CN115196805B - Treatment method for deoiling, dedusting, deacidifying and deaminizing semi-coke wastewater - Google Patents
Treatment method for deoiling, dedusting, deacidifying and deaminizing semi-coke wastewater Download PDFInfo
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Classifications
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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
- C02F9/00—Multistage treatment of water, waste water or sewage
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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
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/001—Processes for the treatment of water whereby the filtration technique is of importance
-
- C—CHEMISTRY; METALLURGY
- 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
- C02F1/24—Treatment of water, waste water, or sewage by flotation
-
- C—CHEMISTRY; METALLURGY
- 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
- C02F1/26—Treatment of water, waste water, or sewage by extraction
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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
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/38—Treatment of water, waste water, or sewage by centrifugal separation
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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
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/40—Devices for separating or removing fatty or oily substances or similar floating material
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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
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
- C02F1/5281—Installations for water purification using chemical agents
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/16—Nitrogen compounds, e.g. ammonia
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- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
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- Organic Chemistry (AREA)
- Physical Water Treatments (AREA)
Abstract
The invention belongs to the technical field of sewage treatment, and discloses a method for deoiling, dedusting, deacidifying and deaminizing semi-coke wastewater. The method comprises the following steps: after partial free ammonia in the water is fixed by an acid adding device, the semi-coke wastewater is sent into a dissolved air floatation device through a lifting pump to carry out air floatation treatment on the wastewater, generated scum is scraped by a scum scraper, bottom sludge is treated and then is transported outwards, water discharged by the air floatation device is subjected to flocculation sedimentation after being filtered, and the scum and sediment are collected into an oil sludge tank; the clear liquid is sent to a double-medium filtering device for filtering residual flocs, the filtrate is sent to a homogenizing tank, the effluent of the homogenizing tank is pressurized by a lifting pump and then sent to the top and the middle of a deacidification tower in two ways, acid gas in the water is removed, the kettle liquid is mixed with alkali liquor and then sent to a deamination tower for steaming ammonia nitrogen to prepare ammonia water, and the treated wastewater is sent to a phenol recovery device for further removing organic matters. The invention ensures the water outlet effect of the working section through the front-end efficient deoiling and dedusting, realizes the efficient removal and recovery of acid gas and ammonia nitrogen through the normal-pressure deacidification and deamination, and improves the purity of byproducts.
Description
Technical Field
The invention belongs to the technical field of sewage treatment, and particularly relates to a treatment method for deoiling, dedusting, deacidifying and deaminizing semi-coke wastewater.
Technical Field
The low-temperature carbonization in low-rank coal is a key technology for realizing the quality and grade utilization of coal, and is widely applied to modern novel coal chemical engineering projects. The semi-coke wastewater is gas washing wastewater of raw gas generated in the middle-low temperature carbonization process of low-rank coal, is rich in refractory pollutants such as middle-low temperature coal tar, suspended matters, sulfides, ammonia nitrogen, phenol and the like, and has very complex raw water quality and high treatment difficulty. This is just about to become the main bottleneck that restricts the quality-classifying and grading utilization of coal, and is also one of the important factors that restricts the development of the quality-classifying and grading utilization industry of coal.
The existing treatment process of oil and dust in semi-coke wastewater mainly comprises oil removal, air floatation, filtration, coarse granulation, flocculation sedimentation and the like, and the treatment process of acid gas and ammonia nitrogen comprises normal pressure ammonia distillation and pressurized steam stripping deacidification deamination, and phenolic substances are recovered through extraction, so that the reduction of the content of oil, dust, acid gas, ammonia nitrogen and total phenol in the wastewater is achieved, and phenol, ammonia and sulfide in the wastewater are recovered to realize the recycling of special pollutants. The biochemical treatment system is combined to achieve the aim of treating the semi-coke wastewater. The oil and dust removal effect directly determines the operation stability of the phenol-ammonia recovery system and the equipment pollution blocking period, and the removal efficiency of acid gas and ammonia nitrogen is also the key of the stable and efficient operation of the biochemical system.
