CN115417488A - Supercritical water oxidation system and method for treating large concentration difference organic waste liquid - Google Patents
Supercritical water oxidation system and method for treating large concentration difference organic waste liquid Download PDFInfo
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- CN115417488A CN115417488A CN202211051990.2A CN202211051990A CN115417488A CN 115417488 A CN115417488 A CN 115417488A CN 202211051990 A CN202211051990 A CN 202211051990A CN 115417488 A CN115417488 A CN 115417488A
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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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
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
Abstract
A supercritical water oxidation system for treating organic waste liquid with large concentration difference comprises a feeding system, an oxygen inlet system, a preheating system, a reaction system, a condensing system, a backpressure system, a salt discharging system and a gas-liquid separation system; the feeding system comprises a low COD waste liquid tank (1), a high COD waste liquid tank (2), a combustion-supporting solvent tank (3), a feeding pump I (4-1) and a feeding pump II (4-2); the oxygen inlet system comprises an oxidant bottle (12), a compressor (13) and a heater (14); the preheating system mainly comprises a preheater (5); the condensation system mainly comprises a cooler I (8-1) and a concentrated brine condenser II (8-2); the invention adopts a mode of connecting the multistage supercritical water oxidation reactors in series to improve the capability of the system for treating the organic matters in the wastewater, so that the conversion rate of the organic matters in the wastewater reaches 99.99 percent.
Description
Technical Field
The invention discloses a supercritical water oxidation system and a supercritical water oxidation method for treating organic waste liquid with large concentration difference, relates to the field of organic waste liquid treatment, particularly provides a system and a method for treating organic waste liquid by utilizing a supercritical water oxidation technology, and aims to treat organic waste liquid with large concentration difference of two or more organic matters.
Technical Field
Supercritical water is water in a special state with temperature and pressure reaching and exceeding the supercritical point (374.3 ℃ and 22.1 MPa) of water, and the water has the characteristics of low density, low viscosity, large diffusion coefficient, small dielectric constant and the like and is widely applied. Because of the low dielectric constant of the supercritical water, the property of the supercritical water is closer to that of a nonpolar solvent, so that the supercritical water is a good solvent for various organic matters and gases (such as air, oxygen, nitrogen and the like), the phase interface between different phase substances is eliminated, and the mass transfer and the heat transfer between the substances are accelerated.
Supercritical water oxidation treatment organic waste liquid is exactly the characteristics of make full use of supercritical water for organic matter and oxidant (air, oxygen etc.) are dissolved each other completely, and then take place quick oxidation reaction, make the organic matter oxidize completely and generate carbon dioxide and water, do not produce other secondary pollutant, consequently are an organic wastewater treatment technology who has the wide application prospect. However, because the supercritical water oxidation reaction is a strong exothermic reaction and limited by reactor materials, the COD value of the organic waste liquid treated by supercritical water oxidation must be moderate, too high COD value can cause the temperature in the reactor to exceed the design temperature due to excessive reaction heat release, thereby causing operation risk, and too low COD value also causes the reaction process to consume a large amount of energy due to the establishment and maintenance of the supercritical water environment, thereby causing high operation cost.
Under the general condition, the organic waste water of many enterprises's variety is various, and concentration difference is great (COD value is from several thousand to several tens of thousands etc.), at first evenly mixes the organic waste water of different COD values through the mode of raw materials emulsification when utilizing supercritical water oxidation technique to handle, configures into the moderate organic waste liquid raw materials of COD value, however, because waste water impurity is more, brings serious challenge to the emulsification technology, inhomogeneous COD value also brings serious challenge to supercritical water oxidation technology. In addition, with the stricter environmental protection policy of the country, the conversion rate of organic matters in the traditional supercritical water oxidation treatment organic wastewater process is only about 99%, and in order to further improve the conversion rate of organic matters, measures such as increasing the reaction temperature and pressure are generally adopted, so that a more rigorous operation environment is created.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide a supercritical water oxidation system and a supercritical water oxidation method for treating organic waste liquid with large concentration difference, and the conversion rate of organic matters is improved.
