CN107032555A - A kind of method for handling oil-containing coal gasification waste water - Google Patents
A kind of method for handling oil-containing coal gasification waste water Download PDFInfo
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- CN107032555A CN107032555A CN201611117273.XA CN201611117273A CN107032555A CN 107032555 A CN107032555 A CN 107032555A CN 201611117273 A CN201611117273 A CN 201611117273A CN 107032555 A CN107032555 A CN 107032555A
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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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D5/00—Condensation of vapours; Recovering volatile solvents by condensation
- B01D5/0033—Other features
- B01D5/0036—Multiple-effect condensation; Fractional condensation
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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
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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
- C02F1/20—Treatment of water, waste water, or sewage by degassing, i.e. liberation of dissolved gases
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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
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/16—Nitrogen compounds, e.g. ammonia
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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
- C02F2101/30—Organic compounds
- C02F2101/32—Hydrocarbons, e.g. oil
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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
- C02F2101/30—Organic compounds
- C02F2101/34—Organic compounds containing oxygen
- C02F2101/345—Phenols
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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
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/34—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32
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Abstract
A kind of method for handling oil-containing coal gasification waste water is by sour gas saturation process, solvent extraction dephenolize and oily process, extractant and carbolic oil separation circuit, depickling and residual solvent recovery process, deamination process, the phenol in oil-containing coal gasification waste water, ammonia, oils are effectively removed.The present invention has technique simple, and energy consumption is low, reclaims the high advantage of product purity.
Description
Technical field
The present invention relates to a kind of processing method of oil-containing coal gasification waste water.
Background technology
It is to solve the important channel of energy problem of China to greatly develop coal chemical industry.But coal chemical industry process can produce it is substantial amounts of
Technique waste water, wherein being a kind of high ammonia nitrogen, high phenol containing pollutants such as substantial amounts of phenol, ammonia, aliphatic acid, oils, sour gas
Value, high CODcr, high chroma and very intractable industrial wastewater, it is necessary to can just be sent after first being handled using chemical separating flow
Biochemical treatment.
The treatment technology and method generally used at present is that the waste water heating from upstream device is carried out into stripping first to take off
Sour deamination, extracting and dephenolizing is carried out after then cooling down, and the waste water containing solvent is heated into progress stripping recycling design again afterwards, most
Biochemical treatment is sent after cooling down afterwards, therefore is needed during processing waste water by waste water progress heating for multiple times and repeatedly cooling, steaming
Steam consumption and circulating cooling water consumption are all than larger；And it is every containing hundreds of even thousands of milligrams in the gas liquor come from upstream device
The grease risen, easily causes the blocking of tower and heat exchanger, shortens the cycle of operation of equipment, while also increasing operating personnel's
Working strength, many factories that are compelled against one's will for easily stifled equipment there is provided standby, so as to increase plant area and investment；And by
Contain Chuck Steak in waste water, part oil is stripped out during deamination together with ammonia, have impact on the quality of byproduct ammonia.
The mutual solubility of the extractant used at present such as isopropyl ether, MIBK etc. and water is larger, its solubility in water point
Not Wei 0.6wt% and 1.7wt%, in order to reclaim this partial solvent, it is necessary to a set of solvent recovery unit of special configuration so that whole
Device long flow path, equipment complexity, high energy consumption, investment are big.
The content of the invention
It is an object of the invention to easily be blocked for equipment present in current coal gasification waste water processing procedure, high energy consumption,
The inferior problem of the ammonia of recovery is simple there is provided a kind of technique, and energy consumption is low, reclaims the high processing oil-containing coal gasification of product purity
The method of waste water.
