CN1884150A - Method for treating coal gasification wastewater by single-tower pressurization stripping and device therefor - Google Patents
Method for treating coal gasification wastewater by single-tower pressurization stripping and device therefor Download PDFInfo
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- CN1884150A CN1884150A CN 200610036072 CN200610036072A CN1884150A CN 1884150 A CN1884150 A CN 1884150A CN 200610036072 CN200610036072 CN 200610036072 CN 200610036072 A CN200610036072 A CN 200610036072A CN 1884150 A CN1884150 A CN 1884150A
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Abstract
The invention discloses a gasification wastewater disposing method and device through single-tower pressurizing stripping, which comprises the following steps: entering the extracted of acid gas or ammonia gas of cold and hot coal gasification wastewater from band lateral line in the stripping tower from top and upper top; blending gas; dividing phases; washing; separating light oil and acid gas; preparing liquid ammonia through two-grade concreting and refining; separating crude phenol and organic solvent from bottom of tower through inversed-extracting autoclave liquid and organic solvent; recycling organic solvent through stripping. The gasification disposing device contains oil acid gas/ammonia stripping tower, extracting tower, acid gas washing tower, solvent stripping tower, solvent recycling tower, oil-water separator, dephlegmator, pump and reservoir.
Description
Technical field
The present invention relates to the processing recovery method of coal gasification waste water, particularly a kind of method for the treatment of coal gasification wastewater by single-tower pressurization stripping.
The invention still further relates to a kind of device of realizing aforesaid method.
Background technology
Lasting high along with oil price, coal more and more comes into one's own in the application of the energy and chemical field.Gasification is to clean, efficiently utilize the effective means of coal, is widely used in the industry such as gas maked coal, synthetic ammonia, coal power generation.Lurgi pressure gasification technology is to use one of maximum gasifying process at present, in this technological process, produces a large amount of high pollution waste water, wherein: COD
CrContent is at 20000mgl
-1More than, being meta-alkalescence, water quality is very complicated.Also contain a large amount of phenol, ammonia, CO in the waste water
2, pollutents such as lipid acid, tar, ketone and amine, wherein, phenol content is high and of a great variety, existing unit phenol has polyphenol again, is difficult to biological degradation.
For such waste water, the mode that generally adopts the chemical separating flow process to combine with biochemical treatment is handled both at home and abroad.Chemical separating comprises unit processes such as extraction, stripping, to remove sour gas, reclaims phenol, ammonia etc.From what we've been able to figure out, the operation of such separation process is generally undesirable.Waste water is removed H through pre-treatment such as flash distillation, sedimentations
2, CH
4And behind tar and the part light oil, enter the acid gas stripping tower and remove CO
2, H
2Sour gas such as S enter the extraction tower extracting and dephenolizing then.Extraction solvent generally adopts diisopropyl ether, and extraction tower is a rotating disc contactor.Waste water after the extraction carries out biochemical treatment through entering biochemical treatment workshop section after deamination and the solvent recuperation again.The running condition of this flow process is very undesirable at present, and the most outstanding shortcoming has two: the one, and dephenolization effect is bad, and the total phenol concentration of processed waste water is still up to 1400mgl
-1About, COD
CrValue 6000mgl
-1More than.Not only cause the waste of phenol, and, be difficult to realize qualified discharge because phenol content and pollution load have substantially exceeded biochemical section processing power, the 2nd, the fouling of equipment is serious with obstruction, has influenced plant efficiency and normal operation.
Extract in the existing technology and before deamination, carries out because the existence of a large amount of ammonia is arranged, waste water be alkalescence on the weak side cause except that phenol efficient low.Ionization takes place in aldehydes matter hardly under acidic conditions, exist with molecularity, and under the alkaline environment when pH＞8, phenol begins to take place ionization (is example with phenol):
When pH＞9, it is more remarkable to dissociate.The PhO of ionic state
-The group wetting ability strengthens, and the solubleness in water increases substantially, thereby causes effect of extracting to worsen.The effective measure of improving effect of extracting are that the pH with when extraction is reduced to below 7, but because the existence of ammonia, water per ton need add hydrochloric acid more than 40 kilograms, is difficult to economically bear.Therefore, under the present technology, pollution load is reduced to satisfies the degree that biochemical workshop section requires.