Under the situation that the current technical means and the national environmental protection department put forward a new standard of 'zero liquid discharge' for the coal chemical wastewater, the removal efficiency of oil, dust, sulfide and ammonia nitrogen is insufficient to meet the requirement of a biochemical treatment system on an imported water quality index, and residual medium and low temperature coal tar, sulfide and ammonia nitrogen cause huge impact on a phenol-ammonia recovery section and a biochemical treatment section, so that the product quality of wastewater recycling recovery is poor and the high-efficiency stable operation of the system is influenced. The prior semi-coke wastewater pretreatment process is characterized in that: (1) long residence time of oil dust removal and large equipment floor area: because part of oil exists in the wastewater stably in the form of emulsified oil, the relative density is close to 1, and the natural sedimentation or floating speed is low; (2) the ammonia condensate reflux amount is large, and the ammonia distillation system has low efficiency: the ammonia nitrogen content of the semi-coke wastewater is 2000-4000 mg/L, a large amount of ammonia nitrogen circulates in an ammonia evaporation system along with ammonia condensate, and the ammonia nitrogen concentration of effluent water is higher than 150mg/L under the condition of pressurization; (3) residual oils plug column internals, contaminate extractants and crude phenol: the phenol-ammonia recovery system is blocked by residual oil and dust, and the oil is discharged out of the system along with crude phenol products in the solvent recovery process; (4) the pretreatment has high anti-blocking requirement, and the equipment investment cost is huge: the deoiling and dedusting process equipment has long residence time, the theoretical plates of the phenol-ammonia recovery system are large, the operating pressure is high, and high-flux anti-blocking patent tower internals are needed, so that the investment of a pretreatment section is huge, and the method is an actual difficulty and challenge for treating the semi-coke wastewater.
Disclosure of Invention
Aiming at the problems existing in the prior art, the invention aims to provide a treatment method for deoiling, dedusting, deacidifying and deaminizing semi-coke wastewater.
The aim of the invention is achieved by the following scheme:
the treatment method for deoiling, dedusting, deacidifying and deaminizing the semi-coke wastewater sequentially comprises a pressurized dissolved air flotation device, a coagulating sedimentation device, a double-medium filtering device, a homogenizing tank, a deacidification tower and a deamination tower which are connected; the pressurized dissolved air floatation device is connected to an underground oil tank, the coagulation sedimentation device and the double-medium filtering device are connected to a sludge dewatering device, the deacidification tower is connected to an acid gas-liquid separation device, and the deamination tower is connected to an ammonia refining and absorbing device through a separator; wherein:
(1) The input end of the pressurized dissolved air floatation device is connected with raw material semi-coke wastewater, a compressed acid gas source and a strong acid output end, the semi-coke wastewater is subjected to pH value adjustment by an acid strengthening device, partial free ammonia in water is fixed, the acidified semi-coke wastewater is dissolved into sufficient acid gas source in the wastewater by a dissolved air pump, the pH value of the wastewater is further reduced, the wastewater is sent into a dissolved air tank, heavy oil and light oil are separated by stable pressure and standing, the heavy oil, the light oil and the water are layered, the oil product is sent into an underground oil tank, the water is sent into the bottom of an air floatation tank by a releaser for air floatation treatment, the upper layer scum is scraped by a scum scraper, bottom oil sludge is precipitated by an inclined plate and then is collected into the underground oil tank together with scum, and the clear liquid of the air floatation tank is extracted from the middle part, namely the semi-coke wastewater;
(2) The input end of the coagulation sedimentation device is connected with a gravity outflow port of an air floatation tank, air floatation water flows into the coagulation tank by gravity, the coagulation tank is provided with a stirring device, the semi-coke wastewater obtained in the step (1) and flocculating agent are fully stirred and coagulated, then the sedimentation tank is used for sedimentation to remove oil sludge, the top oil slick is scraped by an oil scraper, the bottom oil sludge is collected and dehydrated and then is sent out, and a clear liquid in the middle layer, namely the semi-coke wastewater, is extracted;
(3) The double-medium filtering device is used for treating the clear liquid of the semi-coke wastewater obtained in the step (2), filtering suspended matters and flocs in the wastewater, delivering the semi-coke wastewater obtained at the outlet of the filter after deoiling and dedusting into a homogenizing tank to supply the deacidification tower for feeding, and returning the wastewater generated by backwashing to a coagulating sedimentation device;
(4) The deacidification tower is connected with an outlet of a lifting pump behind the homogenizing tank, deacidifies the semi-coke wastewater obtained in the step (3), cold and hot semi-coke wastewater in the step (3) is sent to the top and the middle of the deacidification tower in a split manner, acid gas is extracted from the tower top, the acid gas generated after condensation and gas-liquid separation is sent to an acid gas-liquid separation device, condensate is returned to the homogenizing tank, and the semi-coke wastewater is sent to the deamination tower through a tower kettle lifting pump;
(5) The deamination tower carries out deamination treatment on the semi-coke wastewater obtained in the step (4), the semi-coke wastewater obtained in the step (4) is mixed with alkali liquor through a pipeline mixer, fixed ammonia is converted into free ammonia, the free ammonia is pumped from the upper part of the deamination tower, ammonia-containing steam is condensed by a separator and then partially flows back into the tower, concentrated ammonia gas is extracted from the top of the separator and is prepared into dilute ammonia water through an absorption device or is sent into an ammonia refining working section to prepare liquid ammonia, after heat exchange is carried out on the bottom liquid of the deamination tower and the hot feed of the deacidification tower, the bottom liquid of the ammonia distillation tower is sent into a phenol recovery device after heat exchange is carried out on the bottom liquid of the ammonia distillation tower and the hot feed of the deacidification tower.
