CN112624466A - Coal chemical industry wastewater pretreatment method - Google Patents
Coal chemical industry wastewater pretreatment method Download PDFInfo
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- 239000002351 wastewater Substances 0.000 title claims abstract description 163
- 239000000126 substance Substances 0.000 title claims abstract description 41
- 239000003245 coal Substances 0.000 title claims abstract description 39
- 238000002203 pretreatment Methods 0.000 title claims abstract description 17
- 239000003921 oil Substances 0.000 claims abstract description 109
- 238000000605 extraction Methods 0.000 claims abstract description 80
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 claims abstract description 79
- 230000009615 deamination Effects 0.000 claims abstract description 61
- 238000006481 deamination reaction Methods 0.000 claims abstract description 61
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 44
- 239000002904 solvent Substances 0.000 claims abstract description 36
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 32
- 238000011084 recovery Methods 0.000 claims abstract description 32
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- 239000000295 fuel oil Substances 0.000 claims abstract description 20
- 239000008213 purified water Substances 0.000 claims abstract description 8
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- 238000009835 boiling Methods 0.000 claims description 10
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- 238000010992 reflux Methods 0.000 claims description 7
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- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 4
- ZAFNJMIOTHYJRJ-UHFFFAOYSA-N Diisopropyl ether Chemical compound CC(C)OC(C)C ZAFNJMIOTHYJRJ-UHFFFAOYSA-N 0.000 claims description 4
- NTIZESTWPVYFNL-UHFFFAOYSA-N Methyl isobutyl ketone Chemical compound CC(C)CC(C)=O NTIZESTWPVYFNL-UHFFFAOYSA-N 0.000 claims description 4
- UIHCLUNTQKBZGK-UHFFFAOYSA-N Methyl isobutyl ketone Natural products CCC(C)C(C)=O UIHCLUNTQKBZGK-UHFFFAOYSA-N 0.000 claims description 4
- 230000008929 regeneration Effects 0.000 claims description 4
- 238000011069 regeneration method Methods 0.000 claims description 4
- 239000006004 Quartz sand Substances 0.000 claims description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 3
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- 150000001875 compounds Chemical class 0.000 claims description 2
- 238000009833 condensation Methods 0.000 claims description 2
- 230000005494 condensation Effects 0.000 claims description 2
- 150000002576 ketones Chemical class 0.000 claims description 2
- 229910021529 ammonia Inorganic materials 0.000 abstract description 10
- 238000004065 wastewater treatment Methods 0.000 abstract description 5
- 230000002349 favourable effect Effects 0.000 abstract 1
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- XKMRRTOUMJRJIA-UHFFFAOYSA-N ammonia nh3 Chemical compound N.N XKMRRTOUMJRJIA-UHFFFAOYSA-N 0.000 description 4
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- 238000002360 preparation method Methods 0.000 description 3
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- 238000010586 diagram Methods 0.000 description 2
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- 238000000197 pyrolysis Methods 0.000 description 2
- 239000002893 slag Substances 0.000 description 2
- 239000004912 1,5-cyclooctadiene Substances 0.000 description 1
- CDAWCLOXVUBKRW-UHFFFAOYSA-N 2-aminophenol Chemical compound NC1=CC=CC=C1O CDAWCLOXVUBKRW-UHFFFAOYSA-N 0.000 description 1
- QTWJRLJHJPIABL-UHFFFAOYSA-N 2-methylphenol;3-methylphenol;4-methylphenol Chemical compound CC1=CC=C(O)C=C1.CC1=CC=CC(O)=C1.CC1=CC=CC=C1O QTWJRLJHJPIABL-UHFFFAOYSA-N 0.000 description 1
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- 238000004380 ashing Methods 0.000 description 1
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- 229930003836 cresol Natural products 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000005188 flotation Methods 0.000 description 1
- -1 gasification Chemical compound 0.000 description 1
- 239000002920 hazardous waste Substances 0.000 description 1
- 239000010842 industrial wastewater Substances 0.000 description 1
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- 238000012986 modification Methods 0.000 description 1
- 229910000069 nitrogen hydride Inorganic materials 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 239000002910 solid waste Substances 0.000 description 1
- 239000011273 tar residue Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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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
-
- 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
- C02F1/02—Treatment of water, waste water, or sewage by heating
- C02F1/04—Treatment of water, waste water, or sewage by heating by distillation or evaporation
-
- 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
-
- 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
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/285—Treatment of water, waste water, or sewage by sorption using synthetic organic sorbents
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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
- C02F1/66—Treatment of water, waste water, or sewage by neutralisation; pH adjustment
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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
-
- 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
- C02F2101/30—Organic compounds
- C02F2101/34—Organic compounds containing oxygen
- C02F2101/345—Phenols
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Abstract
The invention discloses a coal chemical industry wastewater pretreatment method, which belongs to the technical field of coal chemical industry wastewater treatment and comprises the following steps: oil removal and solid removal, pre-deoiling, deacidification and deamination, extraction and dephenolization, solvent/phenol recovery and deep dephenolization. The pretreatment method of the coal chemical industry wastewater removes heavy oil, light oil, oil residue, ammonia, acid components and phenol in the wastewater, lightens the operation load of a subsequent biochemical treatment section, and creates favorable conditions for the biochemical treatment of the wastewater; before deacidification and deamination, floating oil, dispersed oil, emulsified oil and dissolved oil in the wastewater are removed in advance, so that the problem of fouling of a deacidification and deamination system is solved; the phenol content of the pretreated purified water is further reduced by setting deep dephenolization, and the shock resistance of a subsequent biochemical treatment section is improved; the recovered heavy oil, light oil, oil residue, acid gas, crude ammonia gas and crude phenol are taken as products to be delivered, so that the resource treatment and the comprehensive utilization of the coal chemical industry wastewater are realized.
