CN103496812A - Method for treating high-concentration phenol-ammonia wastewater - Google Patents
Method for treating high-concentration phenol-ammonia wastewater Download PDFInfo
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Abstract
The invention relates to a method for treating high-concentration phenol-ammonia coal gasification wastewater. The method takes butyl acetate as an extraction agent and comprises the steps of firstly extracting by use of a phenol extraction tower to remove phenols contained in the wastewater, removing the acid gas and ammonia in the wastewater by use of an acid and ammonia removal tower, and recovering the extraction agent in the extraction phase by use of a solvent stripping tower so as to obtain a crude phenol product from the bottom of the tower. The method provided by the invention realizes high-purity removal of the phenols, acid gas, free ammonia and solid ammonia in the coal gasification wastewater so as to meet the requirement of biochemical treatment on the inflow water quality, and obtains the crude phenol product and high-concentration ammonia gas. Compared with the prior art, the method provided by the invention has the advantages of good extraction effect, high phenol removal efficiency, short process flow and low treatment cost; the method is simple and convenient to operate, and the treatment quality is reliable.
Description
Technical field
The present invention relates to the high-concentration phenol and ammonia technical field of waste water processing, particularly depickling deamination the N-BUTYL ACETATE of take are processed the method for high-concentration phenol ammonia waste water as extraction agent again in a kind of first dephenolize.
Background technology
Gasification is to clean, efficiently utilize the effective means of coal, is widely used in the industry such as gas maked coal, coal liquefaction, coal power generation, but has also brought serious problem of environmental pollution.Produce a large amount of high pollution waste water, the pollutents such as the phenol that contains high density, ammonia, sour gas in gasification, coal liquefaction, coal tar process.For this class waste water, just can enter follow-up biochemical treatment after must taking certain technique to remove wherein the phenol of the overwhelming majority, ammonia, sour gas.
Existing high-concentration phenol and ammonia waster water process is a lot, ubiquitous outstanding shortcoming is: 1) deacidifying process is unreasonable, make the sour gas such as carbonic acid gas, hydrogen sulfide of the ionic state of dissolving in waste water can not be converted into cost-effectively free state, cause the residual quantity of sour gas too high; 2) existing extraction agent is not high for the removal efficiency of the polyphenol in waste water, causes in waste water polyphenol content higher, is difficult to reach the requirement of biochemical treatment; When 3) ammonia content in waste water is high, the fluctuation of service of deammoniation tower, because extracted amount, the internal circulating load of ammonia are large, often cause the deammoniation tower tower to be pressed unstable, and the ammonia content of purifying waste water fluctuation is large.
Existence due to above problem, the technique that also there is no at present a kind of mature and reliable, stable operation, make most coal chemical industrial waste waters can meet continuously and stably the requirement of biochemical treatment after pretreatment, cause the still state in discharge beyond standards of a large amount of coal chemical industrial waste waters.
Summary of the invention
The object of the invention is to overcome the defect that prior art exists, provide a kind of first dephenolize again the depickling deamination contain the method for high-concentration phenol and ammonia wastewater treatment, the method can remove phenol, sour gas and ammonia effectively, and can reduce solvent loss.
