CN103601282A - Method for treating refractory wastewater by virtue of supercritical water oxidation technology - Google Patents
Method for treating refractory wastewater by virtue of supercritical water oxidation technology Download PDFInfo
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Abstract
The invention provides a method for treating refractory wastewater by virtue of a supercritical water oxidation technology. The method comprises the following steps of: feeding the preheated wastewater into a salt separator for supercritical desalination, heating an oxidant which is preheated previously through a heat exchanger to a desired temperature, feeding the heated oxidant and the desalinated wastewater into a supercritical water oxidation reactor from the two ends of the reactor, respectively, controlling the system pressure by a back pressure valve, and carrying out a supercritical water oxidation reaction to degrade pollutants in the wastewater into non-toxic matters such as CO2, N2 and H2O; feeding the clean high-temperature and high-pressure fluid obtained after the reaction into the heat exchanger to exchange heat with the wastewater and the oxidant, respectively, and then cooling and separating, returning the excessive oxidant to the supercritical water oxidation reactor and causing the liquid into a normal-pressure gas-liquid separator, discharging the gases such as CO2 and N2 through the top of the normal-pressure gas-liquid separator, and discharging the treated clean water from the bottom of the normal-pressure gas-liquid separator. The method for treating the refractory wastewater by virtue of the supercritical water oxidation technology has the advantages of being high in wastewater treatment efficiency without secondary pollution, and suitable for treating the refractory wastewater different in concentration.
Description
Technical field
The present invention relates to the treatment process of used water difficult to degradate, more specifically say a kind of method of supercritical water oxidation processing used water difficult to degradate.
Background technology
Used water difficult to degradate is a kind of unmanageable trade effluent, is mainly the waste water producing in the production processes such as dyestuff, agricultural chemicals, medical treatment, coking, and quantity discharged is large, Pollutant levels are high, toxicity is large, and its composition is also complicated and changeable, and chemical oxygen demand is high, is difficult to biological degradation.Conventionally, contain the heterogeneous ring compound of a large amount of ammonia nitrogens, aldehydes matter, mononuclear aromatics and polycyclic aromatic hydrocarbons and nitrogenous, sulphur, oxygen in waste water, in waste water, inorganic salt content is also very high.Ammonia and phenols etc. are all the compounds that toxicity is larger, enter water surrounding and can cause serious water pollution, and therefore there is strict regulation in country to the discharge of high-concentration hardly-degradable waste water.Processing to used water difficult to degradate, adopts multiple-stage treatment technology conventionally: coagulation comprises the unit such as precipitation, extraction, stripping, with remove portion lime-ash, and phenols ammonia etc.; Second-stage treatment is mainly biochemical process, can dispose most pollutents in waste water, comprises activated sludge process and Biological fitler method; Advanced treatment comprises Ozonation and active carbon adsorption.Due to advanced treatment somewhat expensive, most enterprises only carry out second-stage treatment to waste water, are about to waste water and carry out the pre-treatment such as solvent extraction dephenolize, the ammonia still process of water vapour stripping, then process with biochemical process.Not only treatment scheme is complicated, facility investment is many, floor space is large for this method, and the ammonia nitrogen of water outlet, COD etc. are difficult to reach emission standard.Day by day serious along with the enhancing of mankind's environmental consciousness and shortage of water resources, water pollution problems, exploiting economy, effectively wastewater processing technology just seems particularly important.
Summary of the invention
The object of the invention is provides a kind of efficient, clean treatment technology for used water difficult to degradate.