COD removal efficiency in the semi-coke wastewater subjected to deoiling, dedusting, deacidifying and deaminizing treatment can reach 32% -63%, oil content can be reduced from 1000-4000 mg/L to 10-50 mg/L, dust content can be controlled within 40mg/L, sulfide content can be reduced from 2000-6000 mg/L to 50mg/L, ammonia nitrogen content can be reduced from 2000-12000 mg/L to 50mg/L, and pH value of effluent water after deaminizing treatment is 6.5-7.0.
Further, the consumption of the strong acid in the step (1) is that the mass concentration of the free ammonia is reacted to 0 mg/L-2000 mg/L;
the gas dissolved amount of the gas source in the step (1) is 10kg CO 2 Water/t 45kg CO 2 Water at 0-70 deg.c and pressure of 0.2-0.6 MPa;
the strong acid of step (1) includes, but is not limited to, H 2 SO 4 、HCL；
The pH value of the step (1) is 5.0-8.0;
the standing time in the step (1) is 0.5-4 h;
the dissolved gas tank versions described in step (1) include, but are not limited to, fill tanks, high efficiency coalescers, cyclone separators, and in-tank tanks;
the air floatation residence time in the step (1) is more than 0.5h;
the stirring residence time of the fully stirred coagulation in the step (2) is more than 0.5h, and the settling and standing residence time is more than 1h;
the flocculant of step (2) includes, but is not limited to PAC, PAFC, PAM, APAM;
the residence time of the homogenizing tank in the step (3) is more than 5min;
the cold and hot feed ratio of the deacidification tower in the step (4) is 1:1-1:6;
the acid gas of step (4) includes, but is not limited to, CO 2 、H 2 S；
The operation pressure of the deacidification tower in the step (4) is normal pressure, the temperature of the tower top is 40-90 ℃, and the pressure of the tower bottom is 98-102 ℃;
the top segregation temperature of the deacidification tower in the step (4) is 40-70 ℃;
the alkali liquor in the step (5) comprises, but is not limited to, naOH solution and KOH solution;
the molar ratio of the consumption of the alkali liquor to the fixed ammonia in the inlet water in the step (5) is 1:1;
the operating pressure of the deamination tower in the step (5) is normal pressure, the extraction proportion is 2-5 wt%, the concentration of free ammonia in the tower bottom is controlled to be less than 50mg/L, the temperature of the tower top is 55-80 ℃, and the temperature of the tower bottom is 102-104 ℃.
Further, the acid gas source supplement in the step (1) is CO obtained from a low-temperature methanol washing section 2 Gas or H 2 S gas;
the wastewater obtained by the air floatation treatment in the step (1) is an acidic gas saturated aqueous solution;
the separated oil product in the step (1) is used as a product output system;
the oil sludge removed in the steps (2) and (3) is output to the system in the form of a filter cake after dehydration;
the acid gas in the step (4) is conveyed to untreated raw gas for desulfurization and decarbonization after being pressurized, or conveyed to a subsequent sulfur recovery unit in other forms;
the alkali liquor in the step (5) adopts fresh alkali liquor or adopts waste alkali liquor of an ammonia refining alkali washing unit to convert free ammonia in water;
and (5) absorbing ammonia gas by desalted water to prepare ammonia water or directly preparing liquid ammonia.
The device of the treatment method for deoiling, dedusting and deacidifying and deaminizing the semi-coke wastewater comprises a dissolved air pump, a dissolved air tank, an air floatation tank, a flocculation sedimentation tank, a double-medium filter, a homogenizing tank, a deacidification tower, an acid gas-liquid separator, an ammonia distillation tower and a sewage pump, wherein:
raw material wastewater is subjected to acid adding and pressurized gas dissolving, then is subjected to standing and layering in a gas dissolving tank, water outlet is connected with an inlet of an air floatation tank, gravity flow of water outlet of the air floatation tank enters an inlet of a flocculation tank, after mechanical stirring and precipitation, clear liquid at an outlet is connected with a lifting pump, a pump outlet is connected with a dual-medium filter, filtered wastewater is connected with a homogenizing tank, cold and hot wastewater is sent into the top and the middle of a deacidification tower, gas phase at the top of the tower is connected with an acid gas-liquid separator, water outlet at the bottom of the deacidification tower is lifted by the pump and then is connected with the upper part of a deamination tower, alkali liquor is connected onto an alkali liquor pipeline by a tee joint, extracted ammonia is connected with an ammonia refining and absorbing device, and water outlet of the deamination tower is lifted by the pump and then is connected with a subsequent extraction unit.
