CN115196805A - Treatment method for deoiling, dedusting, deacidifying and deaminating semi-coke wastewater - Google Patents
Treatment method for deoiling, dedusting, deacidifying and deaminating semi-coke wastewater Download PDFInfo
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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
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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
- C02F1/24—Treatment of water, waste water, or sewage by flotation
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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
- C02F1/26—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
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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
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/16—Nitrogen compounds, e.g. ammonia
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Abstract
The invention belongs to the technical field of sewage treatment, and discloses a method for deoiling, dedusting, deacidifying and deaminating semi-coke wastewater. The method comprises the following steps: after part of free ammonia in the semi-coke wastewater is fixed by an acid adding device, the semi-coke wastewater is sent into a dissolved air floatation device by a lifting pump for wastewater air floatation treatment, generated floating slag is scraped by a slag scraper, bottom sludge is transported outside after being treated, effluent of the air floatation device is filtered and then flocculated and settled, and the floating slag and the sediment are collected in an oil sludge tank; and (3) delivering the clear liquid to a double-medium filtering device to filter residual flocs, delivering the filtrate to a homogenizing tank, pressurizing the outlet water of the homogenizing tank by a lifting pump, then delivering the outlet water of the homogenizing tank to the top and the middle of an acid removal tower in two ways, removing acid gas in the water, mixing the kettle liquid and alkali liquor, delivering the mixture to a deamination tower to evaporate ammonia nitrogen to prepare ammonia water, and delivering the treated wastewater to a phenol recovery device to further remove organic matters. According to the invention, the front end is used for efficiently deoiling and dedusting, so that the water outlet effect of the working section is ensured, the acid gas and ammonia nitrogen are efficiently removed and recovered by deacidifying and deaminating at normal pressure, and the purity of a byproduct is improved.
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 deaminating semi-coke wastewater.
Technical Field
The low-temperature dry distillation of the low-rank coal is a key technology for realizing quality-based grading utilization of the coal, and is widely applied to modern novel coal chemical engineering projects. The semi-coke wastewater is the gas washing wastewater of raw coke gas generated in the middle and low temperature dry distillation process of low-rank coal, is rich in middle and low temperature coal tar, suspended matters, sulfides, ammonia nitrogen, phenol and other difficultly-degradable pollutants, and has very complex raw water quality and great treatment difficulty. The method is a major bottleneck for restricting the quality-based grading utilization of coal and is also one of important factors for restricting the development of the quality-based grading utilization industry.
At present, the treatment process of oil and dust in semi-coke wastewater mainly comprises oil separation, air flotation, filtration, coarse granulation, flocculation precipitation and the like, while the treatment process of acid gas and ammonia nitrogen comprises ammonia distillation under normal pressure and pressure stripping, deacidification and deamination, and then phenolic substances are recovered by extraction, so that the content of the oil, dust, acid gas, ammonia nitrogen and total phenols in the wastewater is reduced, and the phenols, ammonia and sulfides in the wastewater are recovered to realize the recycling of special pollutants. Combining with a biochemical treatment system to achieve the purpose of treating the semi-coke wastewater. The oil and dust removal effect directly determines the running stability of the phenol-ammonia recovery system and the equipment fouling and plugging period, and the removal efficiency of acid gas and ammonia nitrogen is also the key for stable and efficient running of a 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 industry wastewater, the removal efficiency of oil, dust, sulfide and ammonia nitrogen is not enough to meet the requirement of a biochemical treatment system on the imported water quality index, the residual medium and low temperature coal tar, sulfide and ammonia nitrogen cause huge impact on a phenol ammonia recovery working section and a biochemical treatment working section, the quality of products for recycling the wastewater is not good, and the efficient and stable operation of the system is influenced. The prior semi-coke wastewater pretreatment process is characterized in that: (1) the oil dust removal residence time is long, and the occupied area of the equipment is large: part of oil exists in the wastewater in a stable emulsified oil form, the relative density is close to 1, and the natural settling or floating speed is slow; (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 distillation system along with ammonia condensate, and the concentration of the ammonia nitrogen of effluent is higher than 150mg/L under the pressurization condition; (3) residual oils plug the column internals, contaminate the extractant and crude phenol: the phenol-ammonia recovery system is blocked by residual oil and dust, and oil is discharged out of the system along with a crude phenol product in the solvent recovery process; (4) the pretreatment anti-blocking requirement is high, and the equipment investment cost is huge: the deoiling and dedusting process has long retention time of equipment, large theoretical plate number of a phenol ammonia recovery system and high operation pressure, and high-flux anti-blocking type patent tower internals are required, so that the investment of a pretreatment working section is huge, and the method is the actual difficulty and challenge faced by semi-coke wastewater treatment.