Supercritical water oxidation (Supercritical Water Oxidation, SCWO) is emerging in recent years wastewater processing technology.Due to supercritical water (SCW) have that viscosity is low, spread coefficient is high, to organism and the feature such as gas dissolving power is strong.Supercritical Water Oxidation Technology utilizes organism and oxygen complete dissolution characteristics in supercritical water, greatly reduced resistance to mass transfer, organic oxidative degradation can be carried out in homogeneous phase, and organism is almost completely degraded to CO within the short period (<1 minute)
2, N
2and H
2the small molecules non-toxic substances such as O, and inorganic salt solvability in supercritical water sharply reduces, and (solubleness of typical inorganic salt is only 1-100mg.L
-1), make inorganic salt be easy to separation.Adopt supercritical Water Oxidation Technology to process the waste water containing a large amount of inorganic salt, can make the Separation and Recovery of inorganic salt and wastewater treatment carry out simultaneously.Compare with traditional water technology, compare with traditional water technology, supercritical Water Oxidation Technology has advantage clearly
For achieving the above object, the present invention adopts supercritical Water Oxidation Technology to process used water difficult to degradate, and its concrete grammar comprises the steps:
Waste water in wastewater storage tank carries out preheating by high-pressure pump pressurization input heat exchanger, and the waste water after preheating flows into salinity and carries out overcritical desalination from device, if do not need desalination, salt separator does not need work; Simultaneously, oxygenant in oxygenant storage tank carries out preheating via high-pressure pump pressurization input heat exchanger, enter afterwards well heater, if oxidant temperature satisfies the demands, well heater is without work, if oxidant temperature does not reach demand, well heater is started working, oxygenant is heated to required temperature, oxygenant after heating and the waste water after desalination flow into respectively overcritical water oxidization reactor from overcritical water oxidization reactor two ends, system pressure is controlled by back pressure valve, and supercritical water oxidation occurs, and the contaminant degradation in waste water is CO
2, N
2and H
2the toxicological harmless materials such as O; The rear clean high-temperature, high pressure fluid of reaction enters interchanger and waste water and oxygenant and carries out respectively heat exchange, enters afterwards water cooler cooling; High pressure fluid after cooling enters high-pressure gas-liquid separator and carries out separation, and excessive oxygenant returns to overcritical water oxidization reactor by high-pressure gas-liquid separator top and proceeds reaction, and liquid enters atmospheric gas liquid/gas separator by the bottom of high-pressure gas-liquid separator.CO
2, N
2deng gas, by atmospheric gas liquid/gas separator top, discharged, the cleaning water after processing is discharged by atmospheric gas liquid/gas separator bottom, as production, life reuse water, uses.
As mentioned above, waste water is the waste water producing in the production processes such as dyestuff, agricultural chemicals, medical treatment, coking.
As mentioned above, high-pressure pump pressure is 23-30MPa.
As mentioned above, the temperature of waste water after interchanger preheating is 350-375 ℃, and pressure is 23-30MPa.
As mentioned above, oxygenant used can be aqueous hydrogen peroxide solution, ozone or liquid oxygen; Oxygenant consumption be in waste water during organism complete oxidation the 2-5 of theoretical oxygen demand doubly, oxygenant is after preheater and well heater, temperature can rise to 550-700 ℃.
As mentioned above, the temperature of salt separator inside is 500-700 ℃, and pressure is 23-30MPa.
As mentioned above, the temperature of overcritical water oxidization reactor is controlled at 550-700 ℃, and pressure is regulated by back pressure valve, and is controlled at 23-30MPa, and at 10-40, in the residence time of second, the pollutent in waste water can be degraded to CO
2, N
2and H
2the toxicological harmless materials such as O.
As mentioned above, the temperature of high-pressure gas-liquid separator is 20-80 ℃, and pressure is 4-22MPa, and from high-pressure gas-liquid separator top, isolated excessive oxidant Returning reactor recycles.
As mentioned above, reacted high-temperature, high pressure fluid enters two interchanger, and heat exchanger structure is simple, and heat exchange efficiency is high.
As mentioned above, overcritical water oxidization reactor used is tubular reactor.
When as mentioned above, processing COD content is greater than 35000mg/L wastewater sample, it is autothermal reaction.
Compared with prior art, method tool of the present invention has the following advantages:
1. waste water, without carrying out pre-treatment, can directly enter supercritical water oxidation apparatus and process;
2. be suitable for processing the used water difficult to degradate of different concns, be particularly suited for processing the waste water producing in one or more the production processes such as high density dyestuff, agricultural chemicals, medical treatment, coking containing the heterogeneous ring compound of ammonia nitrogen, aldehydes matter, mononuclear aromatics and polycyclic aromatic hydrocarbons, nitrogen, sulphur, oxygen and a large amount of inorganic salt.
