CN117735570A - Process method for removing acid gas from ammonia-containing acidic condensate and recycling ammonia - Google Patents
Process method for removing acid gas from ammonia-containing acidic condensate and recycling ammonia Download PDFInfo
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- CN117735570A CN117735570A CN202311756555.4A CN202311756555A CN117735570A CN 117735570 A CN117735570 A CN 117735570A CN 202311756555 A CN202311756555 A CN 202311756555A CN 117735570 A CN117735570 A CN 117735570A
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- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 title claims abstract description 464
- 239000002253 acid Substances 0.000 title claims abstract description 185
- 229910021529 ammonia Inorganic materials 0.000 title claims abstract description 183
- 238000000034 method Methods 0.000 title claims abstract description 42
- 230000008569 process Effects 0.000 title claims abstract description 30
- 230000002378 acidificating effect Effects 0.000 title claims abstract description 20
- 238000004064 recycling Methods 0.000 title claims description 17
- 239000007789 gas Substances 0.000 claims abstract description 204
- 238000005406 washing Methods 0.000 claims abstract description 82
- 239000007788 liquid Substances 0.000 claims abstract description 77
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims abstract description 16
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 claims abstract description 15
- 229910000037 hydrogen sulfide Inorganic materials 0.000 claims abstract description 15
- BVCZEBOGSOYJJT-UHFFFAOYSA-N ammonium carbamate Chemical compound [NH4+].NC([O-])=O BVCZEBOGSOYJJT-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000001569 carbon dioxide Substances 0.000 claims abstract description 8
- 229910002092 carbon dioxide Inorganic materials 0.000 claims abstract description 8
- KXDHJXZQYSOELW-UHFFFAOYSA-N carbonic acid monoamide Natural products NC(O)=O KXDHJXZQYSOELW-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000004090 dissolution Methods 0.000 claims abstract description 5
- 238000011084 recovery Methods 0.000 claims description 100
- 238000001816 cooling Methods 0.000 claims description 39
- 230000005587 bubbling Effects 0.000 claims description 28
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical class O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 20
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 18
- 229910052717 sulfur Inorganic materials 0.000 claims description 17
- 239000011593 sulfur Substances 0.000 claims description 17
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 15
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 15
- 238000000926 separation method Methods 0.000 claims description 13
- 238000006243 chemical reaction Methods 0.000 claims description 12
- 238000001704 evaporation Methods 0.000 claims description 11
- 230000008020 evaporation Effects 0.000 claims description 11
- 238000002309 gasification Methods 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 8
- 239000006096 absorbing agent Substances 0.000 claims description 7
- 238000007670 refining Methods 0.000 claims description 7
- 125000004122 cyclic group Chemical group 0.000 claims description 6
- 238000012856 packing Methods 0.000 claims description 6
- 238000004519 manufacturing process Methods 0.000 claims description 5
- 230000015572 biosynthetic process Effects 0.000 claims description 2
- 229910000069 nitrogen hydride Inorganic materials 0.000 claims description 2
- 238000005260 corrosion Methods 0.000 abstract description 7
- 230000007797 corrosion Effects 0.000 abstract description 7
- 229910052751 metal Inorganic materials 0.000 abstract description 7
- 239000002184 metal Substances 0.000 abstract description 7
- 230000009467 reduction Effects 0.000 abstract description 4
- 150000003863 ammonium salts Chemical class 0.000 abstract description 3
- 238000002425 crystallisation Methods 0.000 abstract description 3
- 230000008025 crystallization Effects 0.000 abstract description 3
- 230000000903 blocking effect Effects 0.000 abstract description 2
- MWUXSHHQAYIFBG-UHFFFAOYSA-N nitrogen oxide Inorganic materials O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 description 9
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 6
- 238000006477 desulfuration reaction Methods 0.000 description 6
- 230000023556 desulfurization Effects 0.000 description 6
- 229910002091 carbon monoxide Inorganic materials 0.000 description 5
- 238000009833 condensation Methods 0.000 description 5
- 230000005494 condensation Effects 0.000 description 5
- 239000003546 flue gas Substances 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 239000010865 sewage Substances 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 230000008859 change Effects 0.000 description 3
- 230000006837 decompression Effects 0.000 description 3
- 238000000605 extraction Methods 0.000 description 3
- 239000010935 stainless steel Substances 0.000 description 3
- 229910001220 stainless steel Inorganic materials 0.000 description 3
- XKMRRTOUMJRJIA-UHFFFAOYSA-N ammonia nh3 Chemical compound N.N XKMRRTOUMJRJIA-UHFFFAOYSA-N 0.000 description 2
- 239000010866 blackwater Substances 0.000 description 2
- 239000003245 coal Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 229910000975 Carbon steel Inorganic materials 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000000711 cancerogenic effect Effects 0.000 description 1
- 239000010962 carbon steel Substances 0.000 description 1
- 231100000315 carcinogenic Toxicity 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 238000009428 plumbing Methods 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 239000008213 purified water Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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Abstract
The invention discloses a process method for removing acid gas from ammonia-containing acidic condensate and recovering ammonia. The deacidification gas load of the pressurized stripping tower and the acid gas stripping tower is reduced, and the corrosion risk of an acid medium to metal equipment pipelines is reduced; the primary investment cost and the running cost are greatly reduced; the environment for generating ammonium carbamate is not provided, and the problem of equipment corrosion is thoroughly solved; the content of acid gas in ammonia gas extracted from the side line is low, so that the flow is simplified, and the ammonium salt crystallization is prevented from blocking heat exchange equipment; the steps of pressure reduction, temperature reduction and washing are carried out step by step, so that hydrogen sulfide and carbon dioxide in the ammonia gas are dissolved in condensate liquid of each stage of pressure reduction separator to appear in an ionic state, and the ammonia gas reaching the dissolution saturation is flashed and escaped from the condensate liquid, thereby obtaining the ammonia gas with higher purity.