Disclosure of Invention
Aiming at the problems in the prior art, the invention aims to provide a treatment method for de-oiling, dedusting, deacidifying and deaminating semi-coke wastewater.
The purpose of the invention is realized by the following scheme:
a treatment method for deoiling, dedusting and deacidifying and deaminating semi-coke wastewater sequentially comprises a pressurized dissolved air flotation device, a coagulation sedimentation device, a double-medium filtering device, a homogenizing tank, a deacidification tower and a deamination tower which are connected; the pressure dissolved air flotation 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 acid removal tower is connected to an acid gas-liquid separation device, and the ammonia removal tower is connected to an ammonia refining and absorbing device through a dephlegmator; wherein:
(1) The input end of the pressurized dissolved air flotation device is connected with raw material semi-coke wastewater, a compressed acid gas source and a strong acid output end, the pH value of the semi-coke wastewater is adjusted by an acid strengthening device, part of free ammonia in water is fixed, the acidified semi-coke wastewater is dissolved into enough acid gas source 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 water are layered, the oil product is sent into an underground oil tank, the drainage is sent into the bottom of an air flotation tank by a releaser for air flotation treatment, the upper layer floating slag is scraped by a slag scraper, the bottom oil sludge is precipitated by an inclined plate and then is collected into the underground oil tank together with the floating slag, and clear liquid of the air flotation tank, namely the semi-coke wastewater is collected from the middle part;
(2) The input end of the coagulation sedimentation device is connected with a gravity outflow port of an air flotation tank, air flotation effluent flows into the coagulation tank by gravity, the coagulation tank is provided with a stirring device, semi-coke wastewater obtained in the step (1) is fully stirred and coagulated with a flocculating agent, then sedimentation is carried out by a sedimentation tank to remove oil sludge, top floating oil is scraped by an oil scraper, bottom oil sludge is collected and dehydrated and then is delivered outside, and clear liquid of a middle layer, namely semi-coke wastewater, is extracted;
(3) The double-medium filtering device is used for treating the semi-coke wastewater clear liquid obtained in the step (2) to filter suspended matters and flocs in the wastewater, the semi-coke wastewater after oil removal and dust removal is extracted from the outlet of the filter and is sent into a homogenizing tank to be fed to a deacidification tower, and the wastewater generated by backwashing is returned to a coagulation sedimentation device;
(4) The deacidification tower is connected with a homogenizing tank and then an outlet of a lifting pump is used for deacidifying the semi-coke wastewater obtained in the step (3), the semi-coke wastewater in the step (3) is sent to the top and the middle of the deacidification tower in two ways of cooling and heating, 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 sent back to the homogenizing tank, and the semi-coke wastewater is sent to a deamination tower through a tower kettle lifting pump;
(5) And (3) carrying out deamination treatment on the semi-coke wastewater obtained in the step (4) by the deamination tower, mixing the semi-coke wastewater in the step (4) with alkali liquor through a pipeline mixer, converting fixed ammonia into free ammonia, pumping the free ammonia from the upper part of the deamination tower, condensing ammonia-containing steam by a dephlegmator, then partially refluxing the condensed ammonia-containing steam into the tower, preparing concentrated ammonia gas from the top of the dephlegmator into dilute ammonia water by an absorption device or sending the diluted ammonia gas into an ammonia refining section to prepare liquid ammonia, carrying out heat exchange on the deamination tower kettle liquid and thermal feed of an acid removal tower, carrying out heat exchange on the ammonia distillation tower kettle liquid and the thermal feed of the acid removal tower, and then sending the ammonia distillation tower kettle liquid into a phenol recovery device.