Description
Technical Field
The invention relates to a pretreatment method of coal chemical industry wastewater, belonging to the technical field of coal chemical industry wastewater treatment.
Background
The coal chemical industry wastewater refers to industrial wastewater generated in the processes of coal coking, dry distillation, gasification and the like, and is generally brown or brown, has the pH value of 7-10 and is alkaline. The coal chemical industry wastewater has complex composition, and is industrial organic wastewater which is high in oil, COD, ammonia nitrogen and phenol value and difficult to treat. Oil, phenol and ammonia carried in waste waterLow boiling point hydrocarbons, H2S and CO2And the like, and solid suspended matters such as oil residue and the like are required to be removed by pretreatment before the biochemical treatment of the wastewater. The oil carried in the wastewater is mainly floating oil, dispersed oil, emulsified oil and tar in the form of dissolved oil, and comprises light oil with the specific gravity of 0.96-0.98 and heavy oil with the specific gravity of 1.02-1.04; the oil residue is mainly tar residue and belongs to hazardous waste; the phenol includes phenol with an atmospheric boiling point of 182 ℃, cresol with an atmospheric boiling point of 200 ℃, dihydric phenol with an atmospheric boiling point of 280-290 ℃ and polyhydric phenol with a higher boiling point.
At present, the industry generally adopts a pretreatment process route of oil removal, deacidification and deamination, extraction dephenolization and solvent recovery by an oil separation tank and an air flotation tank, and finally carries out biochemical treatment. However, from the practical operation of industrial devices, the effect is not ideal: the front end has poor oil removal effect, the deacidification, deamination and fouling are serious, the oil content of biochemical inlet water is far beyond the design value, and the biochemical treatment section can not normally run; steam consumption of deacidification, deamination, extraction, dephenolization and solvent recovery is large, energy consumption is high, and operation cost is high; the indexes of the wastewater slightly fluctuate, so that the indexes of phenol, oil and the like of biochemical influent water exceed the designed values, and the impact resistance of the whole device is poor. Whether the pretreatment process of the coal chemical wastewater is reasonable or not directly influences whether the biochemical treatment working section at the rear end can reach the standard for discharge or not and the running cost of wastewater pretreatment.
The patent documents of Chinese invention patent application No. 201210144762.X, grant notice No. CN 102659204B and grant notice No. 2013.12.04 disclose a coal chemical wastewater treatment method. The method takes the methyl pentenone as an extracting agent, and the coal chemical wastewater containing phenol, tar, petroleum hydrocarbon and COD, such as gasification, coking, dry distillation, liquefaction, and the like, and the extracting agent are extracted and dephenolized in an extraction tower or a mixing clarifier, and simultaneously most of tar and petroleum hydrocarbon pollutants are removed, so that the pollution load of the wastewater is reduced, the load of a subsequent biochemical section is lightened, and the standard discharge or the recycling of the wastewater is ensured. However, the invention has the following disadvantages: because the tar substances in the coal chemical industry wastewater are divided into light oil (with the specific gravity of 0.96-0.98) and heavy oil (with the specific gravity of 1.02-1.04), the methyl pentenone (with the specific gravity of 0.85) is directly adopted to extract the coal chemical industry wastewater containing the tar substances in an extraction tower or a mixed clarifier, so that the extraction and separation of the light oil can be realized, but the extraction and separation of the heavy oil are difficult to realize, and the heavy oil carries the extracted water phase to a subsequent biochemical working section along with the extracted water phase, thereby influencing the normal operation of the biochemical working section.