A supercritical water oxidation system for treating organic waste liquid with large concentration difference comprises a feeding system, an oxygen inlet system, a preheating system, a reaction system, a condensing system, a backpressure system, a salt discharge system and a gas-liquid separation system; the feeding system comprises a low COD waste liquid tank 1, a high COD waste liquid tank 2, a combustion-supporting solvent tank 3, a feeding pump I4-1 and a feeding pump II 4-2; the oxygen inlet system comprises an oxidant bottle 12, a compressor 13 and a heater 14; the preheating system mainly comprises a preheater 5; the condensation system mainly comprises a cooler I8-1 and a strong brine condenser II 8-2;
the low COD waste liquid tank 1 is connected with the middle section of the shell side of the preheater 5 through a feeding pump I4-1; the high COD waste liquid tank 2 is connected with the lower section of the shell side of the preheater 5 through a feeding pump II 4-2; the outlet end of the shell side of the preheater 5 is connected with a regulating valve III 15-3, and the regulating valve III 15-3 is connected with the top end of a supercritical water oxidation reactor I6; the upper section of the side wall of the supercritical water oxidation reactor I6 is connected with a one-way valve 16, and the outlet of the one-way valve 16 is connected with a supercritical water oxidation reactor II 7; the upper end of the side wall of the supercritical water oxidation reactor II7 is respectively connected with an adjusting valve IV 15-4 and an adjusting valve V15-5; an outlet of the adjusting valve IV 15-4 is connected with the upper end of a tube pass of the preheater 5; an outlet of the regulating valve V15-5 is connected with a pipeline at the lower end of a tube pass of the preheater 5, and the regulating valve V15-5 is connected with a shell pass inlet end of the cooler I8-1; the outlet end of the cooler I8-1 is connected with a backpressure valve 9, and the outlet of the backpressure valve 9 is connected with the middle section of a gas-liquid separator I10-1; after the gas-liquid separator I10-1 passes through the gas-liquid separator, gas is discharged from the top end of the gas-liquid separator I10-1, and liquid is discharged from the bottom end of the gas-liquid separator I10-1;
an outlet of the combustion-supporting solvent tank 3 is connected with a feeding pump III 4-3, an outlet of the feeding pump III 4-3 is connected with an adjusting valve VI 15-6 and an adjusting valve VII 15-7, and outlets of the adjusting valve VI 15-6 and the adjusting valve VII 15-7 are respectively connected with the lower section of the side wall of the supercritical water oxidation reactor I6 and the lower section of the side wall of the supercritical water oxidation reactor II 7;
the outlet of the oxidant bottle 12 is connected with the inlet of a gas compressor 13, the outlet of the gas compressor 13 is connected with a gas heater 14, the outlet of the gas heater 14 is respectively connected with an adjusting valve I15-1 and an adjusting valve II 15-2, and the outlets of the adjusting valve I15-1 and the adjusting valve II 15-2 are respectively connected with the top ends of a supercritical water oxidation reactor I6 and a supercritical water oxidation reactor II 7;
the pipeline at the bottom ends of a supercritical water oxidation reactor I6 and a supercritical water oxidation reactor II7 of the reaction system is gathered and then connected with a cooler II 8-2 shell pass, an outlet of the cooler II 8-2 shell pass is connected with a salt discharge valve 11, an outlet of the salt discharge valve 11 is connected with the middle section of a gas-liquid separator II 10-2, gas is discharged from the top end of the gas-liquid separator II 10-2 after passing through the gas-liquid separator, and liquid is discharged from the bottom end of the gas-liquid separator II 10-2.
Condenser I8-1 is a gas condenser, and condenser II 8-2 is a strong brine condenser.
The oxidizer bottle 12 is a gaseous oxidizer bottle or a liquid oxidizer bottle.
The supercritical water oxidation method of the large concentration difference organic waste liquid of the supercritical water oxidation system for treating the large concentration difference organic waste liquid according to claim 1 comprises the following specific steps:
injecting low-COD waste liquid into a low-COD waste liquid tank 1, injecting the low-COD waste liquid into a shell pass of a preheater 5 through a feeding pump I4-1, controlling the volume of the low-COD waste liquid through the flow of the feeding pump 4-1, and stopping feeding when the volume of the low-COD waste liquid reaches 3/4 of the shell pass volume of the preheater 5;
injecting a combustion-supporting solvent into a combustion-supporting solvent box 3, opening an adjusting valve VI 15-6, keeping the adjusting valve VII 15-7 in a closed state, injecting the combustion-supporting solvent into a supercritical water oxidation reactor I6 through a feeding pump III 4-3, and controlling the volume of waste liquid to be 1/3 of the volume of a reactor I through the flow of the feeding pump III 4-3;
step three, closing the regulating valve VI 15-6, opening the regulating valve VII 15-7, injecting a combustion-supporting solvent into the supercritical water oxidation reactor II7 through the feed pump III 4-3, and controlling the volume of the waste liquid to be 1/3 of the volume of the supercritical water oxidation reactor II7 through the flow of the feed pump III 4-3;
step four, closing the regulating valve VII 15-7, enabling the regulating valve IV 15-4 to be in an opening state, and enabling the regulating valve V15-5 to be in a closing state;
opening a regulating valve I15-1 and a regulating valve II 15-2, opening a gas compressor 13 to pressurize oxygen, heating the oxygen at a heater 14, then feeding the oxygen into a supercritical water oxidation reactor I6 and a supercritical water oxidation reactor II7, and adjusting the opening degrees of the regulating valve I15-1 and the regulating valve II 15-2 to realize the allocation of the gas oxidant amount in the supercritical water oxidation reactor I6 and the supercritical water oxidation reactor II 7;
sixthly, in the supercritical water oxidation reactor I6 and the supercritical water oxidation reactor II7, a combustion-supporting solvent and an oxidant generate oxidation reaction to generate CO2 and H2O, and release a large amount of heat, and the opening degrees of a regulating valve VI 15-6 and a regulating valve VII 15-7 are regulated to enable the combustion-supporting solvent to continuously enter the supercritical water oxidation reactor I6 and the supercritical water oxidation reactor II7 and to be mixed with oxygen to generate oxidation reaction, so that the temperature and the pressure of the supercritical water oxidation reactor I6 and the supercritical water oxidation reactor II7 are gradually increased;