The present invention process step be：
(1) sour gas saturation process：Oil-containing coal gasification waste water enters from saturator top, and sour gas is from saturator bottom
Into sour gas carries out acidifying to reduce the pH value of waste water in saturator to waste water, and the oil-containing coal gasification after acidifying is given up
Water is discharged from saturation tower bottom, feeding extraction tower top, does not enter scrubbing tower at the top of saturator 1 by the sour gas that waste water absorbs
Out sulfur recovery is sent to handle at the top of scrubbing tower after bottom, dilute phenol water washing after deamination, the waste water that wash tower bottoms come out
Enter together with oil-containing coal gasification waste water in saturator；
(2) solvent extraction dephenolize and oily process：The extractant entered into extraction tower waste water and from extraction tower bottom in tower
Counter current contacting carries out multi-stage counter current extraction, comes out the waste water after removing phenol and oil from extraction tower bottom, is come out from extraction tower top
Rich in oil and phenol extraction phase enter extract groove；
(3) extractant and carbolic oil separation circuit：The extraction phase rich in oil and phenol in extract groove by with from phenol tower tower
The extractant that the carbolic oil and phenol column overhead that kettle comes out come out enters phenol tower after exchanging heat respectively, and extractant and carbolic oil are carried out in phenol tower
Rectifying separation, the carbolic oil that phenol tower tower reactor comes out after heat exchange to being delivered to tank field, the extractant warp that the tower top of phenol tower 3 is distilled
Cross and enter solvent circulating slot after heat exchange, the extractant part in solvent circulating slot send extraction tower to recycle afterwards, another portion
Extractant is divided to return in phenol tower；
(4) depickling and residual solvent recovery process：The waste water part after removing phenol and oil is come out from extraction tower bottom to make
Enter for the cold feed of extracting tower from extracting tower top, dilute phenol water of the another part after the deamination with being come out from deammoniation tower is changed
Enter after heat as hot feed in the middle part of the extracting tower, the sour gas that is come out from the top of extracting tower 4 and the extraction in being dissolved in waste water
Take the gaseous mixture of agent to enter cooler, acid qi leel flow container is entered afterwards and carries out solution-air-liquid three phase separation, acid qi leel flow container
The sour gas isolated returns to saturator, and upper phase extractant is returned in solvent circulating slot, and lower floor's liquid phase aqueous solution is returned
Extracting tower, to prevent carbon ammonium Crystallization Plugging heat exchanger tube, the dilute phenol water sprayed into heat-exchange tube of cooler after deamination；
(5) deamination process：Waste water enters from deammoniation tower top after the depickling come out from the bottom of extracting tower 4, while from deamination
Tower top adds sodium hydroxide solution, and the ammoniacal liquor vapour come out from deamination column overhead enters by three heat exchangers and three segregator groups
Into three-level fractional condensation device carry out concentration purification, liquid phase is segregated afterwards and enters ammonia condensate tank, the big portion of fractional condensation liquid in ammonia condensate tank
Divide and return at the top of deammoniation tower as backflow；To avoid accumulation of the sour gas in deamination process, fraction fractional condensation liquid delivers to depickling
Tower, the rich ammonia come out from last segregator enter follow-up ammonia refining unit style into ammoniacal liquor or liquefied ammonia in factory desulfurization,
Denitration is used or as production marketing；A dilute phenol water part after the deamination come out from deamination tower bottom delivers to scrubbing tower and cooling
In device, another part delivers to subsequent biochemical processing.
Sour gas in the step (1) is carbon dioxide.
The pH value of waste water after being acidified in saturator in the step (1) is 6.5-8.5.
Saturator in the step (1) is plate column or packed tower, and saturation temperature is 20-60 DEG C, and pressure is 0.02-
0.30MPag, the number of plates is 10-20 blocks.
Extractant in the step (2) is methyl iso-butyl ketone (MIBK).
The PH of aqueous phase is 6.5-8.5 in extraction tower in the step (2), and extraction temperature is 20-60 DEG C, and extracting pressure is
0.02-0.40MPag, the volume ratio of waste water of the extractant with entering extraction tower is 1:3-10, extraction series is 4-8 grades.
Extraction tower in the step (2) is turntable extracting tower or packed extraction tower or perforated-plate extraction tower.
