CN118949646B - Device and method for purifying crude ammonia and preparing liquid ammonia - Google Patents
Device and method for purifying crude ammonia and preparing liquid ammonia Download PDFInfo
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- CN118949646B CN118949646B CN202411419625.1A CN202411419625A CN118949646B CN 118949646 B CN118949646 B CN 118949646B CN 202411419625 A CN202411419625 A CN 202411419625A CN 118949646 B CN118949646 B CN 118949646B
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- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 title claims abstract description 671
- 229910021529 ammonia Inorganic materials 0.000 title claims abstract description 269
- 238000000034 method Methods 0.000 title claims abstract description 16
- 238000005406 washing Methods 0.000 claims abstract description 151
- 238000007670 refining Methods 0.000 claims abstract description 95
- 239000002253 acid Substances 0.000 claims abstract description 79
- 239000006096 absorbing agent Substances 0.000 claims abstract description 37
- 239000007791 liquid phase Substances 0.000 claims abstract description 12
- 239000005416 organic matter Substances 0.000 claims abstract 6
- 239000007788 liquid Substances 0.000 claims description 58
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 56
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 56
- 238000010521 absorption reaction Methods 0.000 claims description 52
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 32
- 238000010992 reflux Methods 0.000 claims description 22
- 239000010865 sewage Substances 0.000 claims description 16
- 239000000945 filler Substances 0.000 claims description 15
- 238000001816 cooling Methods 0.000 claims description 13
- 238000012856 packing Methods 0.000 claims description 11
- 239000002994 raw material Substances 0.000 claims description 9
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 6
- 229910052717 sulfur Inorganic materials 0.000 claims description 6
- 239000011593 sulfur Substances 0.000 claims description 6
- 239000012071 phase Substances 0.000 claims description 5
- 238000009833 condensation Methods 0.000 claims description 2
- 230000005494 condensation Effects 0.000 claims description 2
- 238000005201 scrubbing Methods 0.000 claims 4
- 238000005265 energy consumption Methods 0.000 abstract 1
- 239000007789 gas Substances 0.000 description 63
- 239000000047 product Substances 0.000 description 10
- 238000002309 gasification Methods 0.000 description 6
- 239000002351 wastewater Substances 0.000 description 5
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 description 3
- 238000007599 discharging Methods 0.000 description 3
- 239000003921 oil Substances 0.000 description 3
- 150000002989 phenols Chemical class 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- XKMRRTOUMJRJIA-UHFFFAOYSA-N ammonia nh3 Chemical compound N.N XKMRRTOUMJRJIA-UHFFFAOYSA-N 0.000 description 2
- 239000012141 concentrate Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 239000000284 extract Substances 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 239000013589 supplement Substances 0.000 description 1
- 230000001502 supplementing effect Effects 0.000 description 1
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/38—Removing components of undefined structure
- B01D53/40—Acidic components
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/007—Energy recuperation; Heat pumps
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/14—Fractional distillation or use of a fractionation or rectification column
- B01D3/143—Fractional distillation or use of a fractionation or rectification column by two or more of a fractionation, separation or rectification step
- B01D3/146—Multiple effect distillation
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/002—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by condensation
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/14—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by absorption
- B01D53/18—Absorbing units; Liquid distributors therefor
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/46—Removing components of defined structure
- B01D53/48—Sulfur compounds
- B01D53/52—Hydrogen sulfide
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
- B01D53/75—Multi-step processes
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
- B01D53/77—Liquid phase processes
- B01D53/78—Liquid phase processes with gas-liquid contact
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/96—Regeneration, reactivation or recycling of reactants
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01C—AMMONIA; CYANOGEN; COMPOUNDS THEREOF
- C01C1/00—Ammonia; Compounds thereof
- C01C1/02—Preparation, purification or separation of ammonia
- C01C1/024—Purification
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01C—AMMONIA; CYANOGEN; COMPOUNDS THEREOF
- C01C1/00—Ammonia; Compounds thereof
- C01C1/02—Preparation, purification or separation of ammonia
- C01C1/12—Separation of ammonia from gases and vapours
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
- F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
- F25J1/00—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures
- F25J1/02—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures requiring the use of refrigeration, e.g. of helium or hydrogen ; Details and kind of the refrigeration system used; Integration with other units or processes; Controlling aspects of the process
- F25J1/0228—Coupling of the liquefaction unit to other units or processes, so-called integrated processes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2257/00—Components to be removed
- B01D2257/40—Nitrogen compounds
- B01D2257/406—Ammonia
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2257/00—Components to be removed
- B01D2257/70—Organic compounds not provided for in groups B01D2257/00 - B01D2257/602
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- Gas Separation By Absorption (AREA)
Abstract
The invention discloses a device and a method for purifying crude ammonia and preparing liquid ammonia, which are used in combination through an acid gas washing tower and an ammonia refining tower, wherein the crude ammonia is subjected to three-stage washing in the acid gas washing tower, the ammonia is refined in the ammonia refining tower, the ammonia is condensed in an ammonia cooler, the ammonia is absorbed in an ammonia absorber, and the like, so that the multistage washing at different temperatures is realized in one device of the acid gas washing tower, the acid gas in the ammonia is fixed in a liquid phase, the acid gas content in the ammonia is less than 3ppm, and the organic matter content in the ammonia is less than 10ppm through the ammonia refining tower. Thoroughly solves the quality problem of ammonia products, provides diversified ammonia products, shortens the flow and reduces the energy consumption.