The fouling of equipment is serious with obstruction in the existing technology.Because CO
2The residual quantity height, and deamination in the end carries out, so more CO is arranged in the operational process always
2With the ammonia coexistence, both easily are deposited on the appts wall in conjunction with producing ammonium salt crystallization (bicarbonate of ammonia, volatile salt), have influenced plant efficiency and normal operation.
Summary of the invention
The objective of the invention is to defective, a kind of method for the treatment of coal gasification wastewater by single-tower pressurization stripping is provided at prior art.
The present invention also aims to provide a kind of device of realizing aforesaid method.
The method for the treatment of coal gasification wastewater by single-tower pressurization stripping of the present invention comprises the steps:
(1) stripping depickling deamination: it is cold that coal gasification waste water is divided, two bursts of stripping tower top and middle and upper parts of extracting out from the band side line of heat enter in the tower, making tower top pressure is 0.2～0.6MPa, 40～80 ℃ of temperature, tower bottom pressure is 0.25～0.6MPa, 120～160 ℃ of temperature, going out gas mixture from the cat head stripping is 0.25～0.45MPa at pressure, temperature is fractional condensation under 110～150 ℃ the condition, then through phase-splitting, ammonia is isolated in washing, sour gas, light oil and water, reclaim light oil, backflow ammonia, water is discharged sour gas and burning, from side line extraction ammoniacal liquor gas through the two-stage fractional condensation, the liquid phase that refluxes then, refining gas phase, extraction still liquid at the bottom of the tower;
(2) extracting and dephenolizing: send into extraction tower top and organic solvent counter-current extraction after the still liquid of step (1) extraction is cooled to 45 ℃, the volume ratio that makes organic solvent and water is 1: 10～1: 6, extraction pH value is 4～7, temperature is 20～60 ℃, deliver to the solvent recovery tower from extraction tower cat head extraction extraction phase, making the recovery tower tower top pressure is 0.1～0.2MPa, 105～120 ℃ of temperature, tower bottom pressure is 0.1～0.2MPa, 200～220 ℃ of temperature, reflux ratio 0.2～0.4 goes out crude phenols and organic solvent through rectifying separation, the loopback organic solvent to be recycling, extraction extracting phase at the bottom of the extraction Tata;
(3) reclaim solvent: the extracting phase of step (2) extraction is delivered to the solvent stripping tower, making tower top pressure is 0.1～0.2MPa, 60～90 ℃ of temperature, tower bottom pressure is 0.1～0.2MPa, and 100～110 ℃ of temperature go out gaseous mixture condensation from the cat head stripping, then at 30～60 ℃ of following phase-splittings branch water outlet in 10～30 minutes and organic solvent, recirculation water, loopback organic solvent to be recycling, and extraction still liquid carries out biochemical treatment at the bottom of the tower.
Organic solvent is diisopropyl ether or hexone described in the step (2).