seventhly, gas mixtures such as high-temperature steam, high-temperature carbon dioxide and the like generated in the reaction process in the supercritical water oxidation reactor I6 and the supercritical water oxidation reactor II7 enter the tube pass of the preheater 5, and the low COD solution preset in the preheater 5 is gradually heated through a heat exchange coil in the preheater 5, so that the shell pass temperature and the pressure of the preheater 5 are gradually increased; if the heating time is too long, the electric heater outside the preheater 5 can be used for auxiliary heating until the temperature and the pressure in the preheater 5 reach and exceed the supercritical point of water, so that the shell side of the preheater 5 is in a complete supercritical state;
step eight, starting a feeding pump I4-1 and a feeding pump II 4-2, setting the flow ratio of the feeding pump I4-1 to the feeding pump to be 10, fully and uniformly mixing two waste liquids with different COD concentrations in shell-side supercritical water of a preheater 5, slowly opening a regulating valve III 15-3, allowing the uniformly mixed reaction materials to enter a supercritical water oxidation reactor I6, closing the feeding pump III 4-3 after setting time, and closing a regulating valve VI 15-6 and a regulating valve VII 15-7;
monitoring the temperature and pressure changes of the supercritical water oxidation reactor I6, and adjusting the flow ratio of the feed pump I4-1 and the feed pump II 4-2 according to the change conditions to ensure that the COD concentration of the uniform materials in the shell side of the preheater 5 is changed to adapt to the temperature and pressure change conditions of the supercritical water oxidation reactor I6; if the temperature in the supercritical water oxidation reactor I6 is high, the flow of the feed pump I4-1 is increased, and if the temperature in the supercritical water oxidation reactor I6 is low, the flow of the feed pump II 4-2 is increased;
step ten, in a stable operation stage, two waste liquids with different concentrations firstly enter a shell pass of a preheater 5, and are completely and uniformly mixed under the action of supercritical water in the shell pass to form a treated waste liquid with uniform COD concentration; the residence time of the two materials in the preheater 5 is ensured by adjusting the opening change of the valve III 15-3; then the wastewater enters a supercritical water oxidation reactor I6 to carry out oxidation reaction, when most of organic matters are oxidized and converted in the supercritical water oxidation reactor I6, a small part of organic matters continue to enter a supercritical water oxidation reactor II7 to carry out further oxidation reaction, and the conversion rate of the organic matters in the wastewater in a two-stage oxidation reactor is ensured to reach 99.99%;
step eleven, along with the reaction, the heat generated by the two-stage reactor may far exceed the energy required by the preheater 5, at the moment, the electric heater of the preheater 5 needs to be stopped in time, and if the heat is still high, the opening degree of the adjusting valve V15-5 can be adjusted, so that part of gas generated by the reaction does not pass through the tube pass of the preheater 5, and directly enters the condenser I8-1 through the adjusting valve V15-5;
step twelve, after waste heat of a supercritical water oxidation reactor I6 and a gas-phase product generated by the reaction is recovered by a preheater 5, the gas-phase product enters a condenser I8-1 for cooling, then is decompressed by a back pressure valve 9, and then enters a gas-liquid separator I10-1, the separated gas product is discharged from the top end of the gas-liquid separator I10-1, and the liquid product is discharged from the bottom end of the gas-liquid separator I10-1;
thirteen, precipitating and settling inorganic salt generated by the reaction from supercritical water in a supercritical water oxidation reactor I6 and a supercritical water oxidation reactor II7, depositing at the bottoms of the supercritical water oxidation reactor I6 and the supercritical water oxidation reactor II7, dissolving in the subcritical water at the bottoms of the supercritical water oxidation reactor I6 and the supercritical water oxidation reactor II7 for the second time to form concentrated brine, cooling by a condenser II 8-2, discharging after gas-liquid separation by a salt discharge valve 11 and a gas-liquid separator II 10-2, discharging gas from the top of the gas-liquid separator II 10-2, and discharging the concentrated brine from the bottom of the gas-liquid separator II 10-2.
In summary, compared with the prior art, the invention has the following advantages:
(1) The invention homogenizes the waste water with larger concentration difference of two organic matters by adopting a preheater capable of reaching a supercritical state, fully utilizes the property of high solubility of supercritical water to the organic matters to homogenize the waste water with larger concentration difference of the two organic matters, and solves the problem of poor homogenization of the traditional emulsification treatment process.
(2) The invention adopts a mode of connecting the multistage supercritical water oxidation reactors in series to improve the capability of the system for treating the organic matters in the wastewater, so that the conversion rate of the organic matters in the wastewater reaches 99.99 percent.
Drawings
FIG. 1 is a process flow diagram of the present invention;
the system comprises a low-COD waste liquid tank 1, a high-COD waste liquid tank 2, a combustion-supporting solvent tank 3, a preheater 5, a supercritical water oxidation reactor I6, a supercritical water oxidation reactor II7, a backpressure system 9, a salt discharge valve 11, an oxidant bottle 12, a compressor 13, a heater 14, a one-way valve 16, a feeding pump I4-1, a feeding pump II 4-2, a condenser 1-1, a condenser II 8-2, a gas-liquid separator I10-1, a gas-liquid separator II 10-2, an adjusting valve I15-1, an adjusting valve II 15-2, an adjusting valve III 15-3, an adjusting valve IV 15-4, an adjusting valve V15-5, an adjusting valve VI 15-6 and an adjusting valve VII.
The specific implementation mode is as follows:
the problem of poor uniformity of the emulsification process of the organic waste liquid with different concentration differences is solved by adopting a preheater capable of achieving a supercritical state. In addition, the invention also provides a method for connecting two supercritical water oxidation reactors in series, so that the conversion rate of organic matters of the whole treatment system reaches 99.99 percent under a milder operation environment, the conversion rate of the organic matters is improved, and the safety and the stability of the operation of the system are improved.