The flocculation sedimentation device comprises a flocculation sedimentation device of a flocculation sedimentation tank and a high-efficiency flocculation reactor;
the deacidification tower is a stripping tower with the theoretical stage number of 10-25, and comprises a reducing tower, a non-reducing tower, a packing tower and a plate tower;
the deamination tower is a stripping tower with the theoretical stage number of 8-20, and the tower top structure comprises, but is not limited to, a separator and a fractional condensation reflux device.
Compared with the prior art, the invention has the following advantages:
(1) The invention is developed aiming at the water quality characteristics of the semi-coke wastewater, effectively improves the removal efficiency of oil, dust, acid gas and ammonia nitrogen in the semi-coke wastewater, reduces the chromaticity and viscosity of the semi-coke wastewater entering a phenol recovery section, avoids the pollution blocking of medium-low temperature coal tar in the wastewater to a deacidification and deamination unit, enhances the long-period operation stability of a wastewater treatment device, reduces the equipment investment cost of the deacidification and deamination unit, provides a better extraction environment for an extraction and dephenolization unit, and provides CO 2 -H 2 SO 4 The acidification and dissolved air floatation coupling flocculation sedimentation is a necessary choice for efficiently removing the oil dust content in the semi-coke wastewater, and the normal pressure removal of acid gas and ammonia nitrogen and the recovery of byproducts not only greatly reduce the operation cost of pretreatment, but also improve the recycling efficiency and create better conditions for biochemical denitrification.
(2) The invention is realized by H 2 SO 4 Fixing partial free ammonia in water, and then passing through CO 2 The dissolved gas reduces the pH value of the wastewater, and through the electric neutralization between dissociated hydrogen ions and emulsified oil, the zeta potential is reduced, the oil drops are destabilized, and CO is used in the air floatation process 2 The adsorption of bubbles accelerates the aggregation and removal of emulsified oil, and under the condition of low pH value, flocculant is added to sweep and net capture residual oil dust, so that the residual oil dust is adsorbed and bridged, and separated from water, the recycling efficiency of medium-low temperature coal tar is greatly improved, and the oil dust content in treated effluent is reduced.
(3) The invention uses CO 2 -H 2 SO 4 The acidification dissolved air floatation coupling flocculation sedimentation, normal pressure deacidification and deamination, the COD removal efficiency in the wastewater can reach 32% -63%, and the oil content is from1000-4000 mg/L is reduced to 10-50 mg/L, the dust content can be controlled within 40mg/L, the sulfide content is reduced to within 50mg/L from 2000-6000 mg/L, the ammonia nitrogen content is reduced to within 50mg/L from 2000-12000 mg/L, and the pH value of effluent water after deamination treatment of the semi-coke wastewater is 6.5-7.0, thereby providing a better extraction environment for extraction dephenolization.
(4) The invention is suitable for the pretreatment of the semi-coke wastewater generated by low-temperature pyrolysis in industrial low-rank coal, has wide pollutant content range for treating the semi-coke wastewater, has little change on the operation conditions of process equipment corresponding to different concentrations of oil, dust, sulfide and ammonia nitrogen, has large operation elasticity, has little change on the basis of the existing semi-coke wastewater pretreatment flow, and is beneficial to the application in the semi-coke wastewater treatment field.
(5) The invention ensures the water outlet effect of the working section through the front-end efficient deoiling and dedusting, avoids the pollution and blockage of the phenol-ammonia recovery working section caused by oil and dust contained in the semi-coke wastewater, correspondingly improves the recycling efficiency of the wastewater and ensures the operation stability of the semi-coke wastewater; through normal pressure deacidification and deamination, the high-efficiency removal and recovery of the acid gas and ammonia nitrogen are realized, and the purity of the byproducts is improved.
Drawings
FIG. 1 is a block diagram of a semi-coke wastewater treatment process of the invention;
fig. 2 is a graph showing the microscopic morphology comparison of the semi-coke wastewater before and after deoiling and dedusting treatment according to the invention.
Detailed Description
The present invention will be described in further detail with reference to specific examples, but embodiments of the present invention are not limited thereto, and fig. 1 is a block diagram of a semi-coke wastewater treatment process according to the present invention.