A kind of device of realizing aforesaid method contains oleic acid gas/aminoacid stripping tower, extraction tower, acid gas washing tower, solvent stripping tower, solvent recovery tower, water-and-oil separator, partial condenser, pump, storage tank, wherein:
Feed pipe connects the opening for feed of oleic acid gas/aminoacid stripping tower, acid gas washing tower by pump, the cat head of acid gas/aminoacid stripping tower connects partial condenser, the two ends outlet of partial condenser connects the import of acid gas washing tower and water-and-oil separator respectively, connect acid gas/aminoacid stripping tower opening for feed at the bottom of the acid gas washing Tata, cat head connects the sour gas incinerator, the water outlet of water-and-oil separator connects acid gas/aminoacid stripping tower opening for feed, and the oil phase outlet connects retrieving arrangement;
The side line of acid gas/aminoacid stripping tower connects another partial condenser, and this partial condenser connects and composes the two-stage partial condenser with a partial condenser again, and its liquid phase outlet connects acid gas/aminoacid stripping tower, and gaseous phase outlet connects follow-up ammonia treatment device;
Connect extraction tower at the bottom of the tower of acid gas/aminoacid stripping tower, the extraction tower cat head connects solvent recovery tower, and the solvent recuperation column overhead connects storage tank, connects the crude phenols retrieving arrangement at the bottom of the tower; Connect the solvent stripping tower at the bottom of the extraction Tata, solvent stripping tower cat head connects another water-and-oil separator, and its oil phase outlet connects storage tank, and the water outlet connects the solvent stripping tower, connects biochemical treatment apparatus at the bottom of the solvent stripping Tata; Storage tank connects extraction tower and solvent recovery tower respectively by pipeline.
Described oleic acid gas/aminoacid stripping tower is to have the stripping tower that side line is extracted out, and its theoretical stage is 15～30 grades, and opening for feed is dumped packing with top, and opening for feed is column plate with the lower section.Described acid gas washing tower is that theoretical stage is 1～4 grade a washing tower.Described extraction tower is that theoretical stage is 2～6 grades, is the packing tower of filler with the grid packing.Described solvent recovery tower is that theoretical stage is 12～20 grades a recovery tower.Described solvent stripping tower is that theoretical stage is 5～15 grades a stripping tower.
The present invention compared with prior art has following advantage:
(1) the inventive method has improved CO
2With the decreasing ratio of ammonia, can be with the CO in original flow process
2Residual quantity is by 2000mgl
-1About be reduced to 10mgl
-1Below, total ammonia content is reduced to 150mgl
-1Below, thereby alleviated ammonium salt crystallization and scale problems in original flow process.
(2) the inventive method is because the pH value when having reduced extraction, effect of extracting improves greatly, the phenol removal rate can be increased to more than 92% by present about 80%, the pollution load of processed waste water descends significantly, alleviate biochemical section processing load, solved the improvement difficult problem of high-concentration phenolic wastewater.
Caustic soda consumption when (3) the present invention also can save ammonia still process, and the solvent loss when having avoided ammonia still process.
Description of drawings
Fig. 1 is a wastewater treatment process synoptic diagram of the present invention; Among the figure: oleic acid gas/aminoacid stripping tower 1, acid gas washing tower 2, solvent stripping tower 3, solvent recovery tower 4, extraction tower 5, water-and- oil separator 6,7, partial condenser 8,9,10, storage tank 11.
Embodiment
Below in conjunction with the drawings and specific embodiments the present invention is further described, the present invention is not limited to this.
As shown in Figure 1, feed pipe connects oleic acid gas/aminoacid stripping tower 1 by pump, acid gas washing tower 2 opening for feeds, the cat head of acid gas/aminoacid stripping tower 1 connects partial condenser 8, the two ends outlet of partial condenser 8 connects the import of acid gas washing tower 2 and water-and-oil separator 6 respectively, connects acid gas/aminoacid stripping tower 1 opening for feed at the bottom of acid gas washing tower 2 towers, and cat head connects the sour gas incinerator, the water outlet of water-and-oil separator 8 connects acid gas/aminoacid stripping tower 1 opening for feed, and the oil phase outlet connects retrieving arrangement.
The side line of acid gas/aminoacid stripping tower 1 connects another partial condenser 9, and partial condenser 9 connects and composes the two-stage partial condenser with a partial condenser 10 again, and the gaseous phase outlet that 9,10 liquid phase outlet connects acid gas/ aminoacid stripping tower 1,10 connects follow-up ammonia treatment device.