The COD removal efficiency of the semi-coke wastewater after the oil removal, dust removal, deacidification and deamination treatment can reach 32-63 percent, the oil content is reduced to 10-50 mg/L from 1000-4000 mg/L, the dust content can be controlled within 40mg/L, the sulfide content is reduced to 50mg/L from 2000-6000 mg/L, the ammonia nitrogen content is reduced to 50mg/L from 2000-12000 mg/L, and the pH value of the effluent after the semi-coke wastewater is subjected to the deamination 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 source in the step (1) has the gas content of 10kg CO 2 Water/t 45kg CO 2 Water/t, the temperature is 0-70 ℃, and the pressure is 0.2-0.6 MPa;
the strong acid in step (1) includes but is not limited to H 2 SO 4 、HCL；
The pH value in the step (1) is 5.0-8.0;
the standing time in the step (1) is 0.5-4 h;
the dissolved air tank type in the step (1) comprises but is not limited to a filling tank, a high-efficiency coalescer, a cyclone separator and a tank-in-tank;
the air floatation retention time in the step (1) is more than 0.5h;
the stirring residence time of the full stirring coagulation in the step (2) is more than 0.5h, and the settling standing residence time is more than 1h;
flocculants in the step (2) include but are not limited to PAC, PAFC, PAM and APAM;
the residence time of the homogenizing tank in the step (3) is more than 5min;
the cold-hot feeding ratio of the deacidification tower in the step (4) is 1-1;
the acid gas in 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 kettle 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) includes but is not limited to NaOH solution and KOH solution;
the mol ratio of the alkali liquor consumption in the step (5) to the fixed ammonia in the inlet water is 1;
the operation pressure of the deamination tower in the step (5) is normal pressure, the extraction proportion is 2wt% -5 wt%, the concentration of free ammonia in a tower kettle is controlled to be less than 50mg/L, the temperature of the top of the tower is 55-80 ℃, and the temperature of the bottom of the tower is 102-104 ℃.
Further, the acid gas source supplement in step (1) is CO taken from the low-temperature methanol washing section 2 Gas or H 2 S gas;
the wastewater obtained by the air flotation treatment in the step (1) is an acid gas saturated aqueous solution;
the separated oil product in the step (1) is used as a product output system;
the oil sludge removal in the steps (2) and (3) is output to a system in a filter cake form after dehydration;
pressurizing the acid gas in the step (4), and then conveying the acid gas into untreated raw coke oven gas for desulfurization and decarburization, or conveying the acid gas to a subsequent sulfur recovery unit in other forms;
adopting fresh alkali liquor as the alkali liquor in the step (5), or adopting waste alkali liquor of an ammonia refining alkali washing unit to convert free ammonia in water;
and (5) absorbing the ammonia gas by desalted water to prepare ammonia water, or directly preparing liquid ammonia.
The device for the treatment method of the deoiling, dedusting, deacidification and deamination of the semi-coke wastewater comprises a dissolved air pump, a dissolved air tank, an air flotation tank, a flocculation sedimentation tank, a double-medium filter, a homogenizing tank, a deacidification tower, an acidic gas-liquid separator, an ammonia still and a sewage pump, wherein:
raw material wastewater is subjected to acidification and pressurization for gas dissolution and then is placed in a dissolved gas tank for layering, the effluent is connected with an inlet of an air flotation tank, the effluent of the air flotation tank enters an inlet of a flocculation tank in a gravity flow mode, the effluent is mechanically stirred and precipitated, the clear effluent is connected with a lift pump, an outlet of the pump is connected with a double-medium filter, the filtered wastewater is connected with a homogenizing tank, the wastewater is cooled and heated in two ways and is sent to the top and the middle of a deacidification tower, the gas at the top of the deacidification tower is connected with an acid gas-liquid separator, the effluent at the bottom of the deacidification tower is lifted by the pump and then connected with the upper part of a deamination tower, alkali liquor is connected onto an alkali liquor pipeline through a tee joint, the extracted ammonia is connected with an ammonia refining and absorbing device, and the effluent of the deamination tower is lifted by the pump and then connected with a subsequent extraction unit.