Description
Technical Field
The invention relates to a coal chemical technology, in particular to a process method for removing acid gas and recycling ammonia from ammonia-containing acidic condensate purified by a raw gas carbon monoxide conversion device in production.
Background
In a raw material gas purifying device in the coal chemical industry, condensate generated in the production process of a carbon monoxide conversion process contains: CO 2 、H 2 S、NH 3 And volatile weak electrolyte. Wherein CO is 2 、H 2 S is an acidic substance, and has a certain corrosion effect on metal equipment and pipelines in the production device. The presence of ammonia causes CO 2 、H 2 The ammonia salt crystals of S block the plumbing. Meanwhile, as the ammonia nitrogen of the system is too high, the difficulty and cost for treating the ammonia nitrogen by the black water of the gasification device are increased, and if the black water is not treated in time, the environment is greatly harmed.
At present, the condensate is mainly treated by adopting a single-tower stripping method and a double-tower stripping method in China:
single column stripping: the acid gas and ammonia in the condensate are stripped out and then cooled and separated. Cooling and separating the acid gas, and then sending the acid gas to a torch or recycling the Claus sulfur; the condensate is sent to flue gas desulfurization or sewage treatment. The operating pressure of the column is between 0.3 and 0.5MPa (g).
Double column stripping: the method is that the transformed condensate is advanced to a No. 1 stripping tower, the acid gas removed from the tower top is sent to sulfur recovery, the tower bottom is obtained to obtain ammonia-containing condensate, and the ammonia-containing condensate is sent to a No. 2 stripping tower. And (3) removing acid gas from the top of the No. 2 stripping tower, delivering sulfur to be recovered, delivering tower bottom liquid to a gasification island, and performing tertiary condensation and deep condensation desulfurization on side extracted gas ammonia to prepare ammonia water. The operation pressure of the top of the No. 1 stripping tower is 0.3MPa (g), the temperature of the top of the tower is 40 ℃ and the temperature of the bottom of the tower is 140 ℃. The operating pressure of the No. 2 stripping tower is 0.5MPa (g), the operating temperature of the tower top is 50 ℃ and the operating temperature of the tower bottom is 158 ℃.
The above process has the following problems:
in the single-tower stripping process, the temperature of the acid gas at the outlet of the stripping tower is about 130 ℃, and the acid gas contains a certain amount of saturated water, so that NH is generated after cooling 4 HS、(NH 4 ) 2 S、NH 4 HCO 3 、(NH 4 ) 2 CO 3 The isoammonium salt crystallization blocks the heat exchange tube of the cooler and simultaneously has the reducing agent ammonium carbamate (NH) 2 COONH 4 ) The generation of the protective layer-oxide film on the surface of the metal is destroyed, and the metal is quickly corroded after losing the protection, so that the equipment pipeline is damaged. The content of ammonia-containing gas in the cooled and separated acid gas is generally 3000 ppm-10000 ppm, and the ammonia-containing gas is sent to a torch for burning or the Claus sulfur is recovered, and the ammonia becomes nitrogen oxides in the burning process of the torch or the Claus sulfur recovery, so that the nitrogen oxides are cancerogenic substances and are discharged into the atmosphere to seriously pollute the environment.
And removing flue gas desulfurization or sewage treatment from the separated ammonia condensate. Due to the H contained in the condensate 2 S、NH 3 Etc., H 2 S content is 2000ppm, NH 3 The content was-30000 ppm. The sewage treatment increases the load of sewage treatment and has great influence on the environment; flue gas desulfurization is carried out due to H in ammonia water 2 And if the S content is high, elemental sulfur is separated out, so that the flue gas desulfurization and denitrification filler is blocked, and the device cannot operate.
The main reason is that the separation depth of ammonia and acid gas is insufficient, and the stripped acid gas contains ammonia and the acid gas is contained in the ammonia water condensate.
Double column stripping process problem 1, the amount of liquid in the bottom of the No. 1 stripper is almost equal to the amount of the conversion condensate, and the liquid is sent to the No. 2 stripper. Because condensate is not transformed, the heat load of the No. 2 stripping tower is still large, the steam consumption is high, and the operation cost is high; and the equipment specification is large, and the one-time investment is large.
Double-tower steam stripping processThe ammonia and the acid are not thoroughly separated in the No. 2, no. 1 stripping tower and the No. 2 stripping tower, and the ammonia and the acid gas coexist to generate the ammonium carbamate (NH) 2 COONH 4 ) Corroding equipment pipelines. Stainless steel materials are selected for the No. 1 stripping tower and the No. 2 stripping tower, S30403, S31603, S32168 and S22053 are selected as the selected materials, and titanium materials are also selected, so that the engineering cost is increased.
The double-tower stripping process has the advantages that the double-tower stripping process has no deacidification property, the double-tower stripping process has large ammonia content in the acid gas, the separation of the ammonia and the acid gas is incomplete, and the separation treatment is not carried out. The acid gas is sent to a torch or is recycled by claus sulfur, so that nitrogen oxides are generated, the environment is polluted, and the waste of ammonia is also caused.
The problem of double-tower stripping technology is that hydrogen sulfide in ammonia gas extracted from the side line of a No. 4 and 2 stripping tower is high, the process for refining the ammonia gas extracted from the side line is complex, the consumption of deep condensation desulfurization is high, and the operation cost is high.