Description
Technical Field
The invention belongs to the field of ammonia purification, and particularly relates to a device and a method for purifying crude ammonia and simultaneously preparing liquid ammonia.
Background
The wastewater quality generated by different coal gasification technologies is different, the ammonia nitrogen wastewater quality generated by the fixed bed gasification technology is the most complex, and the wastewater often contains H 2S、CO2, oil, phenols and other pollutants, and the COD concentration in the wastewater before treatment is more than 20000 mg/L. The ammonia nitrogen wastewater is usually treated by adopting a steam stripping method, and ammonia resources are recovered after acid gas is removed. The conventional stripping process comprises single-tower pressurized stripping and double-tower pressurized stripping, and ammonia-containing steam is subjected to multistage fractional condensation to obtain crude ammonia with higher concentration, wherein the temperature of the crude ammonia is 50-60 ℃, the pressure is 0.2-0.3 mPa (G), H 2O＞1.5%(wt),H2 S is more than 2000ppm, and organic matters (oils, phenols and the like) are more than 3000ppm. Because the H 2 S and organic matters (oils, phenols, etc.) in the crude ammonia gas have high content, the crude ammonia gas can only be used for preparing strong ammonia water with low quality, thereby limiting the application of ammonia products and affecting the economic benefit of the ammonia products.
Disclosure of Invention
The technical scheme of the invention is that the device for purifying crude ammonia and preparing liquid ammonia comprises an acid gas washing tower, an ammonia refining tower, a lower washing circulating pump, a washing cooler, an upper washing circulating pump, an ammonia refining tower reboiler, an ammonia refining tower bottom metering pump, an ammonia cooler, a liquid ammonia tank, a liquid ammonia reflux pump, a liquid ammonia discharge pump, an ammonia absorber, an ammonia water tank, an ammonia water circulating pump and an ammonia lateral line sewage pump;
The crude ammonia gas is connected with the lower part of the acid gas washing tower through a pipeline, the bottom of the acid gas washing tower is connected with the inlet of a washing cooler through a lower washing circulating pump, the outlet of the washing cooler is connected with the middle lower part of the acid gas washing tower through a pipeline, and the outlet of the lower washing circulating pump is connected with an external raw material tank through a pipeline;
The top of the acid gas washing tower is connected with the middle part of the ammonia refining tower through a pipeline, the bottom of the ammonia refining tower is connected with the inlet of an ammonia refining tower reboiler through a pipeline, the outlet of the ammonia refining tower reboiler is connected with the lower part of the ammonia refining tower through a pipeline, and the bottom of the ammonia refining tower is connected to the outside of the tank through an ammonia refining tower bottom metering pump;
The middle part of the ammonia refining tower is connected to the middle part of the sour gas washing tower through an ammonia side line sewage pump, and the outlet of the middle upper part of the ammonia refining tower is divided into two paths, wherein one path is respectively connected with the middle part of the ammonia refining tower and the inlet pipeline of the ammonia side line sewage pump through pipelines, and the other path is connected with the middle lower part of the ammonia refining tower through pipelines;
The top of the ammonia refining tower is connected with the inlet of the ammonia cooler through a pipeline, the outlet of the ammonia cooler is connected with the top of the liquid ammonia tank through a pipeline, and the bottom of the liquid ammonia tank is divided into two paths through a liquid ammonia reflux pump, wherein one path is connected with the top of the ammonia refining tower through a pipeline, and the other path is connected with the lower part of an absorption section of the ammonia absorber through a pipeline;
The desalted water is connected with the top of the absorption section of the ammonia absorber through a pipeline, the bottom of the cooling section of the ammonia absorber is connected with the top of the ammonia water tank through a pipeline, the ammonia water tank is divided into three paths after passing through an ammonia water circulating pump, the first path is connected with the middle part of the absorption section of the ammonia absorber through a pipeline, the second path is connected with the top of the acid gas washing tower through a pipeline, and the third path is connected with external ammonia water through a pipeline.