For achieving the above object, the present invention is achieved like this, and its processing method step is:
(1) waste water extracting and dephenolizing: the coal gasification waste water of carbonated, hydrogen sulfide, ammonia and phenol is sent into to extraction tower top, the N-BUTYL ACETATE of take carries out counter-current extraction as extraction agent, wherein, the volume ratio of N-BUTYL ACETATE and waste water is 1:1-1:15, and tower top pressure is that 0.2-0.4 MPa, temperature are 40-75 ℃; Tower bottom pressure is that 0.2-0.4 MPa, temperature are 120 ℃, makes extraction phase and raffinate waste water;
(2) waste water depickling deamination: step (1) gained raffinate waste water is divided into to hot and cold two strands and sends into the processing of deamination extracting tower, the tower reactor temperature is 130 ~ 170 ℃, tower reactor pressure is 0.3 ~ 0.7MPa, the cold feed temperature is 40 ~ 80 ℃, hot feed is 120 ~ 155 ℃, hot and cold charge ratio is 1:2 ~ 6, extract ammonia out from depickling deammoniation tower middle and upper part, concentrate and make with extra care through three grades of fractional condensation devices that formed by partial condenser and minute flow container, the temperature of one-level fractional condensation device is 110-150 ℃, and pressure is 0.4-0.65 MPa; The temperature of two-stage fractional condensation device is 70-90 ℃, and pressure is 0.3-0.5 MPa, the working pressure 0.21-0.28 MPa of three grades of partial condensers, and service temperature is 36-40 ℃; The ammonia obtained through the fractional condensation of three grades of fractional condensation devices is sent to the ammonia concentrating unit; Partial condenser bottom liquids at different levels enter gun barrel and are divided into the profit two-phase, gun barrel top oil phase as extraction agent extraction be sent to solvent tank, aqueous-phase reflux is to the deamination extracting tower; Deamination extracting tower top sour gas send treatment unit or directly burns; Waste water after deamination extracting tower depickling deamination is delivered in the raw material mixing tank with waste water stoste is mixed and is delivered to extraction tower from depickling deammoniation tower bottom extraction rear portion, and a part is delivered to biochemical section and carried out biochemical treatment;
(3) solvent recuperation: step (1) gained extraction phase is sent into to the solvent stripping tower, and the control tower pressure on top surface is 0.1-0.2 MPa, and tower top temperature is 80-120 ℃, and tower bottom pressure is 0.1-0.2 MPa, and column bottom temperature is 90-120 ℃; The extraction agent of overhead extraction, after cooling recovery, is delivered to solvent tank to recycle, and still liquid is the meal product after treatment.
The inventive method compared with prior art, has following advantage:
(1) using N-BUTYL ACETATE as extraction agent, aldehydes matter in first extraction wastewater carries out the depickling deamination again, makes to extract phenol concentration in rear waste water and is down to biochemical treatment and enters below the phenol concentration that water requires, and has effectively shortened processing technological flow, improve processing efficiency, reduced processing cost;
(2) acid gas removal body and deamination carry out in same tower, have simplified technical process, have reduced process cost;
(3) effectively volatile phenol is separated from ammoniacal liquor, alleviated the refining energy consumption of follow-up ammonia and purified load;
(4) can effectively remove the lower boiling oil pollutant simultaneously.
The accompanying drawing explanation
Fig. 1 is sewage treatment technology process schematic diagram of the present invention.
Embodiment
The present invention processes the method for high-concentration phenol ammonia waste water, to be summed up on the basis of practical experience by the contriver, by the research of long term and a large amount of test gained, this first uses the extraction of phenol extraction tower to remove phenols contained in waste water, and using N-BUTYL ACETATE as extraction agent, not only can avoid the too high impact of waste water basicity, without adding acidic medium to carry out the adjustment of pH value, and have high to aldehydes matter solubleness, separate the characteristics such as fast.Then, use the depickling deammoniation tower to remove sour gas and the ammonia in waste water, there are like this characteristics such as waste water treatment efficiency is high, to remove phenol, ammonia and sour gas effective, and the treating processes power consumption is few; And use the solvent stripping tower to carry out recycle and reuse to the extraction agent in extraction phase, make the consumption of extraction agent seldom.Present method is in wastewater treatment process, can arbitrarily adjust according to the concentration of target processing quality index and Phenol for Waste Water class, sour gas, free ammonia and fixed ammonia, waste water is arbitrarily carried out to repeatedly dephenolize, ammonia and sour gas circular treatment, thereby guarantee that reliably wastewater treatment is up to standard, make processed waste water can reach the requirement of biochemical treatment influent quality.The present invention realizes that coal gasification waste water removes higher phenols and rudimentary phenol, sour gas, free ammonia and fixed ammonia, and obtains crude phenols product and high density ammonia.Test shows, the method effect of extracting is good, and dephenolize efficiency is high, and solvent loss is little.