Phenol tower in the step (3) is plate column, and tower top temperature is 110-170 DEG C, and bottom temperature is 200-260 DEG C；
Pressure is 0.02-0.32MPag；Reflux ratio is 0.15-0.26, and the number of plates is 15-20 blocks.
Extracting tower in the step (4) is to remove sour gas together with remaining in the solvent in waste water, cold feed with
The volume ratio of hot feed is 1:3-6, tower top temperature is 90-110 DEG C, and bottom temperature is 135-160 DEG C；Pressure is 0.25-
0.55MPag；The number of plates is 22-30 blocks.
Deammoniation tower in the step (5) is plate column, and tower top temperature is 135-160 DEG C, and bottom temperature is 145-165
℃；Pressure is 0.30-0.60MPag；The number of plates is 25-30 blocks.
The fractional condensation liquid of 70%-90% volume flows returns to the top conduct of deammoniation tower 5 in ammonia condensate tank in the step (5)
Backflow, the fractional condensation liquid of remaining 10%-30% volume delivers to extracting tower 4.
Deammoniation tower top in the step (5) adds the sodium hydroxide solution that mass concentration is 20-40wt%, addition
For the 0.2-1.0wt% for the wastewater quality for entering deammoniation tower.
The ammoniacal liquor vapour that the step (5) comes out from deamination column overhead enters what is be made up of three heat exchangers and three segregators
Three-level fractional condensation device is that ammoniacal liquor vapour is introduced into one-level heat exchanger, afterwards into one-level segregator, enters back into two grades heat exchangers,
Enter two-stage fractional condensation device afterwards, three-level heat exchanger is finally entered, afterwards into three-level segregator.
The present invention compared with prior art, has the following advantages that：
1. the phenols in waste water can be reclaimed effectively, phenol residual quantity can be reduced to below 400mg/L；Simultaneously in waste water
Oils has preferable removal effect, mitigates the burden of biochemical treatment；
2. blockage problem of the oils in current waste water to equipment can be solved effectively, heat exchanger inventory, extension are reduced
In the plant running cycle, reduce investment outlay；
3. the influence of phenol, oil to ammoniacal liquor or liquefied ammonia quality can be prevented effectively from, ammoniacal liquor or liquefied ammonia purity are improved；
4. waste water is only once heated and a cooling procedure in the inventive method, energy consumption can be greatly lowered.
Brief description of the drawings
Fig. 1 is the process flow diagram of the present invention.
As shown in the figure：1- saturators, 2- extraction towers, 3- phenol towers, 4- extracting towers, 5- deammoniation towers, 6- scrubbing towers, 7- solvents are followed
Annular groove, 8- extract grooves, 9- acidity qi leel flow containers, 10- one-level segregators, 11- two-stage fractional condensation devices, 12- three-level segregators, 13-
Ammonia condensate tank, 14- coolers.
Embodiment
Embodiment 1
(1) sour gas saturation process
The present embodiment chooses the waste water of oil-containing, phenol and ammonia that fixed bed crushed coal pressure gasifying is produced, separates and fills through gas liquor
Put after oil removal, mud dirt, tar and part light oil, total phenol is 5570mg/L, wherein volatile phenol is 4475mg/L, and total ammonia is
8180mg/L, wherein free ammonia are 6230mg/L, and oil is 1110mg/L, and waste water pH value is 9.0, into the saturator 1 of the present invention
Top, saturator 1 uses plate column, and operation temperature is 45 DEG C, and operating pressure is 0.10MPag, and the number of plates is 14, outside device
Come carbon dioxide and from the sour gas containing extractant of acid qi leel flow container 9 from the bottom of saturator 1 enter tower in, two
Person's counter current contacting, solvent gas and carbon dioxide gas are absorbed into waste water by oily waste water, and excessive sour gas is from saturator 1
Top enters in scrubbing tower 6, is further sent follow-up sulfur recovery unit to handle after the next dilute phenol water washing in the bottom of deammoniation tower 5, washed
It is 7.1 to wash the oil-containing phenol water ph value that the waste water that the bottom of tower 6 comes out enters after saturator 1, sour gas saturation, from the bottom of saturator 1
In discharge, feeding extraction tower 2.