Further, the ammonia absorber is divided into an absorption section and a cooling section, wherein the absorption section is provided with two sections of fillers, the upper section is desalted water one-time absorption filler, the lower section is circulating absorption filler, and the cooling section is arranged below the absorption section and is a horizontal shell-and-tube heat exchanger.
Further, the ammonia refining tower is divided into an upper section, a middle section and a lower section, wherein the upper section is provided with a rectifying section, the middle section is provided with a liquid collecting tank, the lower section is provided with a stripping section, and the upper part of the liquid collecting tank of the middle section is provided with annular filler.
The method for purifying crude ammonia and preparing liquid ammonia comprises the following steps:
Firstly, three-stage washing is carried out on crude ammonia gas in an acid gas washing tower
The method comprises the steps of introducing crude ammonia gas containing H 2 S and organic matters into the lower part of an acid gas washing tower, leading out washing liquid from the bottom of the acid gas washing tower, pressurizing by a lower washing circulating pump, carrying out heat exchange with chilled water outside the tank through a washing cooler, reducing the temperature to 20-30 ℃, introducing the ammonia gas into the upper part of a packing at the lower part of the acid gas washing tower, fully contacting with crude ammonia gas containing H 2 S and organic matters, carrying out mass transfer and heat transfer, absorbing acid gas in the crude ammonia gas, carrying out primary washing on the crude ammonia gas, periodically discharging sulfur-containing ammonia liquid from a lower washing circulating pump into an external raw material tank for stripping again, introducing washing liquid in the middle part of the acid gas washing tower from a liquid collecting tank, pressurizing by an upper washing circulating pump, introducing the washing liquid into the upper part of the middle part of the acid gas washing tower, carrying out secondary washing on the crude ammonia gas, further removing acid gas in the crude ammonia gas, introducing concentrated ammonia water from an ammonia water circulating pump from the top of the acid gas washing tower, carrying out tertiary washing on the crude ammonia gas, and simultaneously taking the ammonia gas as a supplementary liquid for the ammonia gas from the top of the acid gas washing tower, wherein the ammonia gas content of the ammonia gas is <3ppm;
second, ammonia refining is carried out on the gas ammonia in an ammonia refining tower
The ammonia gas coming out from the top of the acid gas washing tower enters from the lower part of the annular filler above the liquid collecting tank in the middle section of the ammonia refining tower, fully contacts with partial liquid phase of the low-temperature rectifying section from the upper section, transfers mass and heat, after the temperature is reduced, most of organic matters and partial ammonia gas in ammonia gas are condensed, gas-liquid separation is carried out, the liquid phase is collected in the liquid collecting tank, is pumped into the middle part of the acid gas washing tower through an ammonia side line sewage pump, and the gas phase enters into the rectifying section of the upper section, fully contacts with the reflux liquid in the upper section, transfers mass and heat, and further concentrates the ammonia gas;
Third step, condensing ammonia in ammonia cooler
The pure ammonia gas from the top of the ammonia refining tower is pressurized by a liquid ammonia reflux pump, and enters the top of the ammonia refining tower for reflux, wherein one part is taken as a product and is pressurized by a liquid ammonia discharge pump and then sent to the outside, and the other part is sent to an ammonia absorber for preparing concentrated ammonia water;
Fourth step, ammonia absorption is carried out in an ammonia absorber
The ammonia water is pumped from the liquid ammonia reflux pump and enters an ammonia absorber to carry out ammonia absorption, ammonia water and chilled water are subjected to indirect heat exchange, absorption heat of the ammonia is removed, the ammonia water is cooled and then enters an ammonia water tank, and then the ammonia water tank is pressurized by an ammonia water circulating pump and is divided into three paths, wherein the first path is taken as circulating absorption liquid and sent to an absorption section of the ammonia absorber to circularly absorb the ammonia, the second path is taken as supplementary liquid of an acid gas washing tower, and the third path is taken as ammonia water product to be sent out selectively.