The flocculation and sedimentation device comprises a flocculation and sedimentation tank and flocculation and sedimentation equipment of a high-efficiency flocculation reactor;
the deacidification tower is a stripping tower with 10-25 theoretical stages, and comprises but is not limited to a reducing tower, a non-reducing tower, a packed 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 dephlegmator and a dephlegmator reflux device.
Compared with the prior art, the invention has the following advantages and beneficial effects:
(1) The method 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 chroma and viscosity of the semi-coke wastewater entering a phenol recovery section, avoids the pollution and blockage of medium and low temperature coal tar in the wastewater on a deacidification deamination unit, enhances the long-period running stability of a wastewater treatment device, reduces the equipment investment cost of the deacidification deamination unit, provides a better extraction environment for an extraction dephenolization unit, and provides CO 2 -H 2 SO 4 The acidification dissolved air flotation coupled flocculation sedimentation is the inevitable choice for efficiently removing the oil dust content in the semi-coke wastewater, and the removal of the acid gas and the ammonia nitrogen at normal pressure 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 through H 2 SO 4 Fixing part of free ammonia in water, passing through CO 2 Dissolving gas to reduce pH value of waste water, making the dissociated hydrogen ions and emulsified oil produce electric neutralization reaction so as to reduce zeta potential and make oil drop destabilize, in the course of air-floatation, making CO pass through 2 Accelerating the aggregation and removal of emulsified oil by the adsorption of air bubbles, and adding a flocculating agent to roll up and sweep the residual oil dust under the condition of low pH valueThe bridge is caught and adsorbed, so that the bridge is separated from the water, the recycling efficiency of the medium and low temperature coal tar is greatly improved, and the oil dust content in the treated water is reduced.
(3) The invention passes CO 2 -H 2 SO 4 Acidifying dissolved air flotation coupling flocculation sedimentation, deacidifying and deaminating at normal pressure, wherein the COD removal efficiency in the wastewater can reach 32-63%, the oil content is reduced to 10-50 mg/L from 1000-4000 mg/L, the dust content can be controlled to be within 40mg/L, the sulfide content is reduced to be within 50mg/L from 2000-6000 mg/L, the ammonia nitrogen content is reduced to be within 50mg/L from 2000-12000 mg/L, the pH value of the effluent of semi-coke wastewater subjected to deamination is 6.5-7.0, and a better extraction environment is provided for extraction dephenolization.
(4) The semi-coke wastewater pretreatment method is suitable for pretreatment of semi-coke wastewater generated by low-temperature pyrolysis of industrial low-rank coal, has wide content range of pollutants in the treatable semi-coke wastewater, has little change of process equipment operation conditions corresponding to different oil, dust, sulfide and ammonia nitrogen concentrations, has large operation flexibility, has little change on the basis of the existing semi-coke wastewater pretreatment process, and is beneficial to application of the semi-coke wastewater pretreatment method in the field of semi-coke wastewater treatment.
(5) According to the semi-coke waste water treatment system, the front end is used for efficiently deoiling and dedusting, so that the water outlet effect of the workshop section is ensured, the pollution and blockage of oil and dust contained in semi-coke waste water to the phenol ammonia recovery workshop section are avoided, the waste water recycling efficiency is correspondingly improved, and the operation stability is ensured; the high-efficiency removal and recovery of acid gas and ammonia nitrogen are realized by normal-pressure deacidification and deamination, and the purity of byproducts is improved.
Drawings
FIG. 1 is a block diagram of a semi-coke wastewater treatment process according to the present invention;
FIG. 2 is a comparison graph of the micro-morphology of semi-coke wastewater before and after de-oiling and de-dusting treatment.
Detailed Description
The present invention will be described in further detail with reference to specific examples, but the 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 the removal efficiency of oil, dust, acid gas and ammonia nitrogen in the existing semi-coke wastewater pretreatment process, the invention provides a treatment method for deoiling, dedusting, deacidifying and deaminating, which is efficient in recycling, stable and reliable in operation and free of pollution.