Chinese patent application No. 201510347035.7, No. CN 106315906B, No. 2019.09.13, disclose a method and apparatus for removing ash and oil aminophenol from coal chemical industry wastewater. The invention uses ash residue/tar extraction agent to extract the coal chemical industry waste water for deashing and removing tar, so as to obtain deashing and tar removing waste water and ash-rich and tar-rich extraction agent; sequentially carrying out deacidification treatment and deamination treatment on the deashing slag and tar removal wastewater; extracting, dephenolizing and deoiling the wastewater after the deamination treatment to obtain a phenol-rich oil-rich extractant and dephenolized and deoiled wastewater; part of the phenol-rich and oil-rich extractant is used for the de-ashing of the extractant and the de-tar recycling. Before deacidification and deamination of wastewater, the invention first carries out gravity settling, coke filtration or oil removal pretreatment in an oil separation tank, and then carries out extraction deashing residue and tar removal treatment, thereby effectively solving the pollution and blockage problems of deacidification and deamination of wastewater and extraction dephenolization. However, the invention has the following disadvantages: the extraction agent is adopted to remove ash and tar in the wastewater, the circulation amount of the extraction agent is large, the loss amount of the extraction agent is inevitably large, and the energy consumption for purifying the extraction agent is high; the ash-rich and tar-rich extractant is purified by adopting a rectification mode, so that the fouling and the blockage of a rectification tower are easily caused; the extraction deashing slag detarring is arranged before deacidification and deamination, the pH value of the waste water is high, and the extraction detarring effect is poor.
Chinese patent application No. 202010790858.8, application publication No. CN 111762950A, application publication No. 2020.10.13 disclose a thermally coupled phenol-ammonia wastewater treatment device and method. The method adopts two-stage solvent recovery towers which are connected in series, the two-stage solvent recovery towers are operated under the negative pressure of high vacuum degree, the operation pressure of the former-stage solvent recovery tower is 40-70kPa (a), the operation pressure of the latter-stage solvent recovery tower is 20-40kPa (a), and steam extracted from the side line of the deamination tower is used as a heat source of a reboiler of the former-stage solvent recovery tower. The invention saves the steam consumption of solvent recovery, but because the temperature of the steam extracted from the side line of the deamination tower is 150 ℃, the temperature level of the steam does not meet the requirement of a reboiler on a heat source when the solvent recovery tower is operated under normal pressure or micro negative pressure, the solvent recovery tower has to be operated under high vacuum degree, so that the solvent loss is large, and the waste water treatment cost is not saved.
Disclosure of Invention
The invention provides a pretreatment method of coal chemical wastewater, which solves the problems of poor oil removal effect, severe pollution blockage of a deacidification deamination system, short operation period, substandard crude phenol product, unreasonable heat utilization, high operation cost and poor impact resistance in the prior art.
In order to solve the technical problems, the technical scheme provided by the invention is as follows:
a coal chemical industry wastewater pretreatment method comprises the following steps:
(1) oil removal and solid removal: the coal chemical industry wastewater enters an oil removal and solid removal system, heavy oil, light oil and partial oil residue in the wastewater are removed through a high-efficiency coalescence oil remover, and the oil residue and other solid suspended matters in the wastewater are further removed through a multi-media filter from the wastewater after oil removal;
(2) pre-deoiling: the deoiling and solid removing wastewater in the step (1) is connected to the upper part of an acid saturation extraction tower, acid gas and an extracting agent are connected to the lower part of the acid saturation extraction tower, the wastewater is in countercurrent contact with the acid gas and the extracting agent in the tower, the acid gas is dissolved and saturated in the wastewater to ensure that the pH value in the tower is less than 7, emulsified oil and dissolved oil in the wastewater are extracted to a pre-deoiling extraction phase in an acid environment, the pre-deoiling extraction phase is discharged from the top of the tower to a solvent/phenol recovery system, pre-deoiling wastewater with a small amount of extracting agent is discharged from the bottom of the tower to a deacidification and deamination system, and residual acid gas is discharged from the top of the tower;
(3) deacidifying and deaminating: the deacidification deamination system adopts a double-tower steam stripping process; the pre-deoiling wastewater in the step (2) enters the top of a deacidification tower, and low boiling point hydrocarbons and H dissolved in the pre-deoiling wastewater2S、CO2Removing in a deacidification tower, discharging deacidification wastewater from the bottom of the deacidification tower, introducing the deacidification wastewater into the upper part of a deamination tower, discharging crude ammonia gas from the top of the deamination tower, and discharging deacidification deamination wastewater from the bottom of the deamination tower;
(4) and (3) extraction dephenolization: the deacidification and deamination wastewater is connected to the upper part of a dephenolization extraction tower of an extraction dephenolization system, a dephenolization extracting agent is connected to the lower part of the dephenolization extraction tower, the deacidification and deamination wastewater and the extracting agent are in countercurrent contact in the tower, phenol and homologous compounds in the deacidification and deamination wastewater are dissolved by the extracting agent and discharged from the top of the tower along with a dephenolization extraction phase, the dephenolization wastewater carries a small amount of the extracting agent and is discharged from the bottom of the tower, and the dephenolization extraction phase and the dephenolization wastewater containing the extracting agent are subjected to solvent;
(5) solvent/phenol recovery: introducing resin backwash liquid from the pre-deoiling extraction phase, the dephenolizing extraction phase and the deep dephenolizing system into a phenol tower for distillation, recovering an extracting agent from the top of the phenol tower, recycling the extracting agent from the pre-deoiling system, the extracting dephenolizing system and the deep dephenolizing system, and recovering a crude phenol product from the bottom of the phenol tower; the dephenolized wastewater containing the extracting agent is fed into a water tower for distillation, the extracting agent is recovered from the top of the water tower, and the dephenolized wastewater after the extracting agent is separated is discharged from the bottom of the water tower and is sent to a deep dephenolizing system; the extractant recovered from the phenol tower and the tower top of the water tower is returned to the pre-deoiling system, the extraction dephenolizing system and the deep dephenolizing system for recycling;
(6) deep dephenolization: the dephenolized wastewater after the extraction agent is separated is connected to the top of a resin adsorption tower of a deep dephenolizing system, a small amount of residual phenol oil in the wastewater is further adsorbed by resin, and the pretreated purified water is discharged from the bottom of the resin adsorption tower to a biochemical treatment working section.