As shown in Figure 1,12 fens hot and cold two stocks of coal gasification waste water that contain pollutents such as phenol, ammonia, CO2 do not enter acid gas/aminoacid stripping tower 1 from top and middle and upper part, the CO that stripping goes out
2, H
2Sour gas such as S and little ammonia, light oil, water vapor through partial condenser 8 fractional condensation and acid gas washing tower 2 after, the ammonia that most of stripping goes out refluxes, sour gas 16 is discharged from acid gas washing tower 2 tops, entering torch burns, the liquid phase of partial condenser 8 enters water-and-oil separator 6 and isolates light oil 13, and water refluxes, and enters partial condenser 9 and 10 from the ammoniacal liquor vapour 17 of side line extraction and carries out the two-stage fractional condensation, condensing reflux portion water and little ammonia, gas phase part 18 enter the refining workshop section of ammonia and are processed into liquefied ammonia.Acid gas/aminoacid stripping tower 1 still liquid 15 behind the depickling gas enters extraction tower 5 from top after being cooled to about 45 ℃, carries out counter-current extraction with extraction solvent.Extraction phase 20 pumps in the solvent recovery tower 4, rectifying separation crude phenols 25 and extraction solvent 24, and extraction solvent is recycled to storage tank 11 and recycles.The extracting phase 19 of extraction tower 5 enters solvent stripping tower 3, from top extraction dissolving and extraction solvent 23 and the portion water steam carried secretly, enter water-and-oil separator 7 after the condensation, the isolating water of the lower floor solvent stripping tower 3 that refluxes back, the extraction solvent on upper strata is recycled to storage tank 11 and recycles; The still liquid 22 of solvent stripping tower 3 enters biochemical section and carries out biochemical treatment.Regularly supplementing solvent 21 in storage tank 11 is supplied solvents to extraction tower 5 and solvent recovery tower 4 respectively by storage tank 11.
With flow is 88 tons/hour, the about 6400mgl of total phenol content
-1(the about 3200mgl of volatile phenol
-1, the about 3000mgl of lipid acid
-1); Total ammonia content is 7800mgl
-1, CO
2About 4200mgl
-1, oil content 350mgl
-1, COD
CrBe worth about 25000mgl
-1, the pH value is 10, the pending waste water that water temperature is 80 ℃ is handled by flow process shown in Figure 1.Parameters such as the progression of each tower, pressure, temperature are as follows:
25 grades of acid gas/aminoacid stripping tower theoretical stage, opening for feed top is dumped packing, the opening for feed bottom is a slant-hole tray, 60 ℃ of tower top temperatures, pressure 0.32MPa, 138 ℃ of column bottom temperatures, pressure 0.34MPa.133 ℃ of side line extraction temperature, pressure 0.33MPa, acid gas washing tower washing water yield 200kgh
-1
The extraction tower grid packing, bed stuffing height 12m, the extraction agent hexone adds acid and transfers pH7 before the extraction, and solvent ratio is 1: 6,12 grades of solvent stripping tower theoretical stages, tower top pressure 0.11MPa, produced quantity 2600kgh
-1, 55 ℃ of condensing temperatures, tower bottom pressure 0.12MPa, 102 ℃ of temperature.
18 grades of solvent recovery tower theoretical stages, tower top pressure 0.11MPa, 110 ℃ of temperature, tower bottom pressure 0.12MPa, 215 ℃ of temperature, reflux ratio 0.5.
Result: total phenol content 390mgl in the waste water after the processing
-1, total ammonia content is less than 90mgl
-1, COD
CrBe about 3800mgl
-1, extraction agent is less than 10mgl
-1, can realize qualified discharge through after the biochemical treatment.The about 75mgl of phenol content in the regenerating extracting agent
-1, the about 750mgl of extraction agent content in the crude phenols
-1, reclaiming virgin ammonia liquor concentration is 13%, has all reached corresponding processing requirement.With total phenol content 1600mgl after the existing art breading
-1, COD
CrBe 7000mgl
-1Compare, the phenol removal rate brings up to 94%, COD from 75%
CrDecreasing ratio brings up to 84.8% from 72%.