In order to achieve the purpose, the invention provides the following technical scheme:
a supercritical water oxidation system and method suitable for treating organic waste liquid with large concentration difference. The system mainly comprises a feeding system, an oxygen inlet system, a preheating system, a reaction system, a condensing system, a backpressure system, a salt discharge system, a gas-liquid separation system and the like.
Wherein the feeding system comprises a 1 low COD waste liquid tank, a 2 high COD waste liquid tank, a 3 combustion-supporting solvent tank, a 4 feeding pump and the like; wherein 1 low COD waste liquid case is used for storing the organic waste liquid that COD concentration is lower (for example COD value is less than 5000mg/L organic waste liquid), 2 high COD waste liquid case is used for storing the organic waste liquid that COD concentration is higher (for example COD value is higher than 80000mg/L organic waste liquid), 3 combustion-supporting solvent case is used for the combustion-supporting solvent that uses when storage system establishes the supercritical state, mainly be the liquid fuel that the ignition point is lower, like alcohols, ethers etc. feed pump is used for providing power for different solutions.
The oxygen inlet system comprises an oxidant bottle 12, a gas compressor 13, a gas heater 14 and the like, wherein the gas oxidant mainly provides oxidant such as air, oxygen and the like for the supercritical water oxidation system, the gas compressor provides power for the system oxidant, and the gas heater is used for heating the oxidant. In addition, the gas oxidant bottle 12 may also be a liquid oxidant, such as hydrogen peroxide, and when the oxidant is a liquid oxidant, the gas compressor 13 is modified to be a liquid feed pump.
The preheating system mainly comprises a preheater 5, the preheater comprises an internal heat exchange structure and an external heater, wherein the internal heat exchange structure mainly realizes the recovery of energy in gas products discharged by the reactor in an indirect heat exchange mode and heats materials in a shell pass of the preheater, and the internal heat exchange structure mainly comprises a heat exchange coil, a heat exchange tube nest and other structures for heat exchange. The external heater is mainly used for heating materials in the preheater, and the heater is mainly an electromagnetic heater, an infrared heater, a heat conduction oil heater and other elements for external heating. In addition, the preheater is equipped with two material imports, is used for the entering of different COD concentration organic waste liquid respectively, and wherein the organic waste liquid import of high COD concentration arranges in the organic waste liquid import top of low COD concentration, can effectively promote the homogeneous mixing of two kinds of organic waste liquids.
The reaction system mainly comprises a supercritical water oxidation reactor I6 and a supercritical water oxidation reactor II7 which are connected in series. Two supercritical water oxidation reactors all include combustion-supporting solvent import, reaction material import, oxidant import and arrange the salt mouth, and the reaction material takes place supercritical water oxidation reaction at first in reactor I, generates carbon dioxide and water, and the supercritical water oxidation reaction further takes place for the organic matter that does not take place the conversion in reactor II for the conversion rate of organic matter reaches 99.99% in the waste liquid.
The condensing system mainly comprises a cooler I8-1 and a cooler II 8-2 strong brine condenser, wherein the condenser can be a water condenser or an air condenser and is used for cooling gas and liquid generated after the oxidation reaction.
The back pressure system 9 mainly has a back pressure effect on the whole system and establishes a supercritical reaction environment for the system, and the back pressure system can be a back pressure valve or a complex for realizing the back pressure of the system in a multilayer throttling and pressure reducing mode.
The 10 gas-liquid separation system is mainly used for realizing the effective separation of low-temperature gas-liquid mixture, and can be a gas-liquid separator or other types of gas-liquid separation devices.
The salt discharging system 11 mainly plays a role in discharging strong brine formed in the system in time, and can be a salt discharging valve or other complex bodies capable of playing a role in discharging salt.
1. Description of the connection
Low COD waste liquid case 1 links to each other with charge pump I4-1, and the export of charge pump I4-1 is connected with 5 shell side middle sections of preheater. The high COD waste liquid tank 2 is connected with a feeding pump II 4-2, and an outlet of the feeding pump II 4-2 is connected with a shell pass lower section of a preheater 5. The shell pass outlet end of the preheater 5 is connected with an adjusting valve III 15-3, and the III 15-3 is connected with the top end of a supercritical water oxidation reactor I6. The upper section of the side wall of the supercritical water oxidation reactor I6 is connected with a one-way valve 16 and then connected with a supercritical water oxidation reactor II 7. The upper end of the side wall of the supercritical water oxidation reactor II7 is respectively connected with an adjusting valve IV 15-4 and a regulating valve V15-5. An outlet of the adjusting valve IV 15-4 is connected with the upper end of a tube pass of the preheater 5. An outlet of the regulating valve V15-5 is connected with a pipeline at the lower end of a tube pass of the preheater 5 and then connected with a shell pass inlet end of the cooler I8-1. The outlet end of the cooler I8-1 is connected with a backpressure valve 9, and the outlet is connected with the middle section of a gas-liquid separator I10-1. After passing through the gas-liquid separator, gas is discharged from the top end of the gas-liquid separator I10-1, and liquid is discharged from the bottom end of the gas-liquid separator I10-1.
An outlet of the combustion-supporting solvent tank 3 is connected with a feeding feed pump III 4-3, an outlet of the feeding pump III 4-3 is connected with an adjusting valve VI 15-6 and an adjusting valve VII 15-7, and the outlets are respectively connected with the lower section of the side wall of the supercritical water oxidation reactor I6 and the lower section of the side wall of the supercritical water oxidation reactor II 7.