3. waste water treatment efficiency is high, and Pollutants in Wastewater can approach complete oxidation degraded in tens of seconds;
4. the inorganic salt in waste water can remove in the salt separator before being positioned over overcritical water oxidization reactor, avoid the induce reaction obstruction of device and pipeline of salt sedimentation, and the inorganic salt that simultaneously remove are easy to recycle;
5. process COD content and be greater than 35000mg/L wastewater sample, can rely on autoxidation heat release in reaction process to maintain the required temperature of reaction, do not need additionally to supply with heat.
6. use two interchanger, heat exchanger structure is simple, and heat exchange efficiency is high.
7. apparatus structure is compact, and technical process is short, saves land area;
8. whole treating processes is airtight carries out, non-secondary pollution, and the cleaning water after processing can realize reuse, has good environmental benefit and economic benefit.
Accompanying drawing explanation:
Fig. 1 is schematic flow sheet of the present invention.
In figure: 1. wastewater trough, 2. oxygenant storage tank, 3. waste water pump, 4. cryogenic oxygen agent pump, 5. waste water heat exchanger, 6. oxygenant interchanger, 7. salt separator, 8. overcritical water oxidization reactor, 9. oxidant heater, 10. water cooler, 11. system pressure variable valve, 12,16,18,20 valves, 13. inorganic salt solids, 14. high-pressure gas-liquid separators, 15. back pressure valve, 17. atmospheric gas liquid/gas separators, 19. reuse waters, 21. gases
Embodiment:
Embodiment 1
High-concentration coal gasification waste water containing ammonia nitrogen in high density, phenols, COD and inorganic salt is carried out to supercritical water oxidation processing, and waste water raw water quality used is as shown in table 1.Waste water in wastewater storage tank 1 is forced into 5 preheatings of 24MPa input heat exchanger by high-pressure pump 3, and waste water is preheated to and after 360 ℃, flows into temperature is that the salt separator 7 of 650 ℃ carries out desalination; Meanwhile, oxygenant is forced into 24MPa input heat exchanger 6 by storage tank 2 via high-pressure pump 4 and carries out preheating, and heater via 9 is heated to oxygenant and the waste water after desalination of 640 ℃ and by overcritical water oxidization reactor 8 two ends, is flowed into respectively, carries out supercritical water oxidation.Oxygenant consumption is 4 times of theoretical oxygen demand, and waste water is 32 seconds in the interior residence time of overcritical water oxidization reactor 8, and system pressure is controlled at 24MPa by back pressure valve 11.The temperature that water after processing flows out overcritical water oxidization reactor 8 is 660 ℃, enters high-pressure gas-liquid separator 14 after entering water cooler 10 cool to room temperature after interchanger 5,6 carries out heat recuperation.Isolated excessive oxidant returns to overcritical water oxidization reactor 8 by high-pressure gas-liquid separator top and recycles, and the liquid of high-pressure gas-liquid separator bottom enters atmospheric gas liquid/gas separator 17 after back pressure valve 15 decompressions.CO
2, N
2deng gas, by atmospheric gas liquid/gas separator top, discharged, the cleaning water after processing is discharged by atmospheric gas liquid/gas separator bottom.Effluent quality after processing is in Table 2.