Disclosure of Invention
The invention aims to solve the problems that equipment and pipelines are blocked, corroded, incomplete treatment, influence on the washing effect of low-temperature methanol and the like caused by the circulation superposition of ammonia and acid gas in the existing conversion condensate recovery, and provides a process method for removing the acid gas from the ammonia-containing acid condensate and recovering the ammonia.
The technical problems of the invention are mainly solved by the following technical proposal: a process method for removing acid gas from ammonia-containing acidic condensate and recycling ammonia is characterized by comprising the following steps:
first, ammonia-containing vapor concentration
A. And (3) sending the high-pressure condensate into a flash tank, and flashing out part of the acid gas and the non-condensable gas to send sulfur for recovery.
B. The condensate after flash evaporation exchanges heat through a temperature raising heat exchanger, the temperature is raised to 80-100 ℃ and enters from the upper part of the pressurized stripping tower.
C. The acid gas, the non-condensable gas, the ammonia gas and the saturated water vapor are taken out from the top of the pressurized stripping tower at the temperature of 133-140 ℃ and directly enter the acid gas removal tower, and the mass ratio of the ammonia-containing acid gas is 0.08-0.12 times of that of the conversion condensate.
D. The condensate liquid with the temperature of between 138 ℃ is obtained by pressurizing the tower kettle of the stripping tower, and comprises NH 3 ≤50ppm、H 2 S is less than or equal to 10ppm and is sent to a gasification island.
(II) acid gas removal
The ammonia-containing acid gas from the top of the pressurized stripping tower enters the tower from the bottom of the acid gas removal tower together with the acid gas taken out from the top of the ammonia recovery tower:
E. pressurizing tower bottom liquid of the acid gas removal tower through a tower bottom liquid pump, heating and pressurizing feeding liquid of the stripping tower through a temperature raising heat exchanger, and outputting the feeding liquid in two ways after cooling the tower bottom liquid: one path is cooled to normal temperature by circulating water of a cooler 1, and then enters the middle part of the acid gas removal tower to be fed as washing liquid of the acid gas removal tower for circulating cooling and washing; one path is taken as a recovery liquid to be sent to an ammonia recovery tower for recovering ammonia; wherein, the mass ratio of the circulating cooling washing liquid in the middle part of the acid gas removal tower to the recovery liquid of the ammonia removal recovery tower is as follows: 2.0 to 4.0;
F. the top of the acid gas removal tower is selected to be cooled to normal temperature by a condensate liquid which is clean in the tower bottom of the ammonia recovery tower through a heat recoverer 2 and a cooler 2 for cooling and washing.
G. And (3) conveying the acid gas and the noncondensable gas removed from the top of the acid gas removal tower to sulfur recovery, wherein NH3 in the removed acid gas is less than or equal to 100ppm.
(III) side-draw ammonia recovery
H. The tower kettle recovery liquid from the acid gas removal tower sequentially exchanges heat with the ammonia general heat recoverer 1 with saturated water vapor extracted from the side line of the ammonia recovery tower and exchanges heat with the ammonia general heat recoverer 2 with the condensate of the tower kettle of the ammonia recovery tower to recover heat.
Heating the tower kettle by adopting steam with the pressure of more than 1.0MPa (g), and directly feeding the steam into a reboiler inside and outside the tower for heating; the top of the ammonia recovery tower is selected to be cooled to normal temperature by a condensate liquid which is clean in the tower kettle of the ammonia recovery tower through a heat recoverer 2 and a cooler 2 for cooling and washing.
I. And (3) delivering the ammonia-containing acid gas taken out from the top of the ammonia recovery tower to an acid gas removal tower for recycling to remove the acid gas, and recovering ammonia.
J. After heat is recovered from condensate liquid taken out from the tower bottom of the ammonia gas recovery tower through the heat recovery device 2, part of condensate liquid is cooled to normal temperature through the cooler 2 and then is used for top washing liquid of the acid gas removal tower and the ammonia gas recovery tower, and the rest condensate liquid is sent to a gasification island, wherein NH in the condensate liquid 3 ≤50ppm、H 2 S≤10ppm。
K. Ammonia gas with certain saturated water vapor is extracted from the side line, and enters the fourth step after heat exchange and cooling are carried out on the ammonia gas and the recovery liquid of the tower kettle of the acid gas removal tower through the heat recoverer 1.
(IV) Ammonia refining
L, reducing the pressure of ammonia gas extracted from the side line of an ammonia gas recovery tower after heat exchange of a heat recovery device 1 to 0.25MPa (g), entering a depressurization washing separator 1, cooling and flashing ammonia gas in the depressurization washing separator 1, bubbling and washing the ammonia gas in a separation scrubber through condensate in the scrubber, and washing residual hydrogen sulfide in the ammonia gas through condensate circulating packing in the scrubber.
And M, enabling the ammonia gas subjected to flash evaporation by the washed depressurization washing separator 1 to enter a cooler 3, reducing the temperature to 110 ℃ below zero, decompressing to 0.15MPa (g), entering the depressurization washing separator 2, cooling the ammonia gas subjected to flash evaporation in the depressurization washing separator 2, bubbling and washing the ammonia gas in the separation scrubber through condensate in the scrubber, and washing the ammonia gas through condensate circulating packing in the scrubber to remove residual hydrogen sulfide in the ammonia gas.
And (3) enabling the ammonia gas flashed by the washed depressurization washing separator 2 to enter a cooler 4 to cool to normal temperature, depressurizing to 0.05MPa (g), entering a depressurization bubbling separator, cooling the flashed ammonia gas in the cooler, bubbling and washing the ammonia gas in the separation washer through condensate in the cooler, and feeding the ammonia gas flashed by the depressurization bubbling separator subjected to bubbling and washing to the step five ammonia absorber.