As shown in Figure 1, the present invention processes the method for high-concentration phenol ammonia waste water, is to carry out in the steps below:
(1) waste water extracting and dephenolizing: first the coal gasification waste water of carbonated, hydrogen sulfide, ammonia and phenol is sent into to raw material mixing tank 1, send into extraction tower 2 with feedstock pump 17 by top again, sent into extraction tower 2 using N-BUTYL ACETATE as extraction agent from bottom by solvent tank 8, carry out counter-current extraction, wherein, the volume ratio of N-BUTYL ACETATE and waste water is 1:1-1:15, and extraction tower 2 pressure on top surfaces are that 0.2-0.4 MPa, temperature are 75 ℃; Extraction tower 2 bottom pressures are that 0.2-0.4 MPa, temperature are 120 ℃, by extraction tower 2 tops and bottom, receive respectively to obtain extraction phase and raffinate waste water;
(2) waste water depickling deamination: step (1) gained raffinate waste water is sent into to deamination extracting tower 3 by middle part and process, extract ammonia out from depickling deammoniation tower 3 middle and upper parts, concentrate and make with extra care via partial condenser 16,14,13 and minute flow container 4,5,6 three grades of fractional condensation devices that correspondence forms respectively, the temperature of one-level fractional condensation device (being comprised of partial condenser 16 and minute flow container 4) is 110-150 ℃, and pressure is 0.4-0.65 MPa; The temperature of two-stage fractional condensation device (being comprised of partial condenser 14 and minute flow container 5) is 70-90 ℃, and pressure is 0.3-0.5 MPa; The working pressure 0.21-0.28 MPa of three grades of fractional condensation devices (being formed by partial condenser 13 and minute flow container 6), service temperature is 36-40 ℃; The ammonia obtained through the fractional condensation of three grades of fractional condensation devices is sent to the ammonia concentrating unit and is concentrated; Partial condenser 16,14,13 bottom liquids at different levels enter gun barrel 7 and are separated into oil, water two-phase, and the oil phase on gun barrel 7 tops reclaims as extraction agent extraction and is sent to solvent tank 8 and carries out recycle.Aqueous-phase reflux is circulated and is processed to deamination extracting tower 3; Deamination extracting tower 3 top sour gas are delivered to that treatment unit is processed or are directly burned; Waste water after deamination extracting tower 3 depickling deaminations is delivered in raw material mixing tank 1 with waste water stoste is mixed and is delivered to extraction tower 2 circular treatment from depickling deammoniation tower 3 bottom extraction rear portion, a part is delivered to biochemical section and is carried out biochemical treatment, phenol ammonia content and the wastewater treatment quality objectives of two-part allocation proportion in the high-concentration phenol ammonia waste water determined, and can reach thus the processing target of any quality;
(3) solvent recuperation: step (1) gained extraction phase is sent into to solvent stripping tower 9, and controlling solvent stripping tower 9 pressure on top surfaces is that 0.1-0.2 MPa, temperature are 80-120 ℃, and solvent stripping tower 9 bottom pressures are that 0.1-0.2 MPa, temperature are 90-120 ℃; , delivered to solvent tank 8 and recycled after cooling recovery by the extraction agent of solvent stripping tower 9 top extraction, it is the meal product after treatment that still liquid is delivered to treatment facility by crude phenols pump 11.Number in the figure 10 is reboiler, and label 12,15 is condenser.
Below in conjunction with the drawings and specific embodiments, the present invention will be further described.
Apply the device of above-mentioned processing containing phenol ammonia coal gasification waste water, the coal gasification waste water total phenol content is 16798 mg/L, free ammonia 2018 mg/L, fixed ammonia 1864 mg/L, CO
22435 mg/L, the pH value is 8.7,65 ℃ of water temperatures, flow 107 t/h, processed by flow process shown in Fig. 1.Phenol extraction tower 2 adopts packing tower, 80 ℃ of tower top temperatures, tower top pressure 0.3 MPa, 120 ℃ of column bottom temperatures, tower bottom pressure 0.35 MPa.Depickling deammoniation tower 3 is tray column, 120 ℃ of tower top temperatures, and tower top pressure 0.32 MPa, 160 ℃ of column bottom temperatures, tower bottom pressure 0.36 MPa, middle and upper part gas produced quantity is 3425 kg/h, the overhead gas produced quantity is 3653 kg/h.Three grades of fractional condensation one-level partial condensers working pressure be 0.51 MPa, service temperature is 135.4 ℃; The working pressure of two-stage fractional condensation device is 0.34 MPa, and service temperature is 91 ℃; Working pressure 0.24 MPa of three grades of partial condensers, service temperature is 38 ℃.Solvent stripping tower 9 tower top pressure 0.27 MPa, 85 ℃ of tower top temperatures, tower bottom pressure 0.31 MPa, 135 ℃ of column bottom temperatures, reflux ratio 0.384.Total phenol content 352 mg/L in waste water after processing, free ammonia 25.7 mg/L, fixed ammonia 166.7 mg/L, the carbonic acid gas trace, hydrogen sulfide does not detect.