Wherein, preferably, the heavy oil and the light oil in the step (1) are respectively recovered as products, and the solid suspended substances are collected in the form of oil residues; the high-efficiency coalescence degreaser can adopt 1 stage or multi-stage series connection; one or more groups of efficient coalescence fillers are arranged in the efficient coalescence degreaser, and the efficient coalescence fillers are hydrophilic oleophobic materials or oleophilic hydrophobic materials; the multi-medium filter is internally provided with a plurality of layers of filter media, and the filter media are quartz sand or ceramic balls.
Wherein, preferably, the acid gas introduced into the lower part of the acid saturation extraction tower in the step (2) is low-boiling-point hydrocarbon and H dissolved in the pre-deoiling wastewater removed from the top of the deacidification tower2S and CO2The recycle gas of (1).
Wherein, preferably, the extracting agents of the step (2) and the step (4) are the extracting agents recovered from the water tower and the phenol tower and the extracting agents respectively added from the bottom of the tower, and the extracting agents are ether organic solvents and ketone organic solvents.
Wherein, preferably, the extracting agent is one or more of diisopropyl ether, methyl isobutyl ketone, methyl isopropyl ketone and toluene.
Preferably, the side line extracted steam at the upper part of the deamination tower is used as a heat source of a reboiler of a water tower of the solvent/phenol recovery system, the condensate is returned to the upper part of a side line extraction outlet, and meanwhile, an extractant condensing reflux device arranged at the top of the deamination tower is used for controlling the temperature of crude ammonia gas discharged from the top of the tower to be lower than the azeotropic temperature of water and an extractant at an operating pressure, so that the loss of the extractant caused by the fact that a small amount of the extractant carried in deacidification wastewater enters the crude ammonia gas is avoided.
Wherein, preferably, the resin in the resin adsorption tower in the step (6) is regenerated by periodic backwashing by using the recycled extracting agent, and the resin backwashing liquid desolventizing/phenol recovery system is distilled and separated by a phenol tower
3. Advantageous effects
Compared with the prior art, the coal chemical industry wastewater pretreatment method provided by the invention has the following beneficial effects:
(1) heavy oil, light oil and partial oil residue in the wastewater are removed by adopting a 1-stage or multi-stage series efficient coalescence degreaser, solid suspended matters such as the oil residue and the like are further removed by adopting a multi-medium filter, and floating oil, dispersed oil and oil residue in the wastewater are efficiently removed without introducing any solvent; meanwhile, only the undelivered emulsified oil and dissolved oil remain in the oil-removing and solid-removing wastewater, so that the low oil content in the crude phenol is ensured, and the index of the crude phenol content meets the product requirement;
(2) the pre-deoiling system adjusts the pH value of the deoiling and solid removing wastewater to be less than 7 by adopting the acid gas discharged by the deacidifying and deaminating system, and simultaneously adopts an extracting agent to extract and remove emulsified oil and dissolved oil in the wastewater in an acid environment, so that the oil content of the pre-deoiling wastewater is low, the pollution and blockage problem of the deacidifying and deaminating system is thoroughly solved, and the long-period stable operation of the device is ensured;
(3) steam is extracted from the side line at the upper part of the deamination tower and is used as a heat source of a reboiler of the water tower, so that the steam consumption of the reboiler of the water tower is saved, the operation cost of the device is reduced, and meanwhile, condensate of the reboiler returns to the upper part of a side line extraction outlet, so that the temperature of crude ammonia at the top of the tower is favorably reduced;
(4) an extractant condensing reflux device is arranged at the top of the deamination tower to further control the temperature of the crude ammonia gas, and the temperature of the discharged crude ammonia gas is controlled to be lower than the azeotropic temperature of water and the extractant, so that a small amount of extraction carried in the pre-deoiling wastewater is prevented from being discharged from the tower top along with the crude ammonia gas, and the loss of the extractant is reduced;
(5) after the wastewater is extracted and dephenolized, the wastewater is further dephenolized by resin adsorption of a deep dephenolization system, the lower phenol content in biochemical inlet water can be still ensured when the phenol content of the wastewater fluctuates, and the impact resistance of a biochemical treatment working section is good;
(6) the deep dephenolizing system adopts an extracting agent of the same type as that of the extracting dephenolizing to carry out resin backwashing regeneration, does not introduce other solvents, and does not need to be provided with a backwashing liquid regeneration system independently; the backwash liquid is treated in a solvent/phenol recovery unit in a unified way, and the recovery rate of the crude phenol product is high.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art that other embodiments can be obtained by using the drawings without creative efforts.