Example 1
In order to solve the problem of oil, dust, acid gas and ammonia nitrogen removal efficiency in the existing semi-coke wastewater pretreatment process, the invention provides a treatment method for deoiling, dedusting, deacidifying and deaminizing, which is efficient and resource-efficient, stable and reliable in operation and free of pollution.
It should be noted that, in this embodiment, the air source of the air dissolving device is CO 2 Strong acid adopts H 2 SO 4 The strong alkali adopts NaOH, and the dissolved air tank adopts three-phase rotaryThe flow separation technology and the coalescence deoiling technology improve the separation speed of the process, reduce the sedimentation time and provide qualified and stable effluent quality for the subsequent working section.
Step one: carrying out preliminary separation on oil and dust components of the semi-coke wastewater to obtain clear liquid effluent of the floatation tank; waste water and compressed CO using static mixer 2 、H 2 SO 4 Mixing and homogenizing the solution to make the free ammonia content in water lower than 1000mg/L, treating in a three-phase cyclone separator under pressurized condition to separate heavy oil, light oil and water, delivering the oil product into underground oil tank output system, delivering the water discharge into the bottom of air floatation tank via releaser, and performing CO treatment 2 Air floatation treatment, scraping the upper layer oil product by a slag scraper, removing the lower layer oil product by inclined plate sedimentation, and sending the lower layer oil product into an underground oil tank together with CO 2 The gas is collected by the air bag and returned to the compressor, and the residence time of the floatation tank is set by combining the water quantity, the temperature and the dissolved air pressure, and the specific limitation is not adopted here.
Step two: the air-floating effluent flows into a coagulation tank by gravity, the coagulation tank is provided with a stirring device, a flocculating agent is pumped into the coagulation tank by a dosing device to react with emulsified oil in wastewater, the wastewater is fully mixed with a medicament through the turbulent flow effect of the stirring device, the flocculation sedimentation rate is improved, and the flocculating agent, emulsified oil drops and suspended matters are subjected to net capturing, rolling, electric neutralization and bridging effects, so that liquid-repellent solutes in the wastewater are rapidly removed; the coagulated waste water is sent into a sedimentation tank through a lifting pump to remove flocs and oil slick formed by coalescence in the water, and the discharged water flows through a storage pool to be buffered under the action of the lifting pump and then enters a double-medium filtering device.
Step three: the lifting pump is interlocked with the liquid level of the buffer storage pool, and the speed of the liquid entering the double-medium filter is controlled through the flow, so that the filtering effect of the double-medium filter is ensured; the wastewater still contains a small amount of oil and floccules, the double-medium filter is used as the last procedure of pretreatment deoiling and dedusting, and the wastewater can be sent into a homogenizing tank after the oil and dust contents (namely the oil content in the water is less than or equal to 50mg/L and the suspended matter content is less than or equal to 25 mg/L) in the wastewater reach corresponding qualified indexes, and the microcosmic appearance of the deoiling and dedusting treatment effect is shown in figure 2. The total phenol content in the wastewater comprises phenol oil, and the total phenol content is reduced after deoiling and dedusting treatment.
Step four: the waste water is fed into the deacidification tower by cold and hot feeding through a lifting pump, the hot feeding heat exchange material is not particularly limited, and the acid gas (comprising CO) in the semi-coke waste water is stripped and removed in the deacidification tower 2 And H 2 S) as an important means of acid gas removal, the acid gas content (CO 2 +H 2 S) is reduced to below 50mg/L, the acid gas discharged material is separated by fractional condensation and gas-liquid separation, the condensate is returned to the homogenizing tank, the acid gas is sent to a subsequent sulfur treatment device (including but not limited to non-desulfurized raw gas and a wet catalytic oxidation device), and the wastewater is sent to the deamination tower through a tower kettle lifting pump.
Step five: the NaOH solution is fully mixed with the semi-coke wastewater in a static mixer through a metering pump and is sent into a deamination tower, ammonia nitrogen in the wastewater is distilled off in the deamination tower, the residual amount of the ammonia nitrogen in the effluent is closely related to the adding amount of the NaOH solution and the steam amount of a reboiler, and the ammonia nitrogen (namely NH) in the wastewater is treated by the deamination tower 3 -N、NH 4 + The total N content is reduced to below 50mg/L, the ammonia gas at the top of the tower is condensed and refluxed at the top of the deamination tower through a separator, the ammonia gas is sent to a subsequent ammonia refining section (an ammonia purifying tower, an alkaline washing sedimentation tank and an ammonia absorption tower are arranged), and the treated effluent is sent to a subsequent phenol recovery device. The phenol recovery device may be physically extracted with a solvent such as MIBK or DIPE, or may be complex extracted with a solvent such as TBP, and is not limited thereto.