O, the condensate of the depressurization washing separator 1, the depressurization washing separator 2 and the depressurization bubbling separator are separated and then are pressurized by a centrifugal pump to be sent into an ammonia recovery tower for cyclic treatment.
Production of ammonia product
From pressure-reducing bubbling separationThe ammonia gas flash evaporated by the device enters an ammonia absorber and is mixed with desalted water to prepare ammonia water, and H in the ammonia water 2 S≤10ppm。
In the first step, the concentrated ammonia-containing acid gas, the acid gas in the conversion condensate and the ammonia are all stripped in a pressurized stripping tower at the same time and taken out for treatment in the second step.
In the step (A), the condensate liquid after flash evaporation and the tower bottom liquid of the acid gas removal tower in the step (II) are subjected to heat exchange through a temperature raising heat exchanger, the temperature is raised to 80-100 ℃, and the condensate liquid is input from the upper part of the pressurized stripping tower.
In the step (A), the pressurized stripping tower is operated under the pressure of 0.2MPa (g) to 0.3MPa (g), and the tower kettle adopts low-pressure steam of 0.5MPa (g) to directly enter the tower for heat supply.
In the step (II), the change trend of controlling the operation environment conditions to influence the ionization balance and the dissolution balance is utilized to separate the acid gas and the ammonia in the acid gas removal tower, and the acid gas and the ammonia are not enriched in the same area at the same time, so that the ammonium carbamate is eliminated.
In the second step, the top of the acid gas removal tower is operated under the pressure of 0.13MPa (g) to 0.16MPa (g); the tower bottom is operated at 110-120 ℃, and the tower top is operated at 40-50 ℃.
In the step (III), the acid gas containing a small amount of gas ammonia, which is taken out from the top of the ammonia recovery tower, is returned to the acid gas removal tower in the step (II), and the stripping separation of the acid gas and the ammonia is carried out again, so that the acid gas is removed, and the ammonia is left in the tower kettle; and (3) in the step (II), the tower bottom of the acid gas removal tower contains a small amount of ammonia water condensate of acid gas, and the ammonia water condensate is sent to the ammonia recovery tower in the step (III) to obtain ammonia at the side line.
In the process method for removing acid gas from the ammonia-containing acidic condensate and recycling ammonia, the ammonia in the acid gas taken out of the top of the acid gas removal tower is low, the mass concentration is less than or equal to 100ppm, and the removed acid gas is sent to sulfur for recycling; the hydrogen sulfide content and the mass concentration of the acid gas contained in the gas ammonia extracted from the side line of the ammonia recovery tower are less than or equal to 300ppm, the carbon dioxide content and the mass concentration are less than or equal to 1000ppm, and the gas ammonia is sent to the step (four) for refining.
In the step (III), the recovery liquid after the temperature is raised to 140-150 ℃ is fed from the upper part of the ammonia recovery tower; the operation pressure of the top of the ammonia recovery tower is 0.5MPa (g); the operation temperature of the tower bottom is 158-165 ℃, and the operation temperature of the tower top is 55-65 ℃; the temperature of the side extracted ammonia gas is 148-152 ℃.
In the step (four), ammonia gas extracted from the side line of the ammonia recovery tower in the step (three) is subjected to 1-stage cooling and depressurization, then subjected to 2-stage cooling and depressurization, and subjected to condensate circulation washing by a washing separator; then 3-stage cooling and depressurization are carried out, and bubbling washing is adopted through a washing separator; dissolving the carbon dioxide and hydrogen sulfide which are the acid gases and escape without being dissolved by the condensate liquid in the separated condensate liquid again; the condensate after the cyclic washing is sent to the ammonia recovery tower of the step (III) again to remove acid gas and recover ammonia; cooling the ammonia gas after 3-stage cooling, depressurizing and washing to normal temperature, and then, introducing the ammonia gas into a depressurizing bubbling separator for bubbling separation to obtain flash-separated high-purity ammonia gas, and sending the ammonia gas to the step (V) to prepare ammonia water.
Compared with the prior art, the invention has the beneficial effects that:
1. designing conditions for high-pressure conversion condensate to enter a depressurization flash tank: non-condensable gas and part of acid gas dissolved in condensate liquid under the working condition of high pressure of the shift reaction are flashed out, so that the deacidification gas load of a pressurized stripping tower and an acid gas stripping tower is reduced, and the corrosion risk of acid medium to metal equipment pipelines is reduced.
2. Acid gas and ammonia in the conversion condensate are completely stripped by adopting a pressurized stripping tower, and qualified purified water (NH 3 ≤50ppm、H 2 S is less than or equal to 10 ppm) is sent to a gasification device; the concentrated ammonia-containing acid gas is obtained at the top of the tower and then sent to the next step,the acid gas is separated from ammonia by an acid gas removal column. Because the mass of the treated ammonia-containing acid gas is only 0.08 to 0.12 times of that of the conversion condensate, the equipment specifications and the heat load of the acid gas extraction tower and the ammonia recovery tower are greatly reduced, so that the primary investment cost and the running cost are greatly reduced, and the diameter of the acid gas extraction tower is greatly reduced by only about 0.32 times of the sectional area of the stripping tower in the conventional double-tower stripping.