FIG. 1 is a schematic process flow diagram of a coal chemical wastewater pretreatment method of the present invention;
in the figure: 1. high-efficiency coalescence degreaser, 2 multi-medium filter, 3 acid saturation extraction tower, 4 deacidification tower, 5 deamination tower, 6 dephenolization extraction tower, 7 water tower, 8 phenols tower, 9 resin adsorption tower, 10 hot feed preheater and 11 extractant condensation reflux device
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to the accompanying drawings and specific embodiments of the present invention, and it is to be understood that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The invention provides a pretreatment method of coal chemical industry wastewater, which is characterized in that the coal chemical industry wastewater is subjected to an oil removal and solid removal system to remove solid suspended matters such as floating oil, heavy oil in the form of dispersed oil, light oil, oil residue and the like in the wastewater and respectively recover the solid suspended matters into the heavy oil, the light oil and the oil residue; the deoiling and solid removing wastewater is saturated by acid gas through a pre-deoiling system, emulsified oil and dissolved oil in the wastewater are further extracted and removed, and a pre-deoiling extraction phase is removed from a solvent/phenol recovery system; removing low boiling point hydrocarbons and H dissolved in the pre-deoiled wastewater by a deacidification and deamination system2S and CO2Recovering in an acid gas mode, and simultaneously enriching ammonia in the wastewater into crude ammonia gas and sending out; removing phenol and homologues thereof in the deacidification and deamination wastewater through an extraction and dephenolization system, removing a dephenolization extract phase and a dephenolization wastewater containing an extracting agent to a solvent/phenol recovery system; separating the resin backwash liquid from the pre-deoiling extraction phase, the dephenolizing extraction phase and the deep dephenolizing system by a solvent/phenol recovery system to obtain a solvent for recycling and recovering crude phenol; the dephenolized wastewater after the extraction agent is separated is further dephenolized by a deep dephenolization system to remove phenol and homologues thereof in the wastewater, and then the pretreated purified water is sent to a biochemical treatment working section.
The process flow diagram is shown in figure 1, and specifically comprises the following steps:
(1) oil removal and solid removal: the coal chemical industry wastewater enters an oil removal and solid removal system, heavy oil, light oil and partial oil residue in the wastewater are removed through an efficient coalescence oil remover 1, and the oil residue and other solid suspended matters in the wastewater are further removed through a multi-media filter 2 after the oil is removed; respectively recovering the heavy oil and the light oil as products in the step (1), and collecting solid suspended matters in an oil residue mode; the efficient coalescence degreaser 1 adopts a first-stage series connection; four groups of efficient coalescence fillers are arranged in the efficient coalescence degreaser 1.
(2) Pre-deoiling: the oil-removing and solid-removing waste water in the step (1) is connected to the upper part of an acid saturation extraction tower 3, acid gas and an extracting agent are connected to the lower part of the acid saturation extraction tower 3, the waste water is in countercurrent contact with the acid gas and the extracting agent in the tower, the acid gas is dissolved and saturated in the waste water to ensure that the pH value in the tower is less than 7, and the waste water is subjected to acid environment in which the pH value is less than 7Emulsified oil and dissolved oil in the wastewater are extracted into a pre-deoiling extraction phase, the pre-deoiling extraction phase is discharged from the top of the tower to a solvent/phenol removal recovery system, pre-deoiling wastewater with a small amount of extractant is discharged from the bottom of the tower to a deacidification and deamination system, and residual acid gas is discharged from the top of the tower; the extractant in the step is the extractant recovered from a water tower 7 and a phenol tower 8, and is prepared by mixing the following components in a volume ratio of 1: 2: 2: 1 diisopropyl ether, methyl isobutyl ketone, methyl isopropyl ketone and toluene. The acid gas introduced into the lower part of the acid saturation extraction tower in the step is the acid gas discharged from the top of the deacidification tower 4 for removing the low-boiling-point hydrocarbons and H dissolved in the pre-deoiling wastewater2S and CO2The recycle gas of (1).