The CO used in the above examples 2 -H 2 SO 4 Acidification + three-phase cyclone separator + CO 2 The process flow of air flotation, coagulation sedimentation separation, double-medium filtration, deacidification tower and deamination tower effectively treats oil, dust, acid gas and ammonia nitrogen in the wastewater, and effectively recovers the treated wastewater, wherein the oil content of the wastewater is less than or equal to 50mg/L, the suspended matter content is less than or equal to 25mg/L, the acid gas content is less than or equal to 50mg/L, the ammonia nitrogen content is less than or equal to 50mg/L, a novel pretreatment process technology is provided for recycling the semi-coke wastewater, and a foundation is laid for the quality-classified utilization and green development of coal.
Example 2
On the basis of example 1, this example reduces H 2 SO 4 The consumption and adding a small amount of flocculating agent in the acidification process are used for strengthening the deoiling and dedusting efficiency of the air floatation, increasing the steam quantity of a reboiler of a deacidification tower, and improving the temperature of the top of the tower to 95 ℃ to realize the recycling treatment of the semi-coke wastewater oil, dust, acid gas and ammonia nitrogen, and the pretreatment method comprises the following steps:
step one: carrying out preliminary separation on oil and dust components of the semi-coke wastewater to obtain clear liquid effluent of the floatation tank; waste water and compressed CO using static mixer 2 、H 2 SO 4 Mixing the solution with flocculant, homogenizing to make free ammonia content in water not higher than 3000mg/L, treating in tank under pressure to separate heavy oil, light oil and water, feeding the oil product into dirty oil dewatering device, discharging water, and feeding the discharged water into bottom of air floatation tank to make CO treatment 2 Air floatation treatment, oil and dust removal from waste water under the action of flocculant, upper layer of floc scraping by slag scraper, lower layer of heavy floc settling and removing by sloping plate, and feeding into dirty oil dewatering device together with CO 2 The gas is collected by the gas bag and returned to CO 2 A compressor.
Step two: the air-floating effluent flows into a coagulation tank by gravity, the coagulation tank is provided with a stirring device, a flocculating agent is pumped into the coagulation tank by a dosing device (a metering pump) to react with emulsified oil in wastewater, the wastewater is fully mixed with a medicament through the turbulent flow effect of the stirring device, and the flocculating agent, emulsified oil drops, suspended matters, and the like are subjected to the effects of net capturing, rolling, electric neutralization, bridging and the like, so that liquid-repellent solutes in the wastewater are rapidly removed; the coagulated waste water is sent into a sedimentation tank through a lifting pump to remove flocs and oil slick formed by coalescence in the water, and the discharged water flows through a storage pool to be buffered under the action of the lifting pump and then enters a double-medium filtering device.
Step three: the lifting pump is interlocked with the liquid level of the buffer storage pool, and the speed of the liquid entering the double-medium filter is controlled through the flow, so that the filtering effect of the double-medium filter is ensured; the waste water still contains a small amount of oil and floccules, the double-medium filter can treat the oil and dust content (namely, the oil content in the water is less than or equal to 50mg/L and the suspended matter content is less than or equal to 25 mg/L) in the waste water to reach corresponding qualified indexes, and then the waste water is sent into a homogenizing tank, wherein the total phenol content in the waste water comprises phenol oil, and the total phenol content is reduced after deoiling and dedusting treatment.
Step four: the waste water is fed into the deacidification tower by cold and hot feeding through a lifting pump, the hot feeding heat exchange material is not particularly limited, and the acid gas (comprising CO) in the semi-coke waste water is stripped and removed in the deacidification tower 2 And H 2 S) as an important means for removing the acid gas, wherein the acid gas discharge material contains certain ammonia nitrogen and water vapor, after being cooled to below 60 ℃ and gas-liquid separation, the condensate is returned to a homogenizing tank, the acid gas is sent to a subsequent sulfur treatment device (including but not limited to non-desulfurized raw gas and a wet catalytic oxidation device), the acid gas content of a tower kettle is not limited, and the wastewater is sent to a deamination tower through a tower kettle lifting pump.