(2) solvent extraction dephenolize and oily process
The oil-containing phenol water come out from the bottom of saturator 1 uses methyl-isobutyl by being pumped into the top of extraction tower 2, extractant
Ketone, extractant is pumped into the bottom of extraction tower 2 by solvent circulating slot 7, the two counter current contacting in tower, the phenol in oil-containing phenol water
Agent extraction is extracted with oil to enter in extraction phase, the volume ratio of extractant and waste water is 1:5, extraction pH value is 7.1, extraction temperature
For 45 DEG C, extracting pressure is 0.30MPa, and extraction series is 4 grades, and extract flow to extract from the top settling section of extraction tower 2
In storage tank 8, raffinate is discharged from the bottom of extraction tower 2, in feeding extracting tower 4.
(3) extractant and carbolic oil separation circuit
Extract in extract storage tank 8 is through exchanging heat to the top of phenol tower 3 is entered after 105 DEG C, and the tower top pressure of phenol tower 3 is
0.01MPa, temperature is 113 DEG C, and tower bottom pressure is 0.04MPa, and temperature is 203 DEG C, and reflux ratio is 0.14, and the number of plates is 16, tower
Push up after the extractant distilled is cooled down through heat exchanger and return to solvent circulating slot 7, the carbolic oil that bottom of towe comes out delivers to tank field.
(4) depickling and residual solvent recovery process
A part of cold feed as extracting tower 4 of waste water after removing phenol and oil is come out from extracting tower 4 from the bottom of extraction tower 2
Top enters, as hot feed from depickling after dilute phenol water heat exchange of the another part after the deamination with being come out from deammoniation tower 5
The middle part of tower 4 enters, and the volume ratio of hot and cold two bursts of chargings is 1:5, tower top pressure is 0.30MPa, and temperature is 95 DEG C, tower bottom pressure
For 0.32MPa, temperature is 142 DEG C, and the number of plates is 24, and the mixed gas of sour gas and methyl iso-butyl ketone (MIBK) pushes up vapour from extracting tower 4
Put forward, enter after being cooled to 40 DEG C through cooler 14 and solution-air-liquid three phase separation is carried out in sour gas point flow container 9, gas phase be containing
The sour gas of a small amount of solvent returns to saturator 1, and the liquid phase aqueous solution returns to extracting tower 4, and liquid phase solvent returns to solvent circulating slot 7.
In order to prevent carbon ammonium Crystallization Plugging heat exchanger tube, the dilute phenol water sprayed into the heat exchanger tube of cooler 14 after deamination.
(5) deamination process
Waste water after the depickling come out from the bottom of extracting tower 4 enters in deammoniation tower 5 from top, and tower top pressure is 0.38MPa,
Temperature is 145 DEG C, and tower bottom pressure is 0.40MPa, and temperature is 152 DEG C, and the number of plates is 27, and the ammoniacal liquor vapour gone out from stripped overhead enters
The three-level fractional condensation device being made up of heat exchanger and segregator carries out concentration purification, and the temperature of one-level segregator 10 is 125 DEG C, pressure
For 0.34MPa；The temperature of two-stage fractional condensation device 11 is 85 DEG C, and pressure is 0.30MPa；The temperature of three-level segregator 12 is 40 DEG C, pressure
Power is 0.26MPa.The fractional condensation liquid for 75% volume flow that three-level fractional condensation device is produced returns to the top of deammoniation tower 5 and is used as backflow, its
The fractional condensation liquid of 25% volume of remaininging delivers to the hot feed pipeline of extracting tower 4.The hydrogen that mass concentration is 20wt% is added on the top of deammoniation tower 5
Sodium hydroxide solution, addition is the 0.7wt% for the wastewater quality for entering deammoniation tower.Rich ammonia after concentrated purification enters follow-up
Into ammoniacal liquor or liquefied ammonia, the desulphurization and denitration in factory is personal or is used as production marketing for ammonia refining unit style；Come out from the bottom of deammoniation tower 5
Deamination after a dilute phenol water part deliver in scrubbing tower 6 and cooler 14, another part delivers to subsequent biochemical processing, in waste water
Total phenol content is 330mg/L, and wherein volatile phenol is 45mg/L, and oil content is 30mg/L, and total ammonia content is 78mg/L.