The acid gas washing tower is further divided into an upper section and a lower section which are separated by a liquid collecting box, the lower section is provided with a first-stage circulation washing, the circulation washing temperature is controlled to be 20-30 ℃, the upper section is provided with a second-stage washing, the first-stage circulation washing is controlled to be 10-15 ℃, the other one is one-time washing, the primary washing liquid adopts finished product concentrated ammonia water, enters from the top of the acid gas washing tower, and is supplemented with liquid at the same time, and redundant sulfur-containing ammonia liquid is periodically discharged into a raw material tank for re-stripping.
Further, the primary circulation washing temperature of the lower section of the acid gas washing tower is controlled by the flow of chilled water of a washing cooler, the temperature of the chilled water is less than 20 ℃, the primary circulation washing temperature of the upper section is controlled by the flow of liquid ammonia of an ammonia side line sewage pump, and the temperature is controlled to be 10-15 ℃.
Further, the heat source of the ammonia refining tower is provided by an ammonia refining tower reboiler, the heating medium is hot water, the pressure of the ammonia refining tower is controlled to be 0.15mPa (G), the temperature of the tower top is controlled to be-13.5 ℃, the temperature of the tower bottom is controlled to be 60-65 ℃, and the content of gaseous ammonia organic matters discharged from the tower top is controlled to be less than 10ppm.
Further, the absorption pressure of the ammonia gas is arbitrarily regulated between 0 and 0.2 Pa (G), and the concentration of the ammonia water is 20 to 40 percent by weight.
Further, the heat source of the ammonia refining tower is provided by an ammonia refining tower reboiler, the operating temperature of the tower kettle of the ammonia refining tower is 60-65 ℃, the heating medium is hot water, and the temperature of the hot water is more than 85 ℃.
Further, the ammonia cooler provides low temperature through the gasification of cold source liquid ammonia, and the pressure of the cold side of the ammonia cooler is controlled to be less than or equal to 0.03mPa (G) so as to ensure that the cold source provides enough temperature.
The invention has the following beneficial effects
(1) The invention discloses a method for preparing ammonia gas, which comprises the steps of separating an acid gas washing tower into an upper section and a lower section by a liquid collecting box, wherein the lower section is provided with a first-stage circulation washing, the temperature of the circulation washing is controlled to be 20-30 ℃, the upper section is provided with two-stage washing, the first-stage circulation washing is controlled to be 10-15 ℃, the other stage circulation washing is one-time washing, the one-time washing liquid adopts finished product strong ammonia water, enters from the top of the acid gas washing tower, and simultaneously supplements liquid for the acid gas washing tower, and periodically discharges redundant sulfur-containing ammonia liquid into a raw material tank for steam stripping.
(2) The primary circulation washing temperature of the lower section of the sour gas washing tower is controlled by the flow of chilled water of a washing cooler, the temperature of the chilled water is less than 20 ℃, and the primary circulation washing temperature of the upper section is controlled by the flow of liquid ammonia of an ammonia side line sewage pump.
(3) The pressure of the ammonia refining tower is 0.15mPa (G), the temperature of the tower top is-13.5 ℃, the temperature of the tower bottom is 60-65 ℃, the ammonia refining tower is divided into upper, middle and lower sections, annular packing is arranged above a header tank of the middle section, desulfurized ammonia gas enters from below the annular packing and fully contacts with a part of liquid phase of a low-temperature rectifying section from the upper section, mass transfer and heat transfer are carried out, after the temperature is reduced, most of organic matters and part of ammonia gas in the ammonia gas are condensed, gas-liquid separation is carried out, the liquid phase is collected in the header tank, is pumped into the middle part of an acid gas washing tower through an ammonia side blowdown pump, the gas phase enters a rectifying section of the upper section of the ammonia refining tower and fully contacts with a packing of the upper section, the mass transfer and heat transfer are carried out, gas ammonia is further concentrated, and most of liquid phase of the rectifying section is introduced into a stripping section of the lower section through a pipeline, so that the organic matters and ammonia in the water are further extracted, and the content of the organic matters in the gas ammonia is less than 10ppm.