Step five: the NaOH solution is fully mixed with the semi-coke wastewater in a static mixer by a metering pump and is sent into a deamination tower, ammonia nitrogen in the wastewater is distilled off in the deamination tower, the residual amount of the ammonia nitrogen in the effluent is closely related to the adding amount of the NaOH solution and the steam amount of a reboiler, and the acid gas Content (CO) in the wastewater after being treated by the deamination tower 2 +H 2 S) is reduced to below 50mg/L, ammonia Nitrogen (NH) 3 -N、NH 4 + The total N content is reduced to below 50mg/L, the ammonia gas at the top of the tower is condensed and refluxed at the top of the deamination tower through a separator, the ammonia gas is sent to a subsequent ammonia refining section (an ammonia purifying tower, an alkaline washing sedimentation tank and an ammonia absorption tower are arranged), and the treated effluent is sent to a subsequent phenol recovery device. The phenol recovery device may be physically extracted with a solvent such as MIBK or DIPE, or may be complex extracted with a solvent such as TBP, and is not limited thereto.
Finally, it should be noted that: the above embodiments are only for illustrating the technical solution of the present invention, and are not limiting; although modifications or equivalent substitutions may be made to some of the technical features or aspects set forth in the foregoing embodiments, these modifications or substitutions do not depart from the spirit and scope of the method of the present invention in essence.
Claims (6)
1. A treatment method for deoiling, dedusting, deacidifying and deaminizing semi-coke wastewater is characterized by comprising the following steps: the device sequentially comprises an acidic gas pressurized dissolved air floatation device, a coagulation sedimentation device, a double-medium filtering device, a homogenizing tank, a deacidification tower and a deamination tower which are connected; the acid gas pressurization dissolved gas floatation device is connected to an underground oil tank, the coagulation sedimentation device and the double-medium filtering device are connected to a sludge dewatering device, the deacidification tower is connected to an acid gas-liquid separation device, and the deamination tower is connected to an ammonia refining and absorbing device through a separator; wherein:
(1) The input end of the acid gas pressurizing dissolved gas floatation device is connected with raw material semi-coke wastewater, a compressed acid gas source and a strong acid output end, the semi-coke wastewater is subjected to pH value adjustment by an acid strengthening device, partial free ammonia in water is fixed, the acidified semi-coke wastewater is dissolved into sufficient acid gas source in the wastewater by a dissolved gas pump, the pH value of the wastewater is further reduced, the wastewater is sent into a dissolved gas tank, the heavy oil and the light oil are separated by pressure stabilization and standing, the heavy oil, the light oil and the water are layered, the oil product is sent into an underground oil tank, the water is sent into the bottom of an air floatation tank by a releaser for air floatation treatment, upper-layer scum is scraped by a scum scraper, bottom oil sludge is precipitated by an inclined plate and then is collected into the underground oil tank together with scum, and the middle part is extracted into clear liquid of the air floatation tank, namely the semi-coke wastewater;
(2) The input end of the coagulation sedimentation device is connected with a gravity outflow port of an air floatation tank, air floatation water flows into the coagulation tank by gravity, the coagulation tank is provided with a stirring device, the semi-coke wastewater obtained in the step (1) and flocculating agent are fully stirred and coagulated, then the sedimentation tank is used for sedimentation to remove oil sludge, the top oil slick is scraped by an oil scraper, the bottom oil sludge is collected and dehydrated and then is sent out, and a clear liquid in the middle layer, namely the semi-coke wastewater, is extracted;
(3) The double-medium filtering device is used for treating the semi-coke wastewater obtained in the step (2), filtering suspended matters and flocs in the wastewater, sending the semi-coke wastewater after oil sludge is removed by a filter outlet into a homogenizing tank to supply the deacidification tower for feeding, and returning the wastewater generated by backwashing to a coagulation sedimentation device;
(4) The deacidification tower is connected with an outlet of a lifting pump behind the homogenizing tank, deacidifies the semi-coke wastewater obtained in the step (3), cold and hot semi-coke wastewater in the step (3) is sent to the top and the middle of the deacidification tower in a split manner, acid gas is extracted from the tower top, the acid gas generated after condensation and gas-liquid separation is sent to an acid gas-liquid separation device, condensate is returned to the homogenizing tank, and the semi-coke wastewater is sent to the deamination tower through a tower kettle lifting pump;
(5) The deamination tower carries out deamination treatment on the semi-coke wastewater obtained in the step (4), the semi-coke wastewater in the step (4) is mixed with alkali liquor through a pipeline mixer, fixed ammonia is converted into free ammonia, the free ammonia is pumped from the upper part of the deamination tower, ammonia-containing steam is condensed by a separator and then partially flows back into the tower, concentrated ammonia gas extracted from the top of the separator is prepared into dilute ammonia water through an ammonia refining and absorbing device or is sent into an ammonia refining working section to prepare liquid ammonia, and the bottom liquid of the ammonia still is sent into a phenol recovery device after heat exchange with the hot feed of the deacidification tower;