Embodiment 2
Pending waste water be the same as Example 1, process step be the same as Example 1, concrete technology condition is：
In step (1), saturator 1 uses packed tower, and operation temperature is 53.5 DEG C, and operating pressure is 0.15MPa, theoretical tower
Plate number is 20, and the waste water pH value of oil-containing, phenol and ammonia after sour gas saturation is 7.5.
In step (2), extraction tower 2 uses regular grid packing, and extraction series is 5 grades, the volume ratio of extractant and waste water
For 1:6, extraction temperature is 54 DEG C, and extracting pressure is 0.15MPa, and extraction pH value is 7.5.
In step (3), the tower top pressure of phenol tower 3 is 0.15MPa, and temperature is 144 DEG C, and tower bottom pressure is 0.18MPa, and temperature is
233℃；Reflux ratio is 0.17, and the number of plates is 17.
In step (4), the volume ratio of 4 hot and cold two bursts of chargings of extracting tower is 1:4, tower top pressure is 0.35MPa, and temperature is
100 DEG C, tower bottom pressure is 0.37MPa, and temperature is 146 DEG C, and the number of plates is 25.
In step (5), the tower top pressure of deammoniation tower 5 is 0.43MPa, and temperature is 148 DEG C, and tower bottom pressure is 0.45MPa, temperature
For 156 DEG C, the number of plates is 27.The temperature of one-level segregator 10 is 125 DEG C, and pressure is 0.36MPa；The temperature of two-stage fractional condensation device 11
For 85 DEG C, pressure is 0.32MPa；The temperature of three-level segregator 12 is 40 DEG C, and pressure is 0.24MPa.Three-level fractional condensation device is produced
The fractional condensation liquid of 80% volume flow return to the top of deammoniation tower 5 as backflow, the fractional condensation liquid of remaining 20% volume delivers to extracting tower 4
Hot feed pipeline.The sodium hydroxide solution addition that mass concentration is 25wt% is the wastewater quality into deammoniation tower 5
0.5wt%.It is 295mg/L that total phenol content in the waste water of biochemical treatment apparatus is sent after processing, and wherein volatile phenol is 27mg/L, and oil contains
Measure as 30mg/L, total ammonia content is 89mg/L.
Embodiment 3
Pending waste water equally chooses the waste water of the oil-containing, phenol and ammonia of fixed bed crushed coal pressure gasifying generation, through gas liquor
Separator is gone after oil removal, mud dirt, tar and part light oil, and total phenol is 6186mg/L, and wherein volatile phenol is 4840mg/L,
Total ammonia is 11116mg/L, and wherein free ammonia is 10250mg/L, and oil is 258mg/L, and waste water pH value is 9.4, process step
Be the same as Example 1, concrete technology condition is：
In step (1), saturator 1 uses plate column, and operation temperature is 48.8 DEG C, and operating pressure is 0.20MPa, theoretical tower
Plate number is 14, and the waste water pH value of oil-containing, phenol and ammonia after sour gas saturation is 7.2.
In step (2), extraction tower 2 uses turntable extracting tower, and extraction theory series is 4 grades, the volume of extractant and waste water
Than for 1:7, extraction temperature is 50 DEG C, and extracting pressure is 0.20MPa, and extraction pH value is 7.2.
In step (3), the tower top pressure of phenol tower 3 is 0.22MPa, and temperature is 157 DEG C, and tower bottom pressure is 0.24MPa, and temperature is
250℃；Reflux ratio is 0.24, and the number of plates is 18.