The outlet of the oxygen cylinder 12 is connected with the inlet of a gas compressor 13, the outlet is connected with a gas heater 14, the outlet is connected with regulating valves I15-1 and II, and the outlet of the regulating valve is respectively connected with the top ends of a supercritical water oxidation reactor I6 and a supercritical water oxidation reactor II 7.
Supercritical water oxidation reactor I6 and supercritical water oxidation reactor II7 bottom pipeline are gathered and then are connected with cooler II 8-2 shell side, shell side export is connected with salt valve 11, export and II 10-2 middle sections of vapour and liquid separator are connected, and after passing through vapour and liquid separator, gas is discharged from II 10-2 top of vapour and liquid separator, and liquid is discharged from II 10-2 bottom of vapour and liquid separator.
2. Description of waste liquid treatment Process
(1) Injecting the low-COD waste liquid into a low-COD waste liquid box 1, injecting the waste liquid into the shell pass of the preheater 5 through a feeding pump I, controlling the volume of the waste liquid through the flow of the feeding pump, and stopping feeding when the volume of the waste liquid reaches 3/4 of the volume of the shell pass of the preheater 5;
(2) Injecting a combustion-supporting solvent into a combustion-supporting solvent box 3, opening an adjusting valve VI 15-6, keeping an adjusting valve VII 15-7 in a closed state, injecting the combustion-supporting solvent into a supercritical water oxidation reactor I6 through a feed pump III 4-3, and controlling the volume of waste liquid to be 1/3 of the volume of the supercritical water oxidation reactor I6 through the feed pump;
(3) Closing the regulating valve VI 15-6, opening the regulating valve VII 15-7, injecting a combustion-supporting solvent into the supercritical water oxidation reactor II7 through the feed pump III 4-3, and controlling the volume of the waste liquid to be 1/3 of the volume of the supercritical water oxidation reactor II7 through the feed pump flow;
(4) Closing the regulating valve VII 15-7, enabling the regulating valve IV 15-4 to be in an open state, and enabling the regulating valve V15-5 to be in a closed state;
(5) Opening a regulating valve I15-1 and a regulating valve II 15-2, opening a gas compressor 13 to pressurize oxygen, heating the oxygen at a gas heater 14, then feeding the oxygen into a supercritical water oxidation reactor I6 and a supercritical water oxidation reactor II7, and adjusting the opening degrees of the regulating valve I15-1 and the regulating valve II to realize the allocation of the gas oxidant amount in the two reactors;
(6) In the supercritical water oxidation reactor I6 and the supercritical water oxidation reactor II7, a combustion-supporting solvent and an oxidant generate oxidation reaction to generate CO2 and H2O and release a large amount of heat, the opening degrees of a valve VI 15-6 and a regulating valve VII 15-7 are regulated to enable the combustion-supporting solvent to continuously enter the supercritical water oxidation reactor I6 and the supercritical water oxidation reactor II7 and to be mixed with oxygen to generate oxidation reaction, and the temperature and the pressure of the supercritical water oxidation reactor I6 and the supercritical water oxidation reactor II7 are gradually increased;
(7) The gas mixture such as high-temperature steam and high-temperature carbon dioxide generated in the reaction process enters the tube side of the preheater 5, and the low COD solution preset in the preheater 5 is gradually heated through the heat exchange coil in the preheater 5, so that the shell side temperature and the pressure of the preheater 5 are gradually increased. If the heating time is too long, the electric heater outside the preheater 5 can be used for auxiliary heating until the temperature and the pressure in the preheater 5 reach and exceed the supercritical point of water, so that the shell side of the preheater 5 is in a complete supercritical state;
(8) Starting a feeding pump I4-1 and a feeding pump II 4-2, setting the flow ratio of the feeding pump I4-1 to the feeding pump II to be 10, fully and uniformly mixing two waste liquids with different COD concentrations in shell-side supercritical water of a preheater 5, slowly opening a regulating valve III 15-3, enabling the uniformly mixed reaction materials to enter a supercritical water oxidation reactor I6, closing the feeding pump III 4-3 after a period of time, and closing a regulating valve VI 15-6 and a regulating valve VII 15-7;
(9) The temperature and the pressure of the supercritical water oxidation reactor I6 are monitored, and the flow proportion of the feeding pump I4-1 and the feeding pump II 4-2 is adjusted according to the change situation, so that the COD concentration of the uniform material in the shell side of the preheater 5 is changed to some extent to adapt to the temperature and pressure change situation of the supercritical water oxidation reactor I6. If the temperature in the supercritical water oxidation reactor I6 is higher, increasing the flow of the feed pump I4-1, and if the temperature in the supercritical water oxidation reactor I6 is lower, increasing the flow of the feed pump II 4-2;
(10) In the steady operation stage, the waste liquid of two kinds of different concentrations at first gets into 5 shell passes of preheater, and the complete misce bene forms the comparatively even processing waste liquid of COD concentration under the effect of shell pass supercritical water. The residence time of the two materials in the preheater 5 is ensured by adjusting the opening change of the valve III 15-3. Then the wastewater enters a reactor I6 to carry out oxidation reaction, most of organic matters are oxidized and converted, and a small amount of organic matters continue to enter a reactor II7 to carry out further oxidation reaction, so that the conversion rate of the organic matters in the wastewater in the two-stage oxidation reactor is ensured to reach 99.99%;
(11) Along with the reaction, the heat generated by the two-stage reactor may far exceed the energy required by the preheater 5, at the moment, the electric heater of the preheater 5 needs to be stopped in time, if the heat is still high, the opening degree of the valve V15-5 can be adjusted by the condition, so that part of gas generated by the reaction does not pass through the tube pass of the preheater 5, and directly enters the condenser I8-1 through the adjusting valve V15-5;
(12) Gas-phase products generated by the reaction enter a condenser I8-1 for cooling after waste heat recovery of a preheater 5, then are decompressed through a back pressure valve 9, then enter a gas-liquid separator I10-1, separated gas products are discharged from the top end of the gas-liquid separator, and liquid products are discharged from the bottom end of the gas-liquid separator;
(13) Inorganic salt that the reaction generated precipitates in supercritical water oxidation reactor I6 and supercritical water oxidation reactor II7 supercritical water gradually, subsides, deposit in supercritical water oxidation reactor I6 or supercritical water oxidation reactor II7 bottom to the secondary dissolves in the subcritical water with reactor bottom, forms the strong brine, through II 8-2 cooling of condenser, then discharge after through discharge salt valve 11 and II 10-2 gas-liquid separation of vapour and liquid separator, gaseous discharge from vapour and liquid separator top, the strong brine is discharged from vapour and liquid separator bottom.