(3) Deacidifying and deaminating: the deacidification deamination system adopts a double-tower steam stripping process; the pre-deoiling waste water pipe in the step (2) is respectively provided with two branches, one branch is led into the upper part of the deacidification tower 4, the other branch is heated by the hot feed preheater 10 and then led into the middle upper part of the deacidification tower 4, and low boiling point hydrocarbons and H dissolved in the pre-deoiling waste water2S、CO2Removing in a deacidification tower 4, discharging deacidification wastewater from the bottom of the deacidification tower 4, introducing the wastewater into the upper part of a deamination tower 5, discharging crude ammonia gas from the tower top, and discharging deacidification and deamination wastewater from the bottom of the deamination tower 5; an extractant condensing reflux device 11 is arranged in the upper part of the deamination tower 5, so that the temperature of crude ammonia discharged from the top of the deamination tower is lower than the azeotropic temperature of wastewater and an extractant under the operating pressure of the deamination tower 5, and the extractant condensing reflux device 11 is positioned at the top of the deamination tower 5.
(4) And (3) extraction dephenolization: the deacidification deamination waste water is connected to the upper part of a dephenolizing extraction tower 6 of an extraction dephenolizing system, a dephenolizing extractant is connected to the lower part of the dephenolizing extraction tower 6, the deacidification deamination waste water is in countercurrent contact with the extractant, phenol and homologues thereof in the deacidification deamination waste water are dissolved by the extractant and discharged from the top of the tower along with a dephenolizing extraction phase, the dephenolizing waste water is discharged from the bottom of the tower along with a small amount of the extractant, and the dephenolizing extraction phase and the dephenolizing waste water containing the extractant are subjected to a solvent/phenol recovery system; the extractant in this step is the extractant recovered from the water tower 7 and the phenol tower 8.
(5) Solvent/phenol recovery: resin backwash liquid from the pre-deoiling extraction phase, the dephenolizing extraction phase and the deep dephenolizing system is introduced into a phenol tower 8 for distillation, an extracting agent is recovered from the top of the phenol tower 8, the extracting agent is recycled by a pre-deoiling system, an extracting dephenolizing system and a deep dephenolizing system, and a crude phenol product is recovered from the bottom of the tower; the dephenolized wastewater containing the extracting agent is connected into a water tower 7 for distillation, the extracting agent is recovered from the top of the water tower 7, and the dephenolized wastewater after the extracting agent is separated is discharged from the bottom of the tower and is sent to a deep dephenolizing system; steam is extracted from the upper side line of the deamination tower and is used as a heat source of a reboiler of the water tower; the extracting agents recovered from the top of the phenol tower 8 and the water tower 7 are sent back to the pre-deoiling system, the extraction dephenolization system and the deep dephenolization system for recycling;
(6) deep dephenolization: the dephenolized wastewater after the extraction agent is separated is connected to the top of a resin adsorption tower 9 of a deep dephenolization system, a small amount of residual phenol oil in the wastewater is further adsorbed by resin, and the pretreated purified water is discharged from the bottom of the resin adsorption tower 9 to a biochemical treatment working section.
In the invention, the high-efficiency coalescence degreaser 1 can adopt 1-stage or multi-stage series connection; one or more groups of efficient coalescence fillers are arranged in the efficient coalescence oil remover 1, and the efficient coalescence fillers are hydrophilic oleophobic materials or oleophilic hydrophobic materials; the multi-medium filter 2 is internally provided with a plurality of layers of filter media, and the filter media are quartz sand or ceramic balls.
The extracting agent is one or the combination of more of diisopropyl ether, methyl isobutyl ketone, methyl isopropyl ketone and toluene.
The side-draw steam at the upper part of the deamination tower 5 is used as a heat source of a reboiler of a water tower 7 of a solvent/phenol recovery system, condensate returns to the upper part of a side-draw outlet, and meanwhile, the temperature of crude ammonia discharged from the top of the tower is controlled to be lower than the azeotropic temperature of water and an extracting agent under the operating pressure by an extracting agent condensing reflux device 11 arranged at the top of the deamination tower 5, so that the loss of the extracting agent caused by the fact that a small amount of extracting agent carried in deacidification wastewater enters the crude ammonia is avoided.
Wherein, the resin in the resin adsorption tower 9 in the step (6) adopts the recycled extractant to carry out periodic backwashing regeneration, and the resin backwashing liquid is used for removing the solvent/phenol recovery system and carrying out distillation separation on the phenol tower 8.
The method of the embodiment is used for pretreating coal chemical wastewater. The specification of the inlet water of the coal chemical wastewater is shown in Table 1, the water amount is 34t/h, the color is red brown, and the water temperature is 55 ℃.
Table 1: coal chemical wastewater inlet specification meter
The pretreatment process of the coal chemical industry wastewater comprises the following steps:
the wastewater in the coal chemical industry is subjected to 1-stage efficient coalescence degreaser 1 and multi-media filter 2 to remove solid suspended matters such as floating oil, heavy oil in the form of dispersed oil, light oil, oil residue and the like from the wastewater, and the solid suspended matters are respectively recovered into the heavy oil, the light oil and the oil residue, the specifications of the deoiling and solid removing wastewater are shown in a table 2, and the specifications of the recovered heavy oil, the light oil and the oil residue are shown in a table 3.