Embodiment 2
To carrying out supercritical water oxidation processing containing the high concentration coking of ammonia nitrogen in high density, phenols, COD and inorganic salt, waste water raw water quality used is as shown in table 1.Waste water in wastewater storage tank 1 is forced into 5 preheatings of 25MPa input heat exchanger by high-pressure pump 3, and waste water is preheated to and after 355 ℃, flows into temperature is that the salt separator 7 of 650 ℃ carries out desalination; Meanwhile, oxygen is forced into 25MPa input heat exchanger 6 by storage tank 2 via high-pressure pump 4 and carries out preheating, and the oxygenant and the waste water after desalination that by well heater 9, are heated to 650 ℃ are flowed into by overcritical water oxidization reactor 8 two ends respectively, carry out supercritical water oxidation.Oxygenant consumption is 5 times of theoretical oxygen demand, and waste water is 24 seconds in the interior residence time of overcritical water oxidization reactor 8, and system pressure is controlled at 25MPa by back pressure valve 11.The temperature that water after processing flows out overcritical water oxidization reactor 8 is 650 ℃, after interchanger 5,6 carries out heat recuperation, enters water cooler 10, enters high-pressure gas-liquid separator 14 after cool to room temperature.Isolated excessive oxidant returns to overcritical water oxidization reactor 8 by high-pressure gas-liquid separator top and recycles, and the liquid of high-pressure gas-liquid separator bottom enters atmospheric gas liquid/gas separator 17 after back pressure valve 15 decompressions.CO
2, N
2deng gas, by atmospheric gas liquid/gas separator top, discharged, the cleaning water after processing is discharged by atmospheric gas liquid/gas separator bottom.Effluent quality after processing is in Table 2.
Embodiment 3
Textile fabric dyeing waste water containing ammonia nitrogen, COD and inorganic salt is carried out to supercritical water oxidation processing, and waste water raw water quality used is as shown in table 1.Waste water in wastewater storage tank 1 is forced into 5 preheatings of 25MPa input heat exchanger by high-pressure pump 3.Simultaneously, aqueous hydrogen peroxide solution is forced into 25MPa input heat exchanger 6 by storage tank 2 via high-pressure pump 4 and carries out preheating, the oxygenant and the waste water after desalination that by well heater 9, are heated to 500 ℃ are flowed into by overcritical water oxidization reactor 8 two ends respectively, carry out supercritical water oxidation.Oxygenant consumption is 2.5 times of theoretical oxygen demand, and waste water is 20 seconds in the interior residence time of overcritical water oxidization reactor 8, and system pressure is controlled at 25MPa by back pressure valve 11.The temperature that water after processing flows out overcritical water oxidization reactor 8 is 500 ℃, after interchanger 5,6 carries out heat recuperation, enters water cooler 10, enters high-pressure gas-liquid separator 14 after cool to room temperature.Isolated excessive oxidant returns to overcritical water oxidization reactor 8 by high-pressure gas-liquid separator top and recycles, and the liquid of high-pressure gas-liquid separator bottom enters atmospheric gas liquid/gas separator 17 after back pressure valve 15 decompressions.CO
2, N
2deng gas, by atmospheric gas liquid/gas separator top, discharged, the cleaning water after processing is discharged by atmospheric gas liquid/gas separator bottom.Effluent quality after processing is in Table 2.
Embodiment 4
High density underground gasification waste water containing ammonia nitrogen in high density, phenols, COD and inorganic salt is carried out to supercritical water oxidation processing, and waste water raw water quality used is as shown in table 1.Waste water in wastewater storage tank 1 is forced into 5 preheatings of 25MPa input heat exchanger by high-pressure pump 3, and waste water is preheated to and after 367 ℃, flows into temperature is that the salt separator 7 of 650 ℃ carries out desalination; Simultaneously, aqueous hydrogen peroxide solution is forced into 25MPa input heat exchanger 6 by storage tank 2 via high-pressure pump 4 and carries out preheating, the oxygenant and the waste water after desalination that by well heater 9, are heated to 648 ℃ are flowed into by overcritical water oxidization reactor 8 two ends respectively, carry out supercritical water oxidation.Oxygenant consumption is 3 times of theoretical oxygen demand, and waste water is 24 seconds in the interior residence time of overcritical water oxidization reactor 8, and system pressure is controlled at 25MPa by back pressure valve 11.The temperature that water after processing flows out overcritical water oxidization reactor 8 is 653 ℃, after interchanger 5,6 carries out heat recuperation, enters water cooler 10, enters high-pressure gas-liquid separator 14 after cool to room temperature.Isolated excessive oxidant returns to overcritical water oxidization reactor 8 by high-pressure gas-liquid separator top and recycles, and the liquid of high-pressure gas-liquid separator bottom enters atmospheric gas liquid/gas separator 17 after back pressure valve 15 decompressions.CO
2, N
2deng gas, by atmospheric gas liquid/gas separator top, discharged, the cleaning water after processing is discharged by atmospheric gas liquid/gas separator bottom.Effluent quality after processing is in Table 2.