(4) The pure ammonia gas from the top of the ammonia refining tower is at 0.15mPa (G) and at-13.5 ℃, enters an ammonia cooler to cool the ammonia gas to-25 ℃, the ammonia cooler provides low temperature through gasification of a cold source (liquid ammonia), the pressure of the cold side of the ammonia cooler is controlled to be less than or equal to 0.03mPa (G) (corresponding to the gasification temperature of-28 ℃) so as to ensure that the cold source provides enough temperature, the pure ammonia gas is condensed into liquid ammonia and enters a liquid ammonia tank, one part of the liquid ammonia gas is pressurized by a liquid ammonia reflux pump and then enters the top of the ammonia refining tower to reflux, the other part of the liquid ammonia gas is taken as a product to be delivered after being pressurized by a liquid ammonia discharge pump, and the other part of the liquid ammonia gas is delivered to an ammonia absorber to prepare strong ammonia.
(5) The ammonia water is cooled and then enters an ammonia water tank, and is pressurized by an ammonia water circulating pump to be divided into three paths, wherein the first path is taken as circulating absorption liquid, the circulating absorption liquid is sent into the ammonia absorber absorption section for circulating ammonia absorption, the second path is taken as acid gas washing tower supplementing liquid, and the third path can be selectively taken as ammonia water product for outward delivery.
(6) The ammonia concentration of the ammonia refining tower is high (98%wt), and compared with the traditional ammonia water feeding (20%wt), the treatment load of the ammonia refining tower is greatly reduced, and the equipment investment is correspondingly reduced.
(7) The heat source of the ammonia refining tower is provided by an ammonia refining tower reboiler, the operating temperature of the tower kettle of the ammonia refining tower is 60-65 ℃, the heating medium is hot water, the hot water temperature is more than 85 ℃, and the consumption of steam is saved.
Drawings
FIG. 1 is a process flow diagram of the present invention;
The reference numerals indicate that the acid gas washing tower 1, the ammonia refining tower 2, the lower washing circulating pump 3, the washing cooler 4, the upper washing circulating pump 5, the ammonia refining tower reboiler 6, the ammonia refining tower bottom metering pump 7, the ammonia cooler 8, the liquid ammonia tank 9, the liquid ammonia reflux pump 10, the liquid ammonia discharging pump 11, the ammonia absorber 12, the ammonia tank 13, the ammonia water circulating pump 14 and the ammonia lateral line sewage pump 15.
Detailed Description
As shown in FIG. 1, the device for purifying crude ammonia and preparing liquid ammonia comprises an acid gas washing tower 1, an ammonia refining tower 2, a lower washing circulating pump 3, a washing cooler 4, an upper washing circulating pump 5, an ammonia refining tower reboiler 6, an ammonia refining tower bottom metering pump 7, an ammonia cooler 8, a liquid ammonia tank 9, a liquid ammonia reflux pump 10, a liquid ammonia discharge pump 11, an ammonia absorber 12, an ammonia water tank 13, an ammonia water circulating pump 14 and an ammonia lateral line sewage pump 15.
The ammonia absorber 12 is divided into an absorption section and a cooling section, wherein the absorption section is provided with two sections of fillers, the upper section is desalted water one-time absorption filler, the lower section is circulating absorption filler, and the cooling section is arranged below the absorption section and is a horizontal shell-and-tube heat exchanger.
The ammonia refining tower 2 is divided into an upper rectifying section, a middle collecting tank, a stripping section and an annular packing above the middle collecting tank.
The crude ammonia gas is connected with the lower part of the acid gas washing tower 1 through a pipeline, the bottom of the acid gas washing tower 1 is connected with the inlet of a washing cooler 4 through a lower washing circulating pump 3, the outlet of the washing cooler 4 is connected with the middle lower part of the acid gas washing tower 1 through a pipeline, and the outlet of the lower washing circulating pump 3 is connected with an external raw material tank through a pipeline.
The middle part of the acid gas washing tower 1 is connected with the middle upper part of the acid gas washing tower 1 through an upper washing circulating pump 5, the top of the acid gas washing tower 1 is connected with the middle part of the ammonia refining tower 2 through a pipeline, the bottom of the ammonia refining tower 2 is connected with the inlet of an ammonia refining tower reboiler 6 through a pipeline, the outlet of the ammonia refining tower reboiler 6 is connected with the lower part of the ammonia refining tower 2 through a pipeline, and the bottom of the ammonia refining tower 2 is connected to the outside of the tank through an ammonia refining tower bottom metering pump 7.