the consumption of the strong acid in the step (1) is that the mass concentration of the free ammonia is reacted to 0 mg/L-2000 mg/L;
the dissolved air amount of the acid gas source in the step (1) is 10kg CO 2 Water/t 45kg CO 2 Water at 0-70 deg.c and pressure of 0.2-0.6 MPa;
the strong acid of step (1) includes, but is not limited to, H 2 SO 4 、HCL；
The pH value of the step (1) is 5.0-8.0;
the standing time in the step (1) is 0.5-4 h;
the dissolved gas tank versions described in step (1) include, but are not limited to, fill tanks, high efficiency coalescers, cyclone separators, and in-tank tanks;
the air floatation residence time in the step (1) is more than 0.5h;
the stirring residence time of the fully stirred coagulation in the step (2) is more than 0.5h, and the settling and standing residence time is more than 1h;
the flocculant of step (2) includes, but is not limited to PAC, PAFC, PAM, APAM;
the residence time of the homogenizing tank in the step (3) is more than 5min;
the cold and hot feed ratio of the deacidification tower in the step (4) is 1:1-1:6;
the acid gas of step (4) includes, but is not limited to, CO 2 、H 2 S；
The operation pressure of the deacidification tower in the step (4) is normal pressure, the temperature of the tower top is 40-90 ℃, and the pressure of the tower bottom is 98-102 ℃;
the top segregation temperature of the deacidification tower in the step (4) is 40-70 ℃;
the alkali liquor in the step (5) comprises, but is not limited to, naOH solution and KOH solution;
the molar ratio of the consumption of the alkali liquor to the fixed ammonia in the inlet water in the step (5) is 1:1;
the operating pressure of the deamination tower in the step (5) is normal pressure, the extraction proportion is 2-5 wt%, the concentration of free ammonia in the tower bottom is controlled to be less than 50mg/L, the temperature of the tower top is 55-80 ℃, and the temperature of the tower bottom is 102-104 ℃.
2. The method for deoiling, dedusting, deacidifying and deaminizing the semi-coke wastewater according to claim 1, which is characterized by comprising the following steps:
the acid gas source in the step (1) is supplemented with CO from a low-temperature methanol washing section 2 Gas or H 2 S gas;
the wastewater obtained by the air floatation treatment in the step (1) is an acidic gas saturated aqueous solution;
the oil product separated in the step (1) is used as a product output system;
the oil sludge removed in the steps (2) and (3) is output to the system in the form of a filter cake after dehydration;
the acid gas in the step (4) is conveyed to untreated raw gas for desulfurization and decarbonization after being pressurized, or conveyed to a subsequent sulfur recovery unit in other forms;
the alkali liquor in the step (5) adopts fresh alkali liquor or adopts waste alkali liquor of an ammonia refining alkali washing unit to convert free ammonia in water;
and (5) absorbing ammonia gas by desalted water to prepare ammonia water or directly preparing liquid ammonia.
3. An apparatus for carrying out the method of any one of claims 1-2, characterized in that: including dissolved air pump, dissolved air tank, air supporting pond, coagulating sedimentation device, two medium filters, homogeneity jar, deacidification tower, acid gas-liquid separator, ammonia still, elevator pump, wherein:
raw material wastewater is subjected to acid adding and pressurized gas dissolving, then is subjected to standing and layering in a gas dissolving tank, water outlet is connected with an inlet of an air floatation tank, gravity flow of water outlet of the air floatation tank enters an inlet of a coagulating sedimentation device, after mechanical stirring and sedimentation, clear liquid at an outlet is connected with a lifting pump, a pump outlet is connected with a dual-medium filter, filtered wastewater is connected with a homogenizing tank, cold and hot wastewater is sent into the top and the middle of a deacidification tower, gas phase at the top of the tower is connected with an acid gas-liquid separator, water outlet at the bottom of the deacidification tower is lifted by the pump and then is connected with the upper part of a deamination tower, alkali liquor is connected onto an alkali liquor pipeline through a tee joint, extracted ammonia is connected with an ammonia refining and absorbing device, and water outlet of the deamination tower is lifted by the pump and then is connected with a subsequent extraction unit.
4. A device according to claim 3, characterized in that: the coagulation sedimentation device comprises, but is not limited to, a coagulation sedimentation tank and a coagulation sedimentation device of a high-efficiency coagulation reactor.
5. A device according to claim 3, characterized in that: the deacidification tower is a stripping tower with a theoretical stage number of 10-25 stages, including but not limited to a reducing tower, a non-reducing tower, a packed tower and a plate tower.
6. A device according to claim 3, characterized in that: the deamination tower is a stripping tower with the theoretical stage number of 8-20, and the tower top structure comprises, but is not limited to, a separator and a fractional condensation reflux device.
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