It should be noted that, in this embodiment, the gas source of the gas dissolving device is CO 2 The strong acid is H 2 SO 4 The strong base adopts NaOH, the dissolved air tank adopts a three-phase cyclone separation technology and a coalescence oil removal technology, the separation speed of the process is improved, the settling time is reduced, and qualified and stable effluent quality is provided for the subsequent working section.
The method comprises the following steps: carrying out primary separation on oil and dust components of semi-coke wastewater to obtain clear liquid effluent of an air flotation tank; waste water and compressed CO are mixed by a static mixer 2 、H 2 SO 4 Mixing and homogenizing the solution to make the content of free ammonia in water lower than 1000mg/L, treating in a three-phase cyclone separator under the condition of pressurization to separate heavy oil, light oil and water, delivering the oil product into an underground oil tank output system, delivering the discharged water into the bottom of an air floatation tank through a releaser, and carrying out CO treatment on the discharged water 2 Air floating treatment, scraping the upper layer oil product by a slag scraper, removing the lower layer oil product by inclined plate sedimentation, sending into an underground oil tank together, and introducing CO 2 The gas is collected by the air bag and sent back to the compressor, and the retention time of the air floatation tank needs to be set by combining water quantity, temperature and dissolved gas pressure, which is not limited in detail here.
Step two: the air-floated effluent flows into a coagulation tank by gravity, a stirring device is arranged in the coagulation tank, a flocculating agent is pumped into the coagulation tank by a dosing device to react with emulsified oil in the wastewater, the wastewater and a medicament are fully mixed under the turbulent flow action of the stirring device, the flocculation sedimentation rate is improved, and the flocculating agent, emulsified oil drops and suspended matters are subjected to net catching, rolling, electric neutralization and bridging actions, so that lyophobic solutes in the wastewater are quickly removed; the coagulated wastewater is sent into a settling tank by a lifting pump to remove flocs and oil slick formed by coalescence, and the effluent gravity flows through a storage tank for buffering and then enters a double-medium filtering device under the action of the lifting pump.
Step three: the lifting pump is interlocked with the liquid level of the buffer storage tank, and the speed of the lifting pump entering the double-medium filter is controlled by 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 working procedure of the pretreatment, deoiling and dedusting, the oil and dust content (namely the oil content in the wastewater 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 can reach corresponding qualified indexes and then is sent into a homogenizing tank, and the micro-morphology of the deoiling and dedusting treatment effect is shown in figure 2. It is noted that the total phenol content in the wastewater comprises phenol oil, and the total phenol content is reduced after the treatment of deoiling and dedusting.
Step four: the wastewater is sent into a deacidification tower by cold and hot feed of a lift pump, the hot feed heat exchange material is not particularly limited, and acid gas (including CO) in the semi-coke wastewater is stripped and removed in the deacidification tower 2 And H 2 S) as an important means for acid gas removal, where the acid gas Content (CO) can be reduced 2 +H 2 S) is reduced to below 50mg/L, the acid gas is discharged, after fractional condensation 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), and the wastewater is sent to a deamination tower through a tower kettle lifting pump.
Step five: naOH solution is fully mixed with semi-coke wastewater in a static mixer through a metering pump and is sent into a deamination tower, ammonia nitrogen in the wastewater is evaporated in the deamination tower, the residual amount of the ammonia nitrogen in effluent is closely related to the addition amount of the NaOH solution and the steam amount of a reboiler, and the ammonia nitrogen (namely NH) in the wastewater after the treatment of the deamination tower 3 -N、NH 4 + -N total amount) content is reduced to below 50mg/L, ammonia gas at the top of the tower is condensed and refluxed to the top of the deamination tower through a dephlegmator, the ammonia gas is sent to a subsequent ammonia refining section (an ammonia purification tower, an alkaline washing settling tank and an ammonia absorption tower are arranged), and treated effluent is sent to a subsequent phenol recovery device. The phenol recovery device can perform physical extraction by using solvents such as MIBK and DIPE, and can also perform complex extraction by using solvents such as TBP, and the device is not limited herein.
