pressure, and the emergency discharge port (13) is used for realizing pressure relief and temperature reduction of the reaction system.
8. The supercritical water oxidation tail gas recovery system according to claim 5, wherein the reaction vapor phase-organic wastewater raw material heat exchanger (2) is a coil heat exchanger provided with a reaction vapor phase inlet (21), a reaction vapor phase outlet (22), a jacket organic wastewater inlet (23) and a jacket organic wastewater outlet (24), the high temperature reaction vapor phase enters the reaction vapor phase-organic wastewater raw material heat exchanger (2) from the reaction vapor phase inlet (21) and flows out from the reaction vapor phase outlet (22), the raw wastewater as the supercritical water oxidation reaction flows in from the jacket organic wastewater inlet (23) and flows out from the jacket organic wastewater outlet (24), and the heat of the high temperature reaction vapor phase serves as the primary heating of the raw organic wastewater.
9. The supercritical water oxidation tail gas recovery system of claim 5, wherein the steam drum (3) is provided with a reaction vapor phase inlet (31), a gas-liquid mixing outlet (32), a boiler water inlet (33) and a low-pressure steam outlet (34), boiler water flows into the shell side of the steam drum (3) through the boiler water inlet (33), and reaction vapor phase flows out from the gas-liquid mixing outlet (32) after heat exchange is carried out in the steam drum (3).
10. The supercritical water oxidation tail gas recovery system according to claim 5, wherein the gas-liquid mixture flowing out of the gas-liquid mixing outlet (32) is subjected to gas-liquid separation by a gas-liquid separator (4).
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| CN111234879A (en) * | 2020-03-11 | 2020-06-05 | 西安交通大学 | Supercritical water gasification hydrogen production and slurry supercritical water heat combustion coupling system and process |
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| WO2012177907A1 (en) * | 2011-06-22 | 2012-12-27 | Praxair Technology, Inc. | System and method for oxygen supply for wastewater treatment plant having biological treatment system and supercritical water oxidation treatment of sludge |
| CN102657996A (en) * | 2012-05-28 | 2012-09-12 | 四川亚连科技有限责任公司 | Double-tower low-pressure method for acquiring CO2 in flue gas |
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