In step (4), the volume ratio of 4 hot and cold two bursts of chargings of extracting tower is 1:3, tower top pressure is 0.40MPa, and temperature is
102 DEG C, tower bottom pressure is 0.42MPa, and temperature is 150 DEG C, and the number of plates is 28.
In step (5), the tower top pressure of deammoniation tower 5 is 0.48MPa, and temperature is 152 DEG C, and tower bottom pressure is 0.50MPa, temperature
For 159 DEG C, the number of plates is 30.The temperature of one-level segregator 10 is 130 DEG C, and pressure is 0.38MPa；The temperature of two-stage fractional condensation device 11
For 80 DEG C, pressure is 0.34MPa；The temperature of three-level segregator 12 is 40 DEG C, and pressure is 0.20MPa.Three-level fractional condensation device is produced
The fractional condensation liquid of 90% volume flow return to the top of deammoniation tower 5 as backflow, the fractional condensation liquid of remaining 10% volume delivers to extracting tower 4
Hot feed pipeline.The sodium hydroxide solution addition that mass concentration is 32wt% is the wastewater quality into deammoniation tower 5
0.4wt%.It is 397mg/L that total phenol content in the waste water of biochemical treatment apparatus is sent after processing, and wherein volatile phenol is 73mg/L, and oil contains
Measure as 55mg/L, total ammonia content is 105mg/L.
Embodiment 4
Pending waste water chooses the waste water of oil-containing, phenol and ammonia that the gasification of fixed bed slag is produced, through coal gas water separation device
Go after oil removal, mud dirt, tar and part light oil, total phenol is 5065mg/L, wherein volatile phenol is 3234mg/L, and total ammonia is
25506mg/L, wherein free ammonia are 22420mg/L, and oil is 582mg/L, and waste water pH value is 9.8, and process step is same to be implemented
Example 1, concrete technology condition is：
In step (1), saturator 1 uses plate column, and operation temperature is 45 DEG C, and operating pressure is 0.05MPa, theoretical tray
Number is 16, and the waste water pH value of oil-containing, phenol and ammonia after sour gas saturation is 8.0.
In step (2), extraction tower 2 uses perforated-plate extraction tower, and extraction series is 6 grades, and the volume ratio of extractant and waste water is
1:8, extraction temperature is 45 DEG C, and extracting pressure is 0.10MPa, and extraction pH value is 8.0.
In step (3), the tower top pressure of phenol tower 3 is 0.3MPa, and temperature is 164 DEG C, and tower bottom pressure is 0.32MPa, and temperature is
255℃；Reflux ratio is 0.26, and the number of plates is 20.
In step (4), the tower top pressure of extracting tower 4 is 0.33MPag, and temperature is 99 DEG C, and tower bottom pressure is 0.45MPa, temperature
For 152 DEG C,
In step (5), the tower top pressure of deammoniation tower 5 is 0.43MPa, and temperature is 148 DEG C, and tower bottom pressure is 0.45MPa, temperature
For 156 DEG C, the number of plates is 30.The temperature of one-level segregator 10 is 128 DEG C, and pressure is 0.35MPa；The temperature of two-stage fractional condensation device 11
For 84 DEG C, pressure is 0.28MPa；The temperature of three-level segregator 12 is 40 DEG C, and pressure is 0.15MPa.Three-level fractional condensation device is produced
The fractional condensation liquid of 85% volume flow return to the top of deammoniation tower 5 as backflow, the fractional condensation liquid of remaining 15% volume delivers to extracting tower 4
Hot feed pipeline.The sodium hydroxide solution addition that mass concentration is 40wt% is the wastewater quality into deammoniation tower 5
0.8wt%.It is 315mg/L that total phenol content in the waste water of biochemical treatment apparatus is sent after processing, and wherein volatile phenol is 27mg/L, and oil contains
Measure as 67mg/L, total ammonia content is 56mg/L.