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, effectively recovers the oil-containing wastewaterThe amount is less than or equal to 50mg/L, the content of suspended matters is less than or equal to 25mg/L, the content of acid gas is less than or equal to 50mg/L, and the content of ammonia nitrogen is less than or equal to 50mg/L, so that a novel pretreatment process technology is provided for the resource treatment of semi-coke wastewater, and a foundation is laid for the green development of quality-based graded utilization of coal.
Example 2
On the basis of embodiment 1, the embodiment reduces H 2 SO 4 Consumption and adding a small amount of flocculant in the acidification process to strengthen the air flotation deoiling and dedusting efficiency, increasing the steam quantity of a reboiler of a deacidification tower, and raising the temperature of the tower top to 95 ℃ to realize the resource treatment of semi-coke wastewater oil, dust, acid gas and ammonia nitrogen, wherein the pretreatment method comprises the following steps:
the method comprises the following steps: carrying out primary separation on oil and dust components of semi-coke wastewater to obtain clear liquid effluent of an air flotation tank; waste water and compressed CO are mixed by a static mixer 2 、H 2 SO 4 Mixing the solution and flocculant to homogenize, making the content of free ammonia in water not higher than 3000mg/L, under the condition of pressurization making treatment in tank-in-tank to make heavy oil, light oil and water be separated into layers, feeding the oil product into dirty oil dewatering device, discharging water and feeding it into the bottom portion of air-floatation tank through releaser to make it undergo the process of CO treatment 2 Air floating treatment, removing oil and dust from wastewater under the action of flocculant, scraping the upper layer floc by a residue scraper, removing the lower layer heavy floc by inclined plate sedimentation, and sending into a dirty oil dehydration device together with CO 2 The gas is collected by the air bag and returned to CO 2 A compressor.
Step two: the air-floated 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 (metering pump) to react with emulsified oil in the wastewater, the wastewater and a medicament are fully mixed under the turbulent flow action of the stirring device, and the flocculating agent, emulsified oil drops and suspended matters are subjected to net catching, coiling, sweeping, electric neutralization, bridging and other actions, so that lyophobic solute in the wastewater is quickly removed; the coagulated wastewater is sent into a settling tank through a lifting pump to remove flocs in water and floating oil formed by coalescence, and the effluent gravity flows through a storage tank to be buffered and then enters a double-medium filtering device under the action of the lifting pump.
Step three: the lifting pump is interlocked with the liquid level of the buffer storage tank, and the speed of the lifting pump entering the double-medium filter is controlled by 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 dual-medium filter can process 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 the corresponding qualified index and then send the treated waste water into the homogenizing tank, and the total phenol content in the waste water comprises phenol oil, and the total phenol content is reduced after de-oiling and de-dusting treatment.
Step four: the wastewater is sent into a deacidification tower by cold and hot feed of a lift pump, the hot feed heat exchange material is not particularly limited, and acid gas (including CO) in the semi-coke wastewater 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 is discharged with certain ammonia nitrogen and water vapor, the acid gas is cooled to below 60 ℃, gas-liquid separation is carried out, 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 content of the acid gas in a tower kettle is not limited, and wastewater is sent to a deamination tower through a tower kettle lifting pump.
Step five: the NaOH solution is fully mixed with semi-coke wastewater in a static mixer by a metering pump and sent into a deamination tower, ammonia nitrogen in the wastewater is evaporated in the deamination tower, the residual amount of the ammonia nitrogen in 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 treated by the deamination tower 2 +H 2 S) is reduced to below 50mg/L, ammonia nitrogen (namely NH) 3 -N、NH 4 + -N total amount) content is reduced to below 50mg/L, ammonia gas at the top of the tower is condensed and refluxed to the top of the deamination tower through a dephlegmator, the ammonia gas is sent to a subsequent ammonia refining section (an ammonia purification tower, an alkaline washing settling tank and an ammonia absorption tower are arranged), and treated effluent is sent to a subsequent phenol recovery device. The phenol recovery device can perform physical extraction by using solvents such as MIBK and DIPE, and can also perform complex extraction by using solvents such as TBP, and the device is not limited herein.