Claims (9)
1. supercritical Water Oxidation Technology is processed a method for used water difficult to degradate, it is characterized in that comprising the steps:
Waste water in wastewater storage tank carries out preheating by high-pressure pump pressurization input heat exchanger, and the waste water after preheating flows into salinity and carries out overcritical desalination from device, if do not need desalination, salt separator does not need work; Simultaneously, oxygenant in oxygenant storage tank carries out preheating via high-pressure pump pressurization input heat exchanger, enter afterwards well heater, if oxidant temperature satisfies the demands, well heater is without work, if oxidant temperature does not reach demand, well heater is started working, oxygenant is heated to required temperature, oxygenant after heating and the waste water after desalination flow into respectively overcritical water oxidization reactor from overcritical water oxidization reactor two ends, system pressure is controlled by back pressure valve, and supercritical water oxidation occurs, and the contaminant degradation in waste water is CO
2, N
2and H
2the toxicological harmless materials such as O; The rear clean high-temperature, high pressure fluid of reaction enters interchanger and waste water and oxygenant and carries out respectively heat exchange, enters afterwards water cooler cooling; High pressure fluid after cooling enters high-pressure gas-liquid separator and carries out separation, and excessive oxygenant returns to overcritical water oxidization reactor by high-pressure gas-liquid separator top and proceeds reaction, and liquid enters atmospheric gas liquid/gas separator by the bottom of high-pressure gas-liquid separator;
CO
2, N
2deng gas, by atmospheric gas liquid/gas separator top, discharged, the cleaning water after processing is discharged by atmospheric gas liquid/gas separator bottom, as production, life reuse water, uses.
2. a kind of supercritical Water Oxidation Technology as claimed in claim 1 is processed the method for used water difficult to degradate, it is characterized in that described waste water is the waste water producing in dyestuff, agricultural chemicals, medical treatment or coking production process.
3. a kind of supercritical Water Oxidation Technology as claimed in claim 1 is processed the method for used water difficult to degradate, it is characterized in that described high-pressure pump pressure is 23-30MPa.
4. a kind of supercritical Water Oxidation Technology as claimed in claim 1 is processed the method for used water difficult to degradate, it is characterized in that the temperature of described waste water after interchanger preheating is 350-375 ℃, and pressure is 23-30MPa.
5. a kind of supercritical Water Oxidation Technology as claimed in claim 1 is processed the method for used water difficult to degradate, it is characterized in that described oxygenant is aqueous hydrogen peroxide solution, ozone or liquid oxygen; Oxygenant consumption be in waste water during organism complete oxidation the 2-5 of theoretical oxygen demand doubly, oxygenant is after preheater and well heater, temperature rises to 550-700 ℃.
6. a kind of supercritical Water Oxidation Technology as claimed in claim 1 is processed the method for used water difficult to degradate, it is characterized in that the temperature of described salt separator inside is 500-700 ℃, and pressure is 23-30MPa.
7. a kind of supercritical Water Oxidation Technology as claimed in claim 1 is processed the method for used water difficult to degradate, it is characterized in that the temperature of described supercritical water oxidation is controlled at 550-700 ℃, and is controlled at 23-30MPa, and the residence time is 10-40 second.
8. a kind of supercritical Water Oxidation Technology as claimed in claim 1 is processed the method for used water difficult to degradate, it is characterized in that the temperature of described high-pressure gas-liquid separator is 20-80 ℃, and pressure is 4-22Mpa.
9. a kind of supercritical Water Oxidation Technology as claimed in claim 1 is processed the method for used water difficult to degradate, it is characterized in that described overcritical water oxidization reactor is tubular reactor.
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