3. The removal of acid gas utilizes the principle that ionization balance and dissolution balance change along with the change of environmental conditions; acidic Medium H 2 S、CO 2 With NH 3 The ionization equilibrium constant of the ammonium salt formed in the aqueous solution is changed from large to small by increasing the temperature from normal temperature to 125 ℃; when the temperature exceeds 125 ℃, the ionization equilibrium constant is changed from small to large; h 2 S、CO 2 With NH 3 The solubility in water becomes smaller with an increase in temperature; controlling the operating pressure of the acid gas extraction tower to be 0.15MPa (g), and controlling the operating temperature of the middle lower part of the tower to be 80-130 ℃; in the acid gas stripping tower, acid gas H 2 S、CO 2 Removal from the top of the column of NH 3 The acid gas and the ammonia are separated to the maximum degree and the CO is remained in the tower kettle 2 With NH 3 Are not enriched in the same region at the same time, thereby avoiding the formation of ammonium carbamate (NH) 2 COONH 4 ) Because ammonium carbamate has strong reducibility, the oxide film on the surfaces of metal equipment and pipelines is destroyed, thereby corroding the equipment and the pipelines; because the environment of ammonium carbamate generation is not available, the problem of equipment corrosion is thoroughly solved, and the material of the acid stripping tower is selected from common stainless steel S30508.
4. Because the corrosion problem of equipment is thoroughly solved, the upper section of the ammonia recovery tower adopts common stainless steel S30508, the lower section adopts carbon steel, and the one-time investment cost of the double towers is reduced by about 50 percent.
5. Step two, mainly removing acid gas, and step three, mainly extracting ammonia: the acid gas containing a small amount of ammonia, which is taken out from the top of the ammonia recovery tower, is returned to the acid gas removal tower in the second step, and the stripping separation of the acid gas and the ammonia is carried out again, so that the acid gas is removed and ammonia is recovered; the tower bottom of the acid gas removal tower in the second step contains ammonia condensate with less acid gas, and the ammonia condensate is sent to the ammonia recovery tower in the third step, and ammonia is extracted from the side line; the ammonia in the acid gas taken out of the top of the acid gas removal tower is low, the mass concentration is only within 100ppm, and the removed acid gas is sent to sulfur for recovery; the acid gas contained in the gas ammonia extracted from the side line of the ammonia recovery tower is very low, the mass concentration of hydrogen sulfide is less than 300ppm, and the mass concentration of carbon dioxide is less than 1000ppm; the content of acid gas in ammonia gas extracted from side lines in conventional double-tower stripping in the market is above 1000ppm, and the ammonia gas extracted from side lines can remove acid medium only by three-stage condensation separation and low-temperature sulfur fixation purification, so that the process is complex, and the phenomena of blocking heat exchange equipment and the like due to ammonium salt crystallization can also occur in the treatment process.
6. Adopting a secondary depressurization condensation separation circulation washing refined ammonia recovery tower side line to extract ammonia gas: the principle that the solubility of ammonia in water becomes smaller as the pressure becomes higher and the solubility of ammonia in water becomes larger as the temperature becomes higher is utilized, the ammonia gas extracted from the side line of an ammonia gas recovery tower at 140 ℃ after heat exchange by a heat recovery device 1 is decompressed to 0.25MPa (g) and enters a decompression washing separator 1; the ammonia gas flashed by the depressurization washing separator 1 enters a cooler 3 to be cooled to 110 ℃ below zero, depressurized to 0.15MPa (g) and enters a depressurization washing separator 2; the condensate liquid circulation washing is adopted in the 2-stage depressurization separator, and the carbon dioxide and hydrogen sulfide which are the acid gases and escape without being dissolved by the condensate liquid are dissolved in the separated condensate liquid again, so that the ammonia gas in the gas phase separated by the depressurization separator is purer; and (3) returning the condensate after the cyclic washing to an ammonia recovery tower, removing the acid gas again, and recovering ammonia. Simultaneously, the ammonia gas flashed by the depressurization washing separator 2 enters a cooler 4 to cool to normal temperature, depressurized to 0.05MPa (g) and enters a depressurization bubbling separator; in the process of step-by-step depressurization, cooling and washing, hydrogen sulfide and carbon dioxide in the ammonia gas are dissolved in condensate liquid of each stage of depressurization separator to appear in an ionic state, so that the ammonia gas reaching the dissolution saturation is flashed and escaped from the condensate liquid, and the ammonia gas with higher purity is obtained.
Drawings
FIG. 1 is a schematic flow chart of a process for removing acid gas and recycling ammonia by changing condensate liquid according to the design of the invention.
Detailed Description
The technical scheme of the invention is further specifically described below through examples and with reference to the accompanying drawings.
In this embodiment, as shown in fig. 1, the apparatus includes a depressurization flash tank, a temperature raising heat exchanger, a pressurized stripping tower, an acid gas removal tower, a cooler 1, an ammonia recovery tower, a heat recovery device 1, a heat recovery device 2, a cooler 2, a depressurization washing separator 1, a cooler 3, a depressurization washing separator 2, a cooler 4, a depressurization bubbling separator, an ammonia absorber, and the like.
The method comprises the following steps of:
step one, ammonia-containing acid vapor concentration
And (3) delivering the converted high-pressure condensate into a flash tank with the pressure of 0.4MPa (g), and delivering part of acid gas and non-condensable gas into sulfur for recycling. The condensed liquid after flash evaporation and tower bottom liquid of the acid gas removal tower are heated to 80-100 ℃ through a temperature raising heat exchanger, and enter from the upper part of a pressurized stripping tower, the pressurized stripping tower is operated at the pressure of 0.2-0.3 MPa (g), and the tower bottom adopts 0.5MPa (g) low-pressure steam to directly enter the tower for heat supply (comprising indirect reboiler for heat supply). The acid gas, the non-condensable gas, the ammonia gas and the saturated water vapor are taken out from the top of the tower at the temperature of 133-140 ℃ and directly enter an acid gas removal tower, and the mass ratio of the ammonia-containing acid gas is 0.08-0.12 times of that of the conversion condensate. The condensate (NH) with the temperature of between 138 ℃ is obtained by pressurizing the tower kettle of the stripping tower 3 ≤50ppm、H 2 S is less than or equal to 10 ppm) of air-supplying island.