Apply the device of above-mentioned processing containing phenol ammonia coal gasification waste water, the coal gasification waste water total phenol content is 5364 mg/L, free ammonia 1034 mg/L, fixed ammonia 1508 mg/L, CO
22352 mg/L, the pH value is 7.8,72 ℃ of water temperatures, flow 94 t/h, processed by flow process shown in Fig. 1.Phenol extraction tower 2 adopts packing tower, 78 ℃ of tower top temperatures, tower top pressure 0.28 MPa, 119 ℃ of column bottom temperatures, tower bottom pressure 0.32 MPa.Depickling deammoniation tower 3 is tray column, 117 ℃ of tower top temperatures, and tower top pressure 0.31 MPa, 155 ℃ of column bottom temperatures, tower bottom pressure 0.34 MPa, middle and upper part gas produced quantity is 2357 kg/h, the overhead gas produced quantity is 3294 kg/h.Three grades of fractional condensation one-level partial condensers working pressure be 0.54 MPa, service temperature is 133.7 ℃; The working pressure of two-stage fractional condensation device is 0.38 MPa, and service temperature is 95 ℃; Working pressure 0.21 MPa of three grades of partial condensers, service temperature is 40 ℃.Solvent stripping tower 9 tower top pressure 0.28 MPa, 82 ℃ of tower top temperatures, tower bottom pressure 0.33 MPa, 142 ℃ of column bottom temperatures, reflux ratio 0.377.Total phenol content 368mg/L in waste water after processing, free ammonia 33.2 mg/L, fixed ammonia 139.8 mg/L, the carbonic acid gas trace, hydrogen sulfide does not detect.
Apply the device of above-mentioned processing containing phenol ammonia coal gasification waste water, the coal gasification waste water total phenol content is 4381 mg/L, free ammonia 1285 mg/L, fixed ammonia 1438 mg/L, CO
23452 mg/L, the pH value is 7.2,75 ℃ of water temperatures, flow 116 t/h, processed by flow process shown in Fig. 1.Phenol extraction tower 2 adopts packing tower, 82 ℃ of tower top temperatures, tower top pressure 0.33 MPa, 127 ℃ of column bottom temperatures, tower bottom pressure 0.35 MPa.Depickling deammoniation tower 3 is tray column, 118 ℃ of tower top temperatures, and tower top pressure 0.30 MPa, 166 ℃ of column bottom temperatures, tower bottom pressure 0.36 MPa, middle and upper part gas produced quantity is 4176 kg/h, the overhead gas produced quantity is 2787 kg/h.Three grades of fractional condensation one-level partial condensers working pressure be 0.55 MPa, service temperature is 137.6 ℃; The working pressure of two-stage fractional condensation device is 0.35 MPa, and service temperature is 93 ℃; Working pressure 0.28 MPa of three grades of partial condensers, service temperature is 36 ℃.Solvent stripping tower 9 tower top pressure 0.22 MPa, 86 ℃ of tower top temperatures, tower bottom pressure 0.33 MPa, 139 ℃ of column bottom temperatures, reflux ratio 0.393.Total phenol content 434 mg/L in waste water after processing, free ammonia 24.6 mg/L, fixed ammonia 119.5 mg/L, the carbonic acid gas trace, hydrogen sulfide does not detect.