With flow is 60 tons/hour, the about 5500mgl of total phenol content
-1(the about 3000mgl of volatile phenol
-1, the about 3120mgl of lipid acid
-1), total ammonia 5900mgl
-1, CO
2About 6000mgl
-1, oil content 400mgl
-1, COD
CrBe worth about 23000mgl
-1, the pH value is 9.5, the pending waste water that water temperature is 80 ℃ is handled by flow process shown in Figure 1.Parameters such as the progression of each tower, pressure, temperature are as follows:
55 ℃ of acid gas/aminoacid stripping tower tower top temperature, pressure 0.4MPa, 148 ℃ of column bottom temperatures, pressure 0.43MPa.141 ℃ of side line extraction temperature, pressure 0.42MPa.
Extraction tower bed stuffing height 14m, the extraction agent diisopropyl ether adds acid and transfers pH5 before the extraction, and solvent ratio is 1: 6,10 grades of solvent stripping tower theoretical stages, cat head produced quantity 1020kgh
-1, 35 ℃ of condensing temperatures.
68 ℃ of solvent recovery tower tower top temperatures.
All the other conditions are with example 1.
Total phenol content 450mgl in the waste water after the processing
-1, total ammonia content is less than 80mgl
-1, COD
CrBe about 3900mgl
-1, extraction agent is less than 10mgl
-1, can realize qualified discharge through after the biochemical treatment.The regeneration collection.Get the about 80mgl of phenol content in the agent
-1, the about 250mgl of extraction agent content in the crude phenols
-1, reclaiming virgin ammonia liquor concentration is 14%, has all reached corresponding processing requirement.With total phenol content 1400mgl after the existing art breading
-1, COD
CrBe 6600mgl
-1Compare, the phenol removal rate brings up to 91.8%, COD from 74.5%
CrDecreasing ratio brings up to 83% from 71.3%.
With flow is 100 tons/hour, the about 5300mgl of total phenol content
-1(the about 2600mgl of volatile phenol
-1, the about 2800mgl of lipid acid
-1), total ammonia 6000mgl
-1, CO
2About 9000mgl
-1, oil content 400mgl
-1, COD
CrBe worth about 22000mgl
-1, the pH value is 10, the pending waste water that water temperature is 80 ℃ is handled by flow process shown in Figure 1.Parameters such as the progression of each tower, pressure, temperature are as follows:
Extraction tower bed stuffing height 10m, the extraction agent hexone adds acid and transfers pH5 before the extraction, and solvent ratio is 1: 6.All the other conditions are with example 1.
Total phenol content 320mgl in the waste water after the processing
-1, total ammonia content is less than 80mgl
-1, COD
CrBe about 3300mgl
-1, extraction agent is less than 10mgl
-1, can realize qualified discharge through after the biochemical treatment.The about 90mgl of phenol content in the regenerating extracting agent
-1, the about 200mgl of extraction agent content in the crude phenols
-1, reclaiming virgin ammonia liquor concentration is 13.5%, has all reached corresponding processing requirement.With total phenol content 1360mgl after the existing art breading
-1, COD
CrBe 6300mgl
-1Compare, the phenol removal rate brings up to 94%, COD from 74%
CrDecreasing ratio brings up to 85% from 71.3%.