Claims (13)
1. a kind of method for handling oil-containing coal gasification waste water, it is characterised in that comprise the following steps：
(1) sour gas saturation process：Oil-containing coal gasification waste water enters from saturator top, and sour gas enters from saturator bottom
Enter, the oil-containing coal gasification waste water after acidifying is discharged from saturation tower bottom, feeding extraction tower top, the sour gas not absorbed by waste water
Enter to come out at the top of scrubbing tower after scrubbing tower bottom, dilute phenol water washing after deamination from the top of saturator 1 and send at sulfur recovery
Reason, the waste water that wash tower bottoms come out enters in saturator together with oil-containing coal gasification waste water；
(2) solvent extraction dephenolize and oily process：Into extraction tower waste water with entering the extractant adverse current in tower from extraction tower bottom
Contact carries out multi-stage counter current extraction, and the waste water after removing phenol and oil, the richness come out from extraction tower top are come out from extraction tower bottom
The extraction phase of oil-containing and phenol enters extract groove；
(3) extractant and carbolic oil separation circuit：The extraction phase rich in oil and phenol in extract groove passes through with going out from phenol tower tower reactor
The extractant that the carbolic oil and phenol column overhead come comes out enters phenol tower after exchanging heat respectively, and the carbolic oil that phenol tower tower reactor comes out is after heat exchange
To tank field is delivered to, the extractant that phenol column overhead is distilled enters solvent circulating slot after heat exchange, afterwards in solvent circulating slot
An extractant part send extraction tower to recycle, another part extractant is returned in phenol tower；
(4) depickling and residual solvent recovery process：The waste water part after removing phenol and oil is come out as de- from extraction tower bottom
The cold feed of acid tower enters from extracting tower top, and dilute phenol water of the another part after the deamination with being come out from deammoniation tower exchanges heat it
Enter afterwards as hot feed in the middle part of the extracting tower, the sour gas that is come out from extracting tower top and the solvent in being dissolved in waste water it is mixed
Close gas and enter cooler, acid qi leel flow container is entered afterwards and carries out solution-air-liquid three phase separation, what acid qi leel flow container was isolated
Sour gas returns to saturator, and upper phase extractant is returned in solvent circulating slot, and lower floor's liquid phase aqueous solution returns to extracting tower,
The dilute phenol water sprayed into heat-exchange tube of cooler after deamination；
(5) deamination process：Waste water enters from deammoniation tower top after the depickling come out from depickling tower bottom, while from deammoniation tower top
Sodium hydroxide solution is added, the ammoniacal liquor vapour come out from deamination column overhead enters three be made up of three heat exchangers and three segregators
Level fractional condensation device carries out concentration purification, and the fractional condensation liquid that fractional condensation liquid phase enters in ammonia condensate tank, ammonia condensate tank afterwards is largely returned
As backflow at the top of deammoniation tower, fraction fractional condensation liquid delivers to extracting tower, after the rich ammonia come out from last segregator enters
Into ammoniacal liquor or liquefied ammonia, the desulphurization and denitration in factory is used or as production marketing continuous ammonia refining unit style；Go out from deamination tower bottom
A dilute phenol water part after the deamination come is delivered in scrubbing tower and cooler, and another part delivers to subsequent biochemical processing.
2. a kind of method for handling oil-containing coal gasification waste water as claimed in claim 1, it is characterised in that in the step (1)
Sour gas is carbon dioxide.
3. a kind of method for handling oil-containing coal gasification waste water as claimed in claim 1, it is characterised in that in the step (1)
The pH value of waste water after being acidified in saturator 1 is 6.5-8.5.
4. a kind of method for handling oil-containing coal gasification waste water as claimed in claim 1, it is characterised in that in the step (1)
Saturator is plate column or packed tower, and saturation temperature is 20-60 DEG C, and pressure is 0.02-0.30MPa, and the number of plates is 10-20
Block.