Claims (1)
1. a method of processing the high-concentration phenol ammonia waste water, it is characterized in that: its processing method step is:
(1) waste water extracting and dephenolizing: the coal gasification waste water of carbonated, hydrogen sulfide, ammonia and phenol is sent into to extraction tower top, the N-BUTYL ACETATE of take carries out counter-current extraction as extraction agent, wherein, the volume ratio of N-BUTYL ACETATE and waste water is 1:1-1:15, and tower top pressure is that 0.2-0.4 MPa, temperature are 75 ℃; Tower bottom pressure is that 0.2-0.4 MPa, temperature are 120 ℃, makes the remaining liquid of extraction liquid and extraction;
(2) waste water depickling deamination: the remaining liquid of step (1) gained extraction is sent into to the deamination extracting tower and process, extract ammonia out from depickling deammoniation tower middle and upper part, concentrate and make with extra care through three grades of fractional condensation devices that formed by partial condenser and minute flow container, the temperature of one-level fractional condensation device is 110-150 ℃, and pressure is 0.4-0.65 MPa; The temperature of two-stage fractional condensation device is 70-90 ℃, and pressure is 0.3-0.5 MPa; The ammonia obtained through the fractional condensation of three grades of fractional condensation devices is sent to the ammonia concentrating unit; Partial condenser bottom liquids at different levels enter gun barrel and are divided into the profit two-phase, gun barrel top oil phase as extraction agent extraction be sent to solvent tank, aqueous-phase reflux is to the deamination extracting tower; Deamination extracting tower top sour gas send treatment unit or directly burns; Deliver to extraction tower in wastewater trough before a waste water part after deamination extracting tower depickling deamination is delivered to the solvent stripping tower from the bottom extraction of depickling deammoniation tower with after waste water stoste is mixed, a part is delivered to biochemical section and is carried out biochemical treatment;
(3) solvent recuperation: step (1) gained extraction liquid is sent into to the solvent stripping tower, and the control tower pressure on top surface is 0.1-0.2 MPa, and tower top temperature is 80-120 ℃, and tower bottom pressure is 0.1-0.2 MPa, and column bottom temperature is 90-120 ℃; The extraction agent of overhead extraction, after cooling recovery, is delivered to solvent tank to recycle, and still liquid is the meal product after treatment.
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Cited By (5)
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| CN103964543A (en) * | 2014-05-06 | 2014-08-06 | 河南龙成煤高效技术应用有限公司 | Method for oil and phenol removal from wastewater in field of coal chemical industry |
| CN104276618A (en) * | 2014-10-30 | 2015-01-14 | 河南龙成煤高效技术应用有限公司 | Dephenolizing extraction agent for coal chemical wastewater and use thereof and method for dephenolizing coal chemical wastewater |
| CN105948153A (en) * | 2016-05-25 | 2016-09-21 | 北京中科瑞奥能源科技股份有限公司 | System and process for treating and utilizing phenol-ammonia wastewater |
| CN107311383A (en) * | 2017-08-23 | 2017-11-03 | 赛鼎工程有限公司 | A kind of method for handling oil-containing coal gasification waste water |
| CN110540329A (en) * | 2019-09-09 | 2019-12-06 | 陕西煤业化工集团神木天元化工有限公司 | Phenol-ammonia wastewater treatment method and system |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103964543A (en) * | 2014-05-06 | 2014-08-06 | 河南龙成煤高效技术应用有限公司 | Method for oil and phenol removal from wastewater in field of coal chemical industry |
| CN103964543B (en) * | 2014-05-06 | 2016-01-27 | 河南龙成煤高效技术应用有限公司 | A kind of method of coal chemical technology waste water oil removing dephenolize |
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| CN105948153A (en) * | 2016-05-25 | 2016-09-21 | 北京中科瑞奥能源科技股份有限公司 | System and process for treating and utilizing phenol-ammonia wastewater |
| CN107311383A (en) * | 2017-08-23 | 2017-11-03 | 赛鼎工程有限公司 | A kind of method for handling oil-containing coal gasification waste water |
| CN110540329A (en) * | 2019-09-09 | 2019-12-06 | 陕西煤业化工集团神木天元化工有限公司 | Phenol-ammonia wastewater treatment method and system |
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Application publication date: 20140108 |