Table 2: oil-removing solid waste water specification meter
| Oil removing and solid removing waste water | Specification of |
| pH value | 9.2 |
| Ammonia nitrogen | 4500mg/L |
| H2S | 1200mg/L |
| CO2 | 3200mg/L |
| Phenol and its preparation | 3500mg/L |
| Total phenols | 6000mg/L |
| Petroleum products | 300mg/L |
| Total oil | 1000mg/L |
| Total solid suspension | 100mg/L |
Table 3: heavy oil, light oil and oil residue specification table
| Specification of | Heavy oil | Light oil | Oil residue |
| Recovery amount | 48.5kg/h | 60.4kg/h | 27.7 |
| Water content | 1.8％ | 1.5％ | 1.8％ |
| Heat value | 9050kCal/kg | 8760kCal/kg | 4300kCal/kg |
After the oil removal and solid removal wastewater is saturated by acid gas in an acid saturation extraction tower 3, the pH value is 5.5, emulsified oil and dissolved oil in the wastewater are further extracted and removed by an extracting agent, a pre-deoiling extraction phase is subjected to a solvent/phenol recovery system, residual acid gas is sent out, the pre-deoiling wastewater is subjected to a deacidification and deamination system, the specification of the pre-deoiling wastewater is shown in a table 4, and the specification of the residual acid gas is shown in a table 5.
Table 4: specification table for pre-deoiling waste water
| Pre-deoiled waste water | Specification of |
| pH value | 5.5 |
| Ammonia nitrogen | 4500mg/L |
| H2S | 2800mg/L |
| CO2 | 4500mg/L |
| Phenol and its preparation | 1200mg/L |
| Total phenols | 1800mg/L |
| Petroleum products | 120mg/L |
| Total oil | 220mg/L |
| Total solid suspension | 100mg/L |
Table 5: specification table of residual acid gas
| Residual acid gas | Specification of |
| Air flow | 152kg/h |
| Temperature of | 53℃ |
| H2S+CO2Content (wt.) | 98.4％ |
Removing low boiling point hydrocarbons and H dissolved in the pre-deoiled wastewater by a deacidification and deamination system2S and CO2And the lower part of the deacidification and saturation extraction tower 3 is recovered in an acid gas mode, ammonia in the wastewater is enriched into crude ammonia gas and is sent out, the deacidification and deamination wastewater is sent to an extraction and dephenolization system, the specification of the crude ammonia gas is shown in a table 6, and the specification of the deacidification and deamination wastewater is shown in a table 7.
Table 6: crude ammonia specification meter
| Crude ammonia gas | Specification of |
| Air flow | 156kg/h |
| Temperature of | 45℃ |
| NH3Content (wt.) | 98％ |
| Water content | 2％ |
Table 7: specification table of deacidification deamination waste water
The deacidification deamination waste water is removed phenol and homologues thereof in the waste water by an extraction dephenolization system, a dephenolization extraction phase and an extractant dephenolization waste water solvent/phenol recovery system, and the specifications of the extractant dephenolization waste water are shown in a table 8.
Table 8: specification table of dephenolized wastewater containing extractant
| Dephenolizing waste water containing extractant | Specification of |
| pH value | 7.5 |
| Ammonia nitrogen | 80mg/L |
| H2S | 8mg/L |
| CO2 | 10mg/L |
| Phenol and its preparation | 80mg/L |
| Total phenols | 200mg/L |
| Petroleum products | 60mg/L |
| Total oil | 90mg/L |
| Total solid suspension | 100mg/L |
| Extracting agent | 2.2％ |
Separating the pre-deoiling extraction phase and the dephenolizing extraction phase by a solvent/phenol recovery system to obtain a solvent for recycling and recovering crude phenol, further removing phenol and homologues thereof in the dephenolizing wastewater after separating the extracting agent by a deep dephenolizing system, and then sending the pre-treated purified water to a biochemical treatment working section, wherein the specification of the pre-treated purified water is shown in a table 9, and the specification of the crude phenol is shown in a table 10.