5. a kind of method for handling oil-containing coal gasification waste water as claimed in claim 1, it is characterised in that in the step (2)
Extractant is methyl iso-butyl ketone (MIBK).
6. a kind of method for handling oil-containing coal gasification waste water as claimed in claim 1, it is characterised in that in the step (2)
The PH of aqueous phase is 6.5-8.5 in extraction tower, and extraction temperature is 20-60 DEG C, and extracting pressure is 0.02-0.40MPa, and extractant is with entering
The volume ratio for entering the waste water of extraction tower is 1:3-10, extraction series is 4-8 grades.
7. a kind of method for handling oil-containing coal gasification waste water as claimed in claim 1, it is characterised in that in the step (2)
Extraction tower is turntable extracting tower or packed extraction tower or perforated-plate extraction tower.
8. a kind of method for handling oil-containing coal gasification waste water as claimed in claim 1, it is characterised in that in the step (3)
Phenol tower is plate column, and tower top temperature is 110-170 DEG C, and bottom temperature is 200-260 DEG C, and pressure is 0.02-0.32MPa, backflow
Than for 0.15-0.26, the number of plates is 15-20 blocks.
9. a kind of method for handling oil-containing coal gasification waste water as claimed in claim 1, it is characterised in that in the step (4)
Extracting tower is to remove sour gas together with remaining in the extractant in waste water, and the volume ratio of cold feed and hot feed is 1:3-6,
Tower top temperature is 90-110 DEG C, and bottom temperature is 135-160 DEG C, and pressure is 0.25-0.55MPa, and the number of plates is 22-30 blocks.
10. a kind of method for handling oil-containing coal gasification waste water as claimed in claim 1, it is characterised in that in the step (5)
Deammoniation tower be plate column, tower top temperature be 135-160 DEG C, bottom temperature be 145-165 DEG C, pressure is 0.30-0.60MPag,
The number of plates is 25-30 blocks.
11. a kind of method for handling oil-containing coal gasification waste water as claimed in claim 1, it is characterised in that in the step (5)
Ammonia condensate tank in 70%-90% volume flows fractional condensation liquid return deammoniation tower at the top of as backflow, remaining 10%-30% volume
Fractional condensation liquid deliver to extracting tower 4.
12. a kind of method for handling oil-containing coal gasification waste water as claimed in claim 1, it is characterised in that in the step (5)
Deammoniation tower top add mass concentration be 20-40wt% sodium hydroxide solution, addition be enter deammoniation tower waste water matter
The 0.2-1.0wt% of amount.
13. a kind of method for handling oil-containing coal gasification waste water as claimed in claim 1, it is characterised in that the step (5) from
It is ammoniacal liquor vapour that the ammoniacal liquor vapour that deamination column overhead comes out, which enters the three-level fractional condensation device being made up of three heat exchangers and three segregators,
One-level heat exchanger is introduced into, afterwards into one-level segregator, two grades heat exchangers are entered back into, afterwards into two-stage fractional condensation device,
Three-level heat exchanger is finally entered, afterwards into three-level segregator.
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| CN201611117273.XA CN107032555A (en) | 2016-12-07 | 2016-12-07 | A kind of method for handling oil-containing coal gasification waste water |
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| CN201611117273.XA CN107032555A (en) | 2016-12-07 | 2016-12-07 | A kind of method for handling oil-containing coal gasification waste water |
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| CN111252981A (en) * | 2020-02-10 | 2020-06-09 | 青岛科技大学 | Method and device for treating oily coal chemical wastewater |
| CN112316487A (en) * | 2020-11-02 | 2021-02-05 | 湘潭大学 | Method for continuously extracting phenol mixture and equipment adopting method |
| CN112624466A (en) * | 2020-11-27 | 2021-04-09 | 陕西德信祥能源科技有限公司 | Coal chemical industry wastewater pretreatment method |
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| CN111252981A (en) * | 2020-02-10 | 2020-06-09 | 青岛科技大学 | Method and device for treating oily coal chemical wastewater |
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Application publication date: 20170811 |