Finally, it should be noted that: the above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although modifications or equivalent substitutions may be made in the technical solutions or parts of the technical features set forth in the foregoing embodiments, these modifications or substitutions do not make the essence of the corresponding technical solutions depart from the spirit and scope of the method of the present invention.
Claims (7)
1. A treatment method for deoiling, dedusting, deacidifying and deaminating semi-coke wastewater is characterized by comprising the following steps: the device sequentially comprises an acid gas pressurization dissolved gas flotation device, a coagulation sedimentation device, a double-medium filtering device, a homogenizing tank, an acid removal tower and a deamination tower which are connected; the pressure dissolved air flotation 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 acid removal tower is connected to an acid gas-liquid separation device, and the ammonia removal tower is connected to an ammonia refining and absorbing device through a dephlegmator; wherein:
(1) The input end of the pressurized dissolved air flotation device is connected with raw material semi-coke wastewater, a compressed acid gas source and a strong acid output end, the pH value of the semi-coke wastewater is adjusted by an acid strengthening device, part of free ammonia in water is fixed, the acidified semi-coke wastewater is dissolved into enough acid gas source 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 water are layered, the oil product is sent into an underground oil tank, the drainage is sent into the bottom of an air flotation tank by a releaser for air flotation treatment, the upper layer floating slag is scraped by a slag scraper, the bottom oil sludge is precipitated by an inclined plate and then is collected into the underground oil tank together with the floating slag, and clear liquid of the air flotation tank, namely the semi-coke wastewater is collected from the middle part;
(2) The input end of the coagulation sedimentation device is connected with a gravity outflow port of the air flotation tank, air flotation effluent flows into the coagulation tank by gravity, the coagulation tank is provided with a stirring device, semi-coke wastewater obtained in the step (1) is fully stirred and coagulated with a flocculating agent, then sedimentation is carried out in a sedimentation tank to remove oil sludge, top floating oil is scraped by an oil scraper, bottom oil sludge is collected and dehydrated and then is sent out, and clear liquid of the middle layer, namely semi-coke wastewater, is collected;
(3) The semi-coke wastewater obtained in the step (2) is treated by the double-medium filtering device, suspended matters and flocs in the wastewater are filtered, the semi-coke wastewater after oil sludge removal is extracted from the outlet of the filter and is sent into a homogenizing tank to be fed to an acid removal tower, and the wastewater generated by backwashing returns to a coagulation sedimentation device;
(4) The deacidification tower is connected with a homogenizing tank and then is provided with an outlet of a lifting pump, deacidification treatment is carried out on the semi-coke wastewater obtained in the step (3), the semi-coke wastewater in the step (3) is divided into two parts of cold and hot, the two parts are sent to the top and the middle of the deacidification tower, acid gas is extracted from the top of the tower, the acid gas generated after condensation and gas-liquid separation is sent to an acid gas-liquid separation device, condensate is sent back to the homogenizing tank, and the semi-coke wastewater is sent to the deamination tower through a tower kettle lifting pump;
(5) And (3) carrying out deamination treatment on the semi-coke wastewater obtained in the step (4) by the deamination tower, mixing the semi-coke wastewater in the step (4) with alkali liquor through a pipeline mixer, converting fixed ammonia into free ammonia, pumping the free ammonia from the upper part of the deamination tower, condensing ammonia-containing steam by a dephlegmator, then partially refluxing the condensed ammonia-containing steam into the tower, refining concentrated ammonia gas from the top of the dephlegmator into dilute ammonia water by an ammonia refining and absorbing device or sending the diluted ammonia water into an ammonia refining section to prepare liquid ammonia, and sending the ammonia-evaporating tower kettle liquid into a phenol recovery device after heat exchange with hot feed of the deacidification tower.