A process flow chart of supercritical water oxidation treatment for treating organic waste liquid with large concentration difference, which is shown in figure 1. The specific implementation process of the process flow comprises the following steps:
(1) Injecting the low-COD waste liquid into the preheater 5 through the feeding pump I4-1, controlling the volume of the waste liquid through the flow of the feeding pump, and stopping feeding when the volume of the waste liquid reaches 3/4 of the shell side volume of the preheater 5;
(2) Opening an adjusting valve VI 15-6, keeping an adjusting valve VII 15-7 in a closed state, injecting a combustion-supporting solvent into the supercritical water oxidation reactor I6 through a feeding pump III 4-3, and controlling the volume of the waste liquid to be 1/3 of the volume of the reactor I through the feeding pump flow;
(3) Closing the regulating valve VI 15-6, opening the regulating valve VII 15-7, injecting a combustion-supporting solvent into the supercritical water oxidation reactor II7 through the feed pump III 4-3, and controlling the volume of the waste liquid to be 1/3 of the volume of the reactor II through the flow control of the feed pump;
(4) The regulating valve VII 15-7 is closed, the IV 15-4 is in an open state, and the regulating valve V15-5 is in a closed state;
(5) Opening an adjusting valve I15-1 and an adjusting valve II, opening a gas compressor 13 to pressurize an oxidant, heating the oxidant at a gas heater 14, and then feeding the oxidant into a reactor I and a reactor II, and realizing the allocation of the amount of the gas oxidant in the two reactors through the opening degrees of the adjusting valve I15-1 and the adjusting valve II 15-2;
(6) In a supercritical water oxidation reactor I6 and a supercritical water oxidation reactor II7, a combustion-supporting solvent and an oxidant generate oxidation reaction and emit a large amount of heat, the opening degrees of a valve VI 15-6 and an adjusting valve VII 15-7 are adjusted to ensure that the combustion-supporting solvent continuously enters the supercritical water oxidation reactor I6 and the supercritical water oxidation reactor II7, and the temperature and the pressure of the supercritical water oxidation reactor I6 and the supercritical water oxidation reactor II7 are gradually increased under the action of the oxidant;
(7) High-temperature steam, carbon dioxide and other gases generated in the reaction process enter the tube side of the preheater 5, and the low COD solution preset in the preheater 5 is gradually heated, so that the shell side temperature and the pressure of the preheater 5 are gradually increased. If the heating time is too long, the electric heater outside the preheater 5 can be used for auxiliary heating until the temperature and the pressure in the preheater 5 reach and exceed the supercritical point of water, so that the shell side of the preheater 5 is in a complete supercritical state;
(8) Starting a feed pump I4-1 and a feed pump II 4-2, setting the flow ratio of the two to be 10;
(9) Monitoring the change of the temperature and the pressure of the supercritical water oxidation reactor I6, and adjusting the flow ratio of the feed pump I4-1 and the feed pump II 4-2 according to the change condition to ensure that the COD concentration of the uniform material in the preheater 5 is changed to adapt to the change condition of the temperature and the pressure of the supercritical water oxidation reactor I6;
(10) In the stable operation stage, two waste liquids with different concentrations firstly enter the 5 preheaters, are completely and uniformly mixed under the action of shell-side supercritical water, and the retention time of the two materials in the 5 preheaters is ensured by the change of the opening degree of the regulating valve III 15-3. Then the wastewater enters a supercritical water oxidation reactor I6 to carry out oxidation reaction, most of organic matters are oxidized and converted in the supercritical water oxidation reactor I6, and a small amount of organic matters continue to enter a supercritical water oxidation reactor II7 to carry out further oxidation reaction, so that the conversion rate of the organic matters in the wastewater in a two-stage oxidation reactor is ensured to reach 99.99%;
(11) Along with the reaction, the heat generated by the two-stage reactor may far exceed the energy required by the 5 preheater, at the moment, the electric heater of the 5 preheater needs to be stopped in time, if the heat is still higher, the opening degree of the condition adjusting valve V15-5 can be used, so that part of gas generated by the reaction directly enters the condenser I8-1 through the adjusting valve V15-5;
(12) Gas-phase products generated by the reaction enter a condenser I8-1 for cooling after being subjected to waste heat recovery of a preheater 5, and are discharged after being decompressed by a backpressure system and gas-liquid separation by a gas-liquid separator;
(13) And after inorganic salt generated by the reaction is deposited at the bottom of the reactor, cooling by a condenser II 8-2, and then discharging after gas-liquid separation by a salt discharge system and a gas-liquid separator.