The middle part of the ammonia refining tower 2 is connected to the middle part of the sour gas washing tower 1 through an ammonia lateral line sewage pump 15.
The outlet at the upper part of the ammonia refining tower 2 is divided into two paths, one path is respectively connected with the middle part of the ammonia refining tower 2 and the inlet pipeline of the ammonia side line sewage pump 15 through pipelines, and the other path is connected with the middle lower part of the ammonia refining tower 2 through pipelines.
The top of the ammonia refining tower 2 is connected with the inlet of the ammonia cooler 8 through a pipeline, the outlet of the ammonia cooler 8 is connected with the top of the liquid ammonia tank 9 through a pipeline, the bottom of the liquid ammonia tank 9 is divided into two paths through a liquid ammonia reflux pump 10, one path is connected with the top of the ammonia refining tower 2 through a pipeline, the other path is connected with the lower part of the absorption section of the ammonia absorber 12 through a pipeline, and the bottom of the liquid ammonia tank 9 is connected with external liquid ammonia through a liquid ammonia discharge pump 11 through a pipeline.
The desalted water is connected with the top of the absorption section of the ammonia absorber 12 through a pipeline, the bottom of the cooling section of the ammonia absorber 12 is connected with the top of the ammonia water tank 13 through a pipeline, the ammonia water tank 13 is divided into three paths after passing through the ammonia water circulating pump 14, the first path is connected with the middle part of the absorption section of the ammonia absorber 12 through a pipeline, the second path is connected with the top of the acid gas washing tower 1 through a pipeline, and the third path is connected with external ammonia water through a pipeline.
The external frozen water inlet is respectively connected with the washing cooler 4 and the ammonia absorber 12 cooling section through pipelines, and the washing cooler 4 and the ammonia absorber 12 cooling section are connected with the external frozen water return through pipelines.
The external liquid ammonia is connected with an ammonia cooler 8 through a pipeline, and the ammonia cooler 8 is connected with external gas ammonia through a pipeline.
The process comprises the following steps:
The first step of acid gas washing, namely, introducing crude ammonia containing H 2 S and organic matters into the lower part of an acid gas washing tower 1, leading washing liquid out of the bottom of the acid gas washing tower 1, pressurizing by a lower washing circulating pump 3, carrying out secondary washing on the crude ammonia after the temperature of the washing liquid is reduced to 20-30 ℃, introducing the washing liquid into the upper part of the acid gas washing tower 1, filling the washing liquid above a filler at the lower part of the acid gas washing tower 1, fully contacting the washing liquid with crude ammonia containing H 2 S and organic matters, carrying out mass transfer, absorbing acid gas in the crude ammonia, carrying out primary washing on the crude ammonia, periodically discharging sulfur-containing ammonia liquid from the outlet of the lower washing circulating pump 3 into an external raw material tank for steam stripping, introducing the washing liquid in the middle part of the acid gas washing tower 1 from a liquid collecting tank, pressurizing by an upper washing circulating pump 5, introducing the washing liquid into the upper part of the acid gas washing tower 1, carrying out secondary washing on the crude ammonia, further removing the acid gas in the crude ammonia, controlling the temperature of the secondary washing by a liquid ammonia pump 15 to be 10-15 ℃, carrying out strong ammonia from the ammonia water pump 14, and introducing ammonia gas from the top of the ammonia side line from the top of the ammonia circulating tower as ammonia gas, and carrying out ammonia gas content of the ammonia gas after the ammonia gas is purified from the top of the tower 1, and taking ammonia gas as the ammonia gas with the ammonia content of the ammonia gas and the ammonia gas.
The second ammonia refining step comprises the steps that gas ammonia coming out of the top of the acid gas washing tower 1 enters from the lower part of annular packing above a liquid collecting tank in the middle section of the ammonia refining tower 2, fully contacts with liquid phase of a part of low-temperature rectifying section from the upper section, transfers mass and heat, after the temperature is reduced, most of organic matters and part of ammonia gas in ammonia gas are condensed, gas-liquid separation is carried out, the liquid phase is collected in the liquid collecting tank, the gas phase enters the middle part of the acid gas washing tower through an ammonia side sewage pump 15, the gas phase enters the rectifying section of the upper section, fully contacts with reflux liquid in the upper section, transfers mass and heat, further concentrates gas ammonia, most of liquid phase of the rectifying section is introduced into a stripping section of the lower section through a pipeline, further extracts organic matters and ammonia in water, a heat source of the ammonia refining tower 2 is provided by an ammonia refining tower reboiler 6, a heating medium is hot water, the pressure of the ammonia refining tower 2 is controlled to be 0.15mPa (G), the tower top temperature is-13.5 ℃, the tower bottom temperature is 60-65 ℃, and the content of gas ammonia organic matters coming out from the tower top is less than 10ppm.