In the step, the converted high-pressure condensate is sent to a flash tank with the pressure of 0.4MPa (g), part of acid gas and noncondensable gas are flashed out and sent to sulfur for recovery, so that the deacidification gas load of a pressurized stripping tower and an acid gas stripping tower is reduced, and the corrosion risk of acid medium to metal equipment pipelines is reduced.
Step two, acid gas is removed
The ammonia-containing acid gas from the top of the pressurized stripping tower and the acid gas from the top of the ammonia recovery tower are taken out and fed into the tower from the bottom of the acid gas removal tower together, and the top of the acid gas removal tower is operated under the pressure of 0.13MPa (g) to 0.16MPa (g); the tower bottom is operated at 110-120 ℃, and the tower top is operated at 40-50 ℃.
Heating the tower bottom liquid of the acid gas removal tower to the feed liquid of the pressurized stripping tower through a temperature raising heat exchanger by a tower bottom liquid pump, cooling part of the cooled tower bottom liquid to normal temperature through circulating water of a cooler 1, and taking the middle feed of the acid gas removal tower as the washing of the acid gas removal tower for circulating cooling and washing; and the other tower bottom liquid after passing through the temperature raising heat exchanger is used as recovery liquid to be sent to an ammonia recovery tower for recovering ammonia. The top of the acid gas removal tower is selected to be cooled to normal temperature by a condensate liquid which is clean in the tower bottom of the ammonia recovery tower through a heat recoverer 2 and a cooler 2 for cooling and washing. The mass ratio of the circulating cooling washing liquid in the middle part of the acid gas removal tower to the recovery liquid of the ammonia removal recovery tower is as follows: 2.0 to 4.0.
Delivering the acid gas and noncondensable gas removed from the top of the acid gas removal tower to sulfur recovery, and removing NH in the acid gas 3 ≤100ppm。
Step three, recovering ammonia gas from side line
The tower kettle recovery liquid from the acid gas removal tower sequentially exchanges heat with the ammonia general heat recoverer 1 with saturated water vapor extracted from the side line of the ammonia recovery tower and exchanges heat with the ammonia general heat recoverer 2 with the condensate of the tower kettle of the ammonia recovery tower to recover heat. The recovery liquid after the temperature is raised to 140-150 ℃ is fed from the upper part of the ammonia recovery tower. The operation pressure of the top of the ammonia recovery tower is 0.5MPa (g), the operation temperature of the tower kettle is 158-165 ℃, and the operation temperature of the top of the tower is 55-65 ℃; the temperature of the side extracted ammonia gas is 148-152 ℃. The tower kettle is heated by steam with the pressure of more than 1.0MPa (g), the steam is directly fed into a reboiler in the tower and the reboiler outside the tower for heating, and the clean condensate in the tower kettle of the ammonia recovery tower is selected at the top of the ammonia recovery tower and is cooled to normal temperature through a heat recoverer 2 and a cooler 2 for cooling and washing.
And (3) delivering the ammonia-containing acid gas taken out from the top of the ammonia recovery tower to an acid gas removal tower for recycling to remove the acid gas, and recovering ammonia.
After heat is recovered by the condensate liquid taken out from the tower bottom of the ammonia gas recovery tower through the heat recovery device 2, a part of the condensate liquid is cooled to normal temperature through the cooler 2 and then is used for top washing of the acid gas removal tower and the ammonia gas recovery towerThe residual liquid is sent to gasification island, NH in condensate liquid 3 ≤50ppm、H 2 S≤10ppm。
Ammonia gas with certain saturated water vapor is extracted from the side line, and enters an ammonia gas refining step after heat exchange and cooling are carried out on the ammonia gas with the tower kettle recovery liquid of the acid gas removal tower through the heat recoverer 1.
And (3) taking out the acid gas from the tower top of the ammonia gas recovery tower in the second step and the third step, returning the acid gas to the acid gas removal tower for circularly removing the acid gas, wherein the acid gas removal tower only focuses on removing the acid gas, and the ammonia gas recovery tower only focuses on recovering ammonia.
Step four, ammonia refining
Ammonia gas which is recovered from the side line of an ammonia gas recovery tower at the temperature of 140 ℃ after heat exchange by a heat recovery device 1 is decompressed to 0.25MPa (g), and enters a decompression washing separator 1, the ammonia gas which is cooled and flash evaporated in the decompression washing separator 1 is in the separator, is firstly subjected to condensate bubbling washing in the separator, and is then subjected to condensate circulating packing washing in the separator, so that residual hydrogen sulfide in the ammonia gas is removed. The temperature of the ammonia gas subjected to flash evaporation by the washed depressurization washing separator 1 enters a cooler 3 to be reduced to 110 ℃ below zero, the pressure is reduced to 0.15MPa (g), the ammonia gas subjected to cooling flash evaporation in the cooler enters the depressurization washing separator 2, the ammonia gas is subjected to bubble washing by condensate in the cooler, and residual hydrogen sulfide in the ammonia gas is removed by condensate circulating packing washing in the cooler. The ammonia gas flash evaporated by the depressurization washing separator 2 enters the cooler 4 to be cooled to normal temperature, depressurized to 0.05MPa (g), enters the depressurization bubbling separator, the ammonia gas after cooling flash evaporation in the cooler is in the separator, is bubbled and washed by condensate in the cooler, and the ammonia gas flash evaporated by the depressurization separator after bubbling and washing is sent to the step five ammonia absorber.