Table 9: specification table for pretreated purified water
Table 10: crude phenol specification table
| Crude phenol | Specification of |
| Flow rate | 233.4kg/h |
| Temperature of | 40℃ |
| Phenol and its homologue content | 86.2％ |
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (7)
1. A coal chemical industry wastewater pretreatment method is characterized by comprising the following steps:
(1) oil removal and solid removal: the coal chemical industry wastewater enters an oil removal and solid removal system, heavy oil, light oil and partial oil residue in the wastewater are removed through a high-efficiency coalescence oil remover, and the oil residue and other solid suspended matters in the wastewater are further removed through a multi-media filter from the wastewater after oil removal;
(2) pre-deoiling: the deoiling and solid removing wastewater in the step (1) is connected to the upper part of an acid saturation extraction tower, acid gas and an extracting agent are connected to the lower part of the acid saturation extraction tower, the wastewater is in countercurrent contact with the acid gas and the extracting agent in the tower, the acid gas is dissolved and saturated in the wastewater to ensure that the pH value in the tower is less than 7, emulsified oil and dissolved oil in the wastewater are extracted to a pre-deoiling extraction phase in an acid environment, the pre-deoiling extraction phase is discharged from the top of the tower to a solvent/phenol recovery system, the pre-deoiling wastewater with a small amount of extracting agent is discharged from the bottom of the tower to a deacidification and deamination step, and residual acid gas is discharged from the top of the tower;
(3) deacidifying and deaminating: the deacidification deamination system adopts a double-tower steam stripping process; the pre-deoiling wastewater in the step (2) enters the top of a deacidification tower, and low boiling point hydrocarbons and H dissolved in the pre-deoiling wastewater2S、CO2Removing in a deacidification tower, discharging acid gas from the bottom of the deacidification tower, introducing the acid gas into the upper part of a deamination tower, discharging crude ammonia gas from the top of the deamination tower, and discharging deacidification and deamination wastewater from the bottom of the deamination tower;
(4) and (3) extraction dephenolization: the deacidification and deamination wastewater is connected to the upper part of a dephenolization extraction tower of an extraction dephenolization system, a dephenolization extracting agent is connected to the lower part of the dephenolization extraction tower, the deacidification and deamination wastewater and the extracting agent are in countercurrent contact in the tower, phenol and homologous compounds in the deacidification and deamination wastewater are dissolved by the extracting agent and discharged from the top of the tower along with a dephenolization extraction phase, the dephenolization wastewater is accompanied with a small amount of the extracting agent and discharged from the bottom of the tower, and the dephenolization extraction phase and the dephenolization wastewater containing the extracting agent enter a solvent;
(5) solvent/phenol recovery: introducing resin backwash liquid from the pre-deoiling extraction phase, the dephenolizing extraction phase and the deep dephenolizing system into a phenol tower for distillation, recovering an extracting agent from the top of the phenol tower, recycling the extracting agent from the pre-deoiling system, the extracting dephenolizing system and the deep dephenolizing system, and recovering a crude phenol product from the bottom of the phenol tower; the dephenolized wastewater containing the extracting agent is fed into a water tower for distillation, the extracting agent is recovered from the top of the water tower, and the dephenolized wastewater after the extracting agent is separated is discharged from the bottom of the water tower and is sent to a deep dephenolizing system; the extractant recovered from the phenol tower and the tower top of the water tower is returned to the pre-deoiling system, the extraction dephenolizing system and the deep dephenolizing system for recycling;
(6) deep dephenolization: the dephenolized wastewater after the extraction agent is separated is connected to the top of a resin adsorption tower of a deep dephenolizing system, a small amount of residual phenol oil in the wastewater is further adsorbed by resin, and the pretreated purified water is discharged from the bottom of the resin adsorption tower to a biochemical treatment working section.
2. The coal chemical industry wastewater pretreatment method according to claim 1, characterized in that: respectively recovering the heavy oil and the light oil as products in the step (1), and collecting solid suspended matters in an oil residue mode; the high-efficiency coalescence degreaser can adopt 1-stage or multi-stage series connection; one or more groups of efficient coalescence fillers are arranged in the efficient coalescence degreaser, and the efficient coalescence fillers are hydrophilic oleophobic materials or oleophilic hydrophobic materials; the multi-medium filter is internally provided with a plurality of layers of filter media, and the filter media are quartz sand or ceramic balls.
3. The coal chemical industry wastewater pretreatment method according to claim 1, characterized in that: the acid gas introduced into the lower part of the acid saturation extraction tower in the step (2) is used for removing low-boiling-point hydrocarbons and H dissolved in the pre-deoiling wastewater discharged from the top of the deacidification tower2S and CO2The recycle gas of (1).
4. The coal chemical industry wastewater pretreatment method according to claim 1, characterized in that: the extracting agents in the step (2) and the step (4) are the extracting agents recovered from the water tower and the phenol tower and the extracting agents respectively added from the bottom of the tower, and the extracting agents are ether and ketone organic solvents.
5. The coal chemical industry wastewater pretreatment method according to claim 4, characterized in that: the extracting agent is one or a combination of more of diisopropyl ether, methyl isobutyl ketone, methyl isopropyl ketone and toluene.
6. The coal chemical industry wastewater pretreatment method according to claim 1, characterized in that: and meanwhile, the temperature of crude ammonia gas discharged from the top of the tower is controlled to be lower than the azeotropic temperature of water and an extracting agent under the operating pressure by an extracting agent condensation reflux device arranged at the top of the deamination tower.
7. The coal chemical industry wastewater pretreatment method according to claim 1, characterized in that: and (3) carrying out periodic backwashing regeneration on the resin in the resin adsorption tower in the step (6) by adopting a recycled extracting agent, and carrying out distillation separation on a phenol tower of a solvent/phenol recovery system of resin backwashing liquid.
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