And condensing the pure ammonia, namely enabling the pure ammonia to flow back to the top of the ammonia refining tower 2 after being pressurized by a liquid ammonia reflux pump 10, enabling the pure ammonia to flow out after being pressurized by a liquid ammonia discharge pump 11, and enabling the pure ammonia to flow out after being pressurized by the liquid ammonia reflux pump 10, enabling the pure ammonia to flow into an ammonia cooler 8, enabling the ammonia cooler 8 to cool the ammonia to 25 ℃ below zero, enabling the ammonia cooler 8 to provide low temperature through gasification of a cold source (liquid ammonia) so as to ensure that the cold source provides enough temperature, and enabling the pure ammonia to flow into a liquid ammonia tank 9 after being condensed into liquid ammonia, and enabling the pure ammonia to flow out after being pressurized by the liquid ammonia reflux pump 10, enabling the pure ammonia to be delivered to the ammonia absorber 12 after being pressurized by a liquid ammonia discharge pump 11 as a product, and enabling the pure ammonia to be delivered to the ammonia absorber 12 to prepare strong ammonia.
The fourth step of ammonia absorption, namely, the liquid ammonia sent from a liquid ammonia reflux pump 10 enters an ammonia absorber 12 for ammonia absorption, the ammonia absorber 12 is divided into an absorption section and a cooling section, the absorption section is provided with two sections of fillers, the upper section is desalted water once absorption filler, the lower section is circulating absorption filler, the cooling section is a horizontal shell-and-tube heat exchanger below the absorption section, ammonia water and chilled water indirectly exchange heat to remove the absorption heat of ammonia, the absorption pressure of the ammonia gas is randomly regulated between 0 and 0.2 Pa (G), the concentration of the ammonia water is 20-40 percent by weight, the ammonia water is cooled and then enters an ammonia water tank 13, and then the ammonia water is pressurized by an ammonia water circulating pump and is divided into three paths, wherein the first path is used as circulating absorption liquid, the circulating absorption liquid is sent into the absorption section of the ammonia absorber 12, the second path is used as the supplementary liquid of an acid gas washing tower 1, and the third path can be selectively sent as an ammonia water product.
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| CN102992351A (en) * | 2012-11-05 | 2013-03-27 | 青岛科技大学 | Method and device for purifying ammonia recovered from coal chemical industry wastewater |
| CN104355343A (en) * | 2014-11-04 | 2015-02-18 | 赛鼎工程有限公司 | Purification technology for ammonia recycled from wastewater from coal gasification |
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| JP2009256488A (en) * | 2008-04-17 | 2009-11-05 | Takuma Co Ltd | Gas purification system and ammonia treatment method |
| JP5501730B2 (en) * | 2009-10-22 | 2014-05-28 | 三菱重工業株式会社 | Ammonia recovery device and recovery method |
| CN108744882B (en) * | 2018-05-29 | 2021-02-26 | 浙江天采云集科技股份有限公司 | Method for recycling waste gas in LED-MOCVD process through full-temperature-range pressure swing adsorption ammonia extraction |
| CN220827260U (en) * | 2023-09-19 | 2024-04-23 | 爱智环境科技(西安)有限公司 | Coal gasification ammonia-containing wastewater high-efficiency comprehensive recovery device |
| CN220758035U (en) * | 2023-09-19 | 2024-04-12 | 爱智环境科技(西安)有限公司 | High-efficient ammonia stripping device of transform lime set single tower |
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| CN102992351A (en) * | 2012-11-05 | 2013-03-27 | 青岛科技大学 | Method and device for purifying ammonia recovered from coal chemical industry wastewater |
| CN104355343A (en) * | 2014-11-04 | 2015-02-18 | 赛鼎工程有限公司 | Purification technology for ammonia recycled from wastewater from coal gasification |
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