Condensate of the depressurization washing separator 1, the depressurization washing separator 2 and the depressurization bubbling separator is separated and then pumped into an ammonia recovery tower for cyclic treatment by adopting a centrifugal pump.
In the step, ammonia gas extracted from the side line is subjected to gradual depressurization and temperature reduction, and ammonia water condensate is circularly washed to remove residual acid gas of the ammonia gas.
Step five, preparing ammonia product
The ammonia gas from the flash evaporation of the depressurization bubbling separator enters an ammonia absorber andmixing desalted water to obtain required ammonia water H 2 S≤10ppm。
The main index data of this example and the prior art are shown in table 1 after actual detection.
Table 1: compared with the prior art, the main index data of the application embodiment of the embodiment
The technical means not described in the present invention are all known to those skilled in the art.
The above embodiments are illustrative of the present invention, and not limiting, and any equivalent changes or equivalent modifications made according to the technical ideas of the present invention still fall within the scope of the technical proposal of the present invention without departing from the principle of the technical proposal.
Claims (10)
1. A process method for removing acid gas from ammonia-containing acidic condensate and recycling ammonia is characterized by comprising the following steps:
first, ammonia-containing vapor concentration
A. Feeding the high-pressure condensate into a flash tank, and flashing out part of acid gas and noncondensable gas to feed sulfur for recovery;
B. the condensate after flash evaporation exchanges heat through a temperature raising heat exchanger, the temperature is raised to 80-100 ℃ and enters from the upper part of the pressurized stripping tower;
C. acid gas, non-condensable gas, ammonia gas and saturated water vapor are taken out from the top of the pressurized stripping tower at 133-140 ℃ and directly enter an acid gas removal tower, and the mass ratio of the ammonia-containing acid gas is 0.08-0.12 times of that of the conversion condensate;
D. the condensate liquid with the temperature of between 138 ℃ is obtained by pressurizing the tower kettle of the stripping tower, and comprises NH 3 ≤50ppm、H 2 S is less than or equal to 10ppmA gasification island;
(II) acid gas removal
The ammonia-containing acid gas from the top of the pressurized stripping tower enters the tower from the bottom of the acid gas removal tower together with the acid gas taken out from the top of the ammonia recovery tower:
E. pressurizing tower bottom liquid of the acid gas removal tower through a tower bottom liquid pump, heating and pressurizing feeding liquid of the stripping tower through a temperature raising heat exchanger, and outputting the feeding liquid in two ways after cooling the tower bottom liquid: one path is cooled to normal temperature by circulating water of a cooler 1, and then enters the middle part of the acid gas removal tower to be fed as washing liquid of the acid gas removal tower for circulating cooling and washing; one path is taken as a recovery liquid to be sent to an ammonia recovery tower for recovering ammonia; wherein, the mass ratio of the circulating cooling washing liquid in the middle part of the acid gas removal tower to the recovery liquid of the ammonia removal recovery tower is as follows: 2.0 to 4.0;
F. the top of the acid gas removal tower is selected to be cooled to normal temperature by a condensate liquid which is clean in the tower kettle of the ammonia recovery tower through a heat recoverer 2 and a cooler 2 for cooling and washing;
G. delivering the acid gas and noncondensable gas removed from the top of the acid gas removal tower to sulfur recovery, wherein NH3 in the removed acid gas is less than or equal to 100ppm;
(III) side-draw ammonia recovery
H. The tower kettle recovery liquid from the acid gas removal tower sequentially exchanges heat with an ammonia general heat recoverer 1 with saturated water vapor extracted from the side line of the ammonia recovery tower and exchanges heat with an ammonia recovery tower kettle condensate general heat recoverer 2 to recover heat;
heating the tower kettle by adopting steam with the pressure of more than 1.0MPa (g), and directly feeding the steam into a reboiler inside and outside the tower for heating; the top of the ammonia recovery tower is selected to be cooled to normal temperature by a condensate liquid which is clean in the tower kettle of the ammonia recovery tower through a heat recoverer 2 and a cooler 2 for cooling and washing;
I. the ammonia-containing acid gas taken out from the top of the ammonia recovery tower is sent to an acid gas removal tower for recycling to remove the acid gas, and ammonia is recovered;
J. after the condensate liquid taken out from the tower bottom of the ammonia gas recovery tower is subjected to heat recovery by the heat recovery device 2, part of condensate liquid is cooled to normal temperature by the cooler 2 and then is used for the top washing liquid of the acid gas removal tower and the ammonia gas recovery tower, and the rest condensate liquid isDelivering NH in condensate to gasification island 3 ≤50ppm、H 2 S≤10ppm；
K. Ammonia gas with certain saturated water vapor is extracted from the side line, and enters the fourth step after heat exchange and cooling are carried out on the ammonia gas and the tower kettle recovery liquid of the acid gas removal tower through the heat recoverer 1;
(IV) Ammonia refining
L, reducing the pressure of ammonia gas extracted from the side line of an ammonia gas recovery tower after heat exchange of a heat recoverer 1 to 0.25MPa (g), entering a depressurization washing separator 1, cooling and flashing ammonia gas in the depressurization washing separator 1, bubbling and washing the ammonia gas in a separation scrubber through condensate in the scrubber, and washing residual hydrogen sulfide in the ammonia gas through condensate circulating packing in the scrubber;
m, the ammonia gas flash-evaporated by the washed depressurization washing separator 1 enters a cooler 3 to be cooled to 110 ℃ below zero, the pressure is reduced to 0.15MPa (g), the ammonia gas flash-evaporated by cooling in the depressurization washing separator 2 enters a depressurization washing separator 2, the ammonia gas flash-evaporated by cooling in the depressurization washing separator 2 is subjected to bubbling washing by condensate in the separator, and residual hydrogen sulfide in the ammonia gas is removed by circulating packing washing by condensate in the separator;
the ammonia gas flashed by the washed depressurization washing separator 2 enters a cooler 4 to be cooled to normal temperature, depressurized to 0.05MPa (g), enters a depressurization bubbling separator, the ammonia gas cooled and flashed in the cooler is bubbled and washed by condensate in the separator, and the ammonia gas flashed by the depressurization bubbling separator subjected to bubbling washing is sent to a step five ammonia absorber;
o, the condensate of the depressurization washing separator 1, the depressurization washing separator 2 and the depressurization bubbling separator are separated and then are pressurized by a centrifugal pump to be sent into an ammonia recovery tower for cyclic treatment;
production of ammonia product
The ammonia gas from the flash evaporation of the depressurization bubbling separator enters an ammonia absorber and is mixed with desalted water to prepare ammonia water, and H in the ammonia water 2 S≤10ppm。
2. The process for removing acid gas from an acidic condensate containing ammonia and recovering ammonia according to claim 1, wherein in the step (one), the concentrated acidic gas containing ammonia, the acidic gas in the shifted condensate and ammonia are all stripped and taken out simultaneously in a pressurized stripper and sent to the step (two).