Claims (4)
1. A supercritical water oxidation system for treating organic waste liquid with large concentration difference comprises a feeding system, an oxygen inlet system, a preheating system, a reaction system, a condensing system, a backpressure system, a salt discharge system and a gas-liquid separation system; the feeding system comprises a low COD waste liquid tank (1), a high COD waste liquid tank (2), a combustion-supporting solvent tank (3), a feeding pump I (4-1) and a feeding pump II (4-2); the oxygen inlet system comprises an oxidant bottle (12), a compressor (13) and a heater (14); the preheating system mainly comprises a preheater (5); the condensation system mainly comprises a cooler I (8-1) and a concentrated brine condenser II (8-2);
the low COD waste liquid tank (1) is connected with the middle section of the shell side of the preheater (5) through a feeding pump I (4-1); the high COD waste liquid tank (2) is connected with the lower section of the shell pass of the preheater (5) through a feeding pump II (4-2); the shell pass outlet end of the preheater (5) is connected with a regulating valve III (15-3), and the regulating valve III (15-3) is connected with the top end of a supercritical water oxidation reactor I (6); the upper section of the side wall of the supercritical water oxidation reactor I (6) is connected with a one-way valve (16), and the outlet of the one-way valve 1 (6) is connected with a supercritical water oxidation reactor II (7); the upper end of the side wall of the supercritical water oxidation reactor II (7) is respectively connected with an adjusting valve IV 1 (5-4) and an adjusting valve V (15-5); the outlet of the regulating valve IV (15-4) is connected with the upper end of the tube pass of the preheating (5); an outlet of the regulating valve V1 (5-5) is connected with a pipeline at the lower end of a tube pass of the preheater (5), and a regulating valve V (15-5) is connected with a shell pass inlet end of the cooler I (8-1); the outlet end of the cooler I (8-1) is connected with a back pressure valve (9), and the outlet of the back pressure valve (9) is connected with the middle section of the gas-liquid separator I (10-1); after the gas-liquid separator I (10-1) passes through the gas-liquid separator, gas is discharged from the top end of the gas-liquid separator I (10-1), and liquid is discharged from the bottom end of the gas-liquid separator I (10-1);
an outlet of the combustion-supporting solvent tank (3) is connected with a feeding pump III (4-3), an outlet of the feeding pump III (4-3) is connected with a regulating valve VI (15-6) and a regulating valve VII (15-7), and outlets of the regulating valve VI (15-6) and the regulating valve VII (15-7) are respectively connected with the lower section of the side wall of the supercritical water oxidation reactor I (6) and the lower section of the side wall of the supercritical water oxidation reactor II (7);
the outlet of the oxidant bottle (12) is connected with the inlet of a gas compressor (13), the outlet of the gas compressor (13) is connected with a gas heater (14), the outlet of the gas heater (14) is respectively connected with a regulating valve I (15-1) and a regulating valve II (15-2), and the outlets of the regulating valve I (15-1) and the regulating valve II (15-2) are respectively connected with the top ends of a supercritical water oxidation reactor I (6) and a supercritical water oxidation reactor II (7);
a pipeline at the bottom ends of a supercritical water oxidation reactor I (6) and a supercritical water oxidation reactor II (7) of the reaction system is gathered and then connected with a cooler II (8-2) shell pass, an outlet of the cooler II (8-2) shell pass is connected with a salt discharge valve (11), an outlet of the salt discharge valve (11) is connected with the middle section of a gas-liquid separator II (10-2), after passing through the gas-liquid separator, gas is discharged from the top end of the gas-liquid separator II (10-2), and liquid is discharged from the bottom end of the gas-liquid separator II (10-2).
2. The supercritical water oxidation system for treating large concentration difference organic waste liquid according to claim 1, wherein the condenser I (8-1) is a gas condenser, and the condenser II (8-2) is a concentrated brine condenser.
3. The supercritical water oxidation system for treating large concentration difference organic waste liquid according to claim 1 or 2, characterized in that the oxidizer bottle (12) is a gas oxidizer bottle or a liquid oxidizer bottle.