Claims (8)
1. the method for a treating coal gasification wastewater by single-tower pressurization stripping is characterized in that comprising the steps:
(1) stripping depickling deamination: it is cold that coal gasification waste water is divided, two bursts of stripping tower top and middle and upper parts of extracting out from the band side line of heat enter in the tower, making tower top pressure is 0.2～0.6MPa, 40～80 ℃ of temperature, tower bottom pressure is 0.25～0.6MPa, 120～160 ℃ of temperature, going out gas mixture from the cat head stripping is 0.25～0.45MPa at pressure, temperature is fractional condensation under 110～150 ℃ the condition, then through phase-splitting, ammonia is isolated in washing, sour gas, light oil and water, reclaim light oil, backflow ammonia, water is discharged sour gas and burning, from side line extraction ammoniacal liquor gas through the two-stage fractional condensation, the liquid phase that refluxes then, refining gas phase, extraction still liquid at the bottom of the tower;
(2) extracting and dephenolizing: send into extraction tower top and organic solvent counter-current extraction after the still liquid of step (1) extraction is cooled to 45 ℃, the volume ratio that makes organic solvent and water is 1: 10～1: 6, extraction pH value is 4～7, temperature is 20～60 ℃, deliver to the solvent recovery tower from extraction tower cat head extraction extraction phase, making the recovery tower tower top pressure is 0.1～0.2MPa, 55～120 ℃ of temperature, tower bottom pressure is 0.1～0.2MPa, 200～220 ℃ of temperature, reflux ratio 0.2～0.4 goes out crude phenols and organic solvent through rectifying separation, the loopback organic solvent to be recycling, extraction extracting phase at the bottom of the extraction Tata;
(3) reclaim solvent: the extracting phase of step (2) extraction is delivered to the solvent stripping tower, making tower top pressure is 0.1～0.2MPa, 60～90 ℃ of temperature, tower bottom pressure is 0.1～0.2MPa, and 100～110 ℃ of temperature go out gaseous mixture condensation from the cat head stripping, then at 30～60 ℃ of following phase-splittings branch water outlet in 10～30 minutes and organic solvent, recirculation water, loopback organic solvent to be recycling, and extraction still liquid carries out biochemical treatment at the bottom of the tower.
2. method according to claim 1 is characterized in that organic solvent is diisopropyl ether or hexone described in the step (2).
3. a device of realizing claim 1 or 2 described methods is characterized in that comprising oleic acid gas/aminoacid stripping tower, extraction tower, acid gas washing tower, solvent stripping tower, solvent recovery tower, water-and-oil separator, partial condenser, pump, storage tank, wherein:
Feed pipe connects the opening for feed of oleic acid gas/aminoacid stripping tower, acid gas washing tower by pump, the cat head of acid gas/aminoacid stripping tower connects partial condenser, the two ends outlet of partial condenser connects the import of acid gas washing tower and water-and-oil separator respectively, connect acid gas/aminoacid stripping tower opening for feed at the bottom of the acid gas washing Tata, cat head connects the sour gas incinerator, the water outlet of water-and-oil separator connects acid gas/aminoacid stripping tower opening for feed, and the oil phase outlet connects retrieving arrangement;
The side line of acid gas/aminoacid stripping tower connects another partial condenser, and this partial condenser connects and composes the two-stage partial condenser with a partial condenser again, and its liquid phase outlet connects acid gas/aminoacid stripping tower, and gaseous phase outlet connects follow-up ammonia treatment device;
Connect extraction tower at the bottom of the tower of acid gas/aminoacid stripping tower, the extraction tower cat head connects solvent recovery tower, and the solvent recuperation column overhead connects storage tank, connects the crude phenols retrieving arrangement at the bottom of the tower; Connect the solvent stripping tower at the bottom of the extraction Tata, solvent stripping tower cat head connects another water-and-oil separator, and its oil phase outlet connects storage tank, and the water outlet connects the solvent stripping tower, connects biochemical treatment apparatus at the bottom of the solvent stripping Tata; Storage tank connects extraction tower and solvent recovery tower respectively by pipeline.
4. device according to claim 3 is characterized in that described oleic acid gas/aminoacid stripping tower is to have the stripping tower that side line is extracted out, and its theoretical stage is 15～30 grades, and opening for feed is above to be dumped packing, and opening for feed is column plate with the lower section.
5. device according to claim 3 is characterized in that described acid gas washing tower is that theoretical stage is 1～4 grade a washing tower.
6. device according to claim 3 is characterized in that described extraction tower is that theoretical stage is 2～6 grades, is the packing tower of filler with the grid packing.
7. device according to claim 3 is characterized in that described solvent recovery tower is that theoretical stage is 12～20 grades a recovery tower.
8. device according to claim 3 is characterized in that described solvent stripping tower is that theoretical stage is 5～15 grades a stripping tower.
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