2. The method for deoiling, dedusting, deacidifying and deaminating semi-coke wastewater according to claim 1, which is characterized in that:
the consumption of the strong acid in the step (1) is to react the mass concentration of the free ammonia to 0 mg/L-2000 mg/L;
the gas content of the acid gas source in the step (1) is 10kg of CO 2 Per t water 45kg CO 2 Water/t, the temperature is 0-70 ℃, and the pressure is 0.2-0.6 MPa;
the strong acid in step (1) includes but is not limited to H 2 SO 4 、HCL；
The pH value in the step (1) is 5.0-8.0;
the standing time in the step (1) is 0.5-4 h;
the dissolved air tank type in the step (1) comprises but is not limited to a filling tank, a high-efficiency coalescer, a cyclone separator and a tank-in-tank;
the air floatation retention time of the step (1) is more than 0.5h;
the stirring residence time of the full stirring coagulation in the step (2) is more than 0.5h, and the settling standing residence time is more than 1h;
the flocculant in the step (2) comprises but is not limited to PAC, PAFC, PAM and APAM;
the residence time of the homogenizing tank in the step (3) is more than 5min;
the cold-hot feeding ratio of the deacidification tower in the step (4) is 1-1;
the acid gas in step (4) includes but is not limited to CO 2 、H 2 S；
The operating 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 kettle 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) includes but is not limited to NaOH solution and KOH solution;
the mol ratio of the alkali liquor consumption in the step (5) to the fixed ammonia in the inlet water is 1;
the operation pressure of the deamination tower in the step (5) is normal pressure, the extraction proportion is 2wt% -5 wt%, the concentration of free ammonia in a tower kettle is controlled to be less than 50mg/L, the temperature of the top of the tower is 55-80 ℃, and the temperature of the bottom of the tower is 102-104 ℃.
3. The method for deoiling, dedusting, deacidifying and deaminating semi-coke wastewater according to claim 2, which is characterized by comprising the following steps of:
the acid gas source supplement in the step (1) is CO taken 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 acid gas saturated aqueous solution;
the separated oil product in the step (1) is used as a product output system;
the oil sludge removal in the steps (2) and (3) is output to a system in a filter cake form after dehydration;
pressurizing the acid gas in the step (4), and then conveying the acid gas into untreated raw coke oven gas for desulfurization and decarburization, or conveying the acid gas to a subsequent sulfur recovery unit in other forms;
adopting fresh alkali liquor as the alkali liquor in the step (5), or adopting waste alkali liquor of an ammonia refining alkali washing unit to convert free ammonia in water;
and (5) absorbing the ammonia gas by desalted water to prepare ammonia water, or directly preparing liquid ammonia.
4. A device for carrying out the method according to any one of claims 1 to 3, characterized in that: including dissolved air pump, dissolved air jar, air supporting pond, coagulating sedimentation pond, two medium filter, homogeneity jar, deacidification tower, acid gas vapour and liquid separator, ammonia still, sewage pump, wherein:
raw material wastewater is subjected to acidification and pressurization to dissolve gas and then is subjected to standing and layering in a dissolved gas tank, the effluent is connected with an inlet of an air flotation tank, the effluent gravity flow of the air flotation tank enters an inlet of a coagulation sedimentation tank, the effluent is subjected to mechanical stirring and sedimentation, the clear effluent is connected with a lift pump, the outlet of the pump is connected with a double-medium filter, the filtered wastewater is connected with a homogenizing tank, the wastewater is subjected to cold separation and hot separation and is sent to the top and the middle of a deacidification tower, the gas at the top of the deacidification tower is connected with an acidic gas-liquid separator, the effluent at the bottom of the deacidification tower is lifted by a pump and is connected with the upper part of the deamination tower, alkali liquor is connected to an alkali liquor pipeline by a tee joint, the extracted ammonia is connected with an ammonia refining and absorbing device, and the effluent of the deamination tower is lifted by the pump and is connected with a subsequent extraction unit.
5. The apparatus of claim 4, wherein: the flocculation and sedimentation device comprises a flocculation and sedimentation tank and flocculation and sedimentation equipment of a high-efficiency flocculation reactor.
6. The apparatus of claim 4, wherein: the deacidification tower is a stripping tower with 10-25 theoretical stages, and comprises but is not limited to a reducing tower, a non-reducing tower, a packed tower and a plate tower.
7. The apparatus of claim 4, wherein: 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 dephlegmator and a dephlegmator reflux device.
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