4. The supercritical water oxidation method of the large concentration difference organic waste liquid of the supercritical water oxidation system for treating the large concentration difference organic waste liquid according to claim 1 comprises the following specific steps:
injecting low-COD waste liquid into a low-COD waste liquid tank (1), injecting the low-COD waste liquid into a shell pass of a preheater (5) through a feeding pump I (4-1), controlling the volume of the low-COD waste liquid through the flow of the feeding pump (4-1), and stopping feeding when the volume of the low-COD waste liquid reaches 3/4 of the shell pass volume of the preheater (5);
injecting a combustion-supporting solvent into a combustion-supporting solvent box (3), opening an adjusting valve VI (15-6), keeping an adjusting valve VII (15-7) in a closed state, injecting the combustion-supporting solvent into a supercritical water oxidation reactor I (6) through a feed pump III (4-3), and controlling the volume of waste liquid to be 1/3 of the volume of the supercritical water oxidation reactor I (6) through the flow of the feed pump III (4-3);
step three, closing the regulating valve VI (15-6), opening the regulating valve VII (15-7), injecting a combustion-supporting solvent into the supercritical water oxidation reactor II (7) through a feeding pump III (4-3), and controlling the volume of the waste liquid to be 1/3 of the volume of the supercritical water oxidation reactor II (7) through the flow of the feeding pump III (4-3);
step four, closing the regulating valve VII 1 (5-7), enabling the regulating valve IV (15-4) to be in an open state, and enabling the regulating valve V (15-5) to be in a closed state;
opening a regulating valve I (15-1) and a regulating valve II (15-2), opening a gas compressor (13), pressurizing oxygen, heating the oxygen at a heater (14), and then introducing the oxygen into a supercritical water oxidation reactor I (6) and a supercritical water oxidation reactor II (7), and adjusting the gas oxidant amount in the supercritical water oxidation reactor I (6) and the supercritical water oxidation reactor II (7) by adjusting the opening degrees of the regulating valve I (15-1) and the regulating valve II (15-2);
sixthly, in the supercritical water oxidation reactor I (6) and the supercritical water oxidation reactor II (7), a combustion-supporting solvent and an oxidant are subjected to oxidation reaction to generate CO2 and H2O and release a large amount of heat, and the opening degrees of a regulating valve VI (15-6) and a regulating valve VII (15-7) are regulated to ensure that the combustion-supporting solvent continuously enters the supercritical water oxidation reactor I (6) and the supercritical water oxidation reactor II (7) and is mixed with oxygen to perform oxidation reaction, so that the temperature and the pressure of the supercritical water oxidation reactor I (6) and the supercritical water oxidation reactor II (7) are gradually increased;
step seven, gas mixtures such as high-temperature steam, high-temperature carbon dioxide and the like generated in the reaction process in the supercritical water oxidation reactor I (6) and the supercritical water oxidation reactor II (7) enter the tube side of the preheater (5), and a low COD solution preset in the preheater (5) is gradually heated through a heat exchange coil in the preheater (5), so that the shell side temperature and the pressure of the preheater (5) are gradually increased; if the heating time is too long, the electric heater outside the preheater (5) can be used for auxiliary heating until the temperature and the pressure in the preheater (5) reach and exceed the supercritical point of water, so that the shell side of the preheater (5) is in a complete supercritical state;
step eight, starting a feeding pump I (4-1) and a feeding pump II (4-2), setting the flow ratio of the feeding pump I (4-1) to the feeding pump II to be 10, fully and uniformly mixing two waste liquids with different COD concentrations in shell-side supercritical water of a preheater (5), slowly opening a regulating valve III (15-3), allowing the uniformly mixed reaction materials to enter a supercritical water oxidation reactor I (6), closing the feeding pump III (4-3) after setting time, and closing a regulating valve VI (15-6) and a regulating valve VII (15-7);
monitoring the temperature and pressure changes of the supercritical water oxidation reactor I (6), and adjusting the flow ratio of the feed pump I (4-1) and the feed pump II (4-2) according to the change conditions to ensure that the COD concentration of the uniform material in the shell pass of the preheater (5) is changed to adapt to the temperature and pressure change conditions of the supercritical water oxidation reactor I (6); if the temperature in the supercritical water oxidation reactor I (6) is higher, increasing the flow of the feed pump I (4-1), and if the temperature in the supercritical water oxidation reactor I (6) is lower, increasing the flow of the feed pump II (4-2);
step ten, in a stable operation stage, two waste liquids with different concentrations firstly enter a shell pass of a preheater (5) and are completely and uniformly mixed under the action of supercritical water in the shell pass to form a treated waste liquid with uniform COD concentration; the residence time of the two materials in the preheater (5) is ensured by adjusting the opening change of the valve III (15-3); then the wastewater enters a supercritical water oxidation reactor I (6) for oxidation reaction, when most of organic matters are oxidized and converted in the supercritical water oxidation reactor I (7), a small part of organic matters continue to enter a supercritical water oxidation reactor II (7) for further oxidation reaction, and the conversion rate of the organic matters in the wastewater in a two-stage oxidation reactor is ensured to reach 99.99%;
eleventh, along with the reaction, the heat generated by the two-stage reactor may far exceed the energy required by the preheater (5), at this time, the electric heater of the preheater (5) needs to be stopped in time, if the heat is still high, the opening degree of the regulating valve V (15-5) can be adjusted, so that part of gas generated by the reaction does not pass through the tube pass of the preheater (5), and directly enters the condenser I (8-1) through the regulating valve V (15-5);
step twelve, after waste heat recovery of a supercritical water oxidation reactor I (6) and a gas-phase product generated by the reaction through a preheater 5), cooling the gas-phase product in a condenser I (8-1), then decompressing the gas-phase product through a backpressure valve (9), and then feeding the gas-phase product into a gas-liquid separator I (10-1), wherein the separated gas product is discharged from the top end of the gas-liquid separator I (10-1), and the liquid product is discharged from the bottom end of the gas-liquid separator I (10-1);
and thirteen, gradually precipitating and settling inorganic salt generated by the reaction from supercritical water in the supercritical water oxidation reactor I (6) and the supercritical water oxidation reactor II (7), depositing at the bottoms of the supercritical water oxidation reactor I (6) and the supercritical water oxidation reactor II (7), dissolving in subcritical water at the bottoms of the supercritical water oxidation reactor I (6) and the supercritical water oxidation reactor II (7) for a second time to form concentrated brine, cooling by the condenser II (8-2), then discharging after gas-liquid separation by the salt discharge valve (11) and the gas-liquid separator II (10-2), discharging gas from the top of the gas-liquid separator II (10-2), and discharging the concentrated brine from the bottom of the gas-liquid separator II (10-2).
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