3. The process for removing acid gas from ammonia-containing acidic condensate and recovering ammonia according to claim 1, wherein in step (one), the flashed condensate is simultaneously subjected to heat exchange with the tower bottom liquid of the acid gas removing tower in step (two) through a temperature raising heat exchanger, and the temperature is raised to 80-100 ℃ and is input from the upper part of the pressurized stripping tower.
4. The process for removing acid gas from an ammonia-containing acidic condensate and recovering ammonia according to claim 1, wherein in step (one) B, the pressurized stripping column is operated under a pressure of 0.2MPa (g) to 0.3MPa (g), and the bottom of the column is directly fed with low-pressure steam of 0.5MPa (g) to supply heat.
5. The process for removing acid gas from an ammonia-containing acidic condensate and recovering ammonia according to claim 1, wherein in step (two), the acid gas and ammonia are separated in the acid gas removal column by controlling the variation trend of the ionization balance and the dissolution balance influenced by the operation environment conditions, and are not simultaneously enriched in the same region, thereby eliminating the formation of ammonium carbamate.
6. The process for removing acid gas from an ammonia-containing acidic condensate and recovering ammonia according to claim 1, wherein in the second step, the top of the acid gas removing column is operated under a pressure of 0.13MPa (g) to 0.16MPa (g); the tower bottom is operated at 110-120 ℃, and the tower top is operated at 40-50 ℃.
7. The process for removing acid gas from ammonia-containing acidic condensate and recovering ammonia according to claim 1, wherein in step (III), the acid gas containing a small amount of ammonia gas, which is taken out from the top of the ammonia gas recovery tower, is returned to the acid gas removal tower in step (II), stripping and separating the acid gas and ammonia are performed again, the acid gas is removed, and ammonia is left in the tower bottom; and (3) in the step (II), the tower bottom of the acid gas removal tower contains a small amount of ammonia water condensate of acid gas, and the ammonia water condensate is sent to the ammonia recovery tower in the step (III) to obtain ammonia at the side line.
8. The process for removing acid gas from ammonia-containing acidic condensate and recycling ammonia according to claim 7, wherein the acid gas taken out from the top of the acid gas removing tower has low ammonia content and mass concentration less than or equal to 100ppm, and the removed acid gas is sent to sulfur for recycling; the hydrogen sulfide content and the mass concentration of the acid gas contained in the gas ammonia extracted from the side line of the ammonia recovery tower are less than or equal to 300ppm, the carbon dioxide content and the mass concentration are less than or equal to 1000ppm, and the gas ammonia is sent to the step (four) for refining.
9. The process for removing acid gas from an ammonia-containing acidic condensate and recovering ammonia according to claim 1, wherein in the third step, the recovered liquid after the temperature is raised to 140 ℃ to 150 ℃ is fed from the upper part of an ammonia recovery tower; the operation pressure of the top of the ammonia recovery tower is 0.5MPa (g); the operation temperature of the tower bottom is 158-165 ℃, and the operation temperature of the tower top is 55-65 ℃; the temperature of the side extracted ammonia gas is 148-152 ℃.
10. The process for removing acid gas from ammonia-containing acidic condensate and recycling ammonia according to claim 1, wherein in the step (four), ammonia gas extracted from a side line of the ammonia recycling tower in the step (three) is subjected to 1-stage cooling and depressurization, then subjected to 2-stage cooling and depressurization, and subjected to condensate circulation washing through a washing separator; then 3-stage cooling and depressurization are carried out, and bubbling washing is adopted through a washing separator; dissolving the carbon dioxide and hydrogen sulfide which are the acid gases and escape without being dissolved by the condensate liquid in the separated condensate liquid again; the condensate after the cyclic washing is sent to the ammonia recovery tower of the step (III) again to remove acid gas and recover ammonia; cooling the ammonia gas after 3-stage cooling, depressurizing and washing to normal temperature, and then, introducing the ammonia gas into a depressurizing bubbling separator for bubbling separation to obtain flash-separated high-purity ammonia gas, and sending the ammonia gas to the step (V) to prepare ammonia water.
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