CN114887462A - Ammonia tail gas treatment device and treatment method - Google Patents
Ammonia tail gas treatment device and treatment method Download PDFInfo
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- CN114887462A CN114887462A CN202210520809.1A CN202210520809A CN114887462A CN 114887462 A CN114887462 A CN 114887462A CN 202210520809 A CN202210520809 A CN 202210520809A CN 114887462 A CN114887462 A CN 114887462A
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- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 title claims abstract description 120
- 229910021529 ammonia Inorganic materials 0.000 title claims abstract description 55
- 238000000034 method Methods 0.000 title claims abstract description 41
- 238000010521 absorption reaction Methods 0.000 claims abstract description 398
- 239000007788 liquid Substances 0.000 claims abstract description 76
- 238000006243 chemical reaction Methods 0.000 claims abstract description 62
- 238000012856 packing Methods 0.000 claims abstract description 50
- 239000000945 filler Substances 0.000 claims description 109
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 claims description 102
- DHMQDGOQFOQNFH-UHFFFAOYSA-N Glycine Chemical compound NCC(O)=O DHMQDGOQFOQNFH-UHFFFAOYSA-N 0.000 claims description 42
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 34
- 230000015572 biosynthetic process Effects 0.000 claims description 27
- 238000003786 synthesis reaction Methods 0.000 claims description 27
- VKYKSIONXSXAKP-UHFFFAOYSA-N hexamethylenetetramine Chemical compound C1N(C2)CN3CN1CN2C3 VKYKSIONXSXAKP-UHFFFAOYSA-N 0.000 claims description 25
- 239000004471 Glycine Substances 0.000 claims description 20
- 239000000463 material Substances 0.000 claims description 12
- 238000001816 cooling Methods 0.000 claims description 10
- 239000013589 supplement Substances 0.000 claims description 8
- FOCAUTSVDIKZOP-UHFFFAOYSA-N chloroacetic acid Chemical compound OC(=O)CCl FOCAUTSVDIKZOP-UHFFFAOYSA-N 0.000 claims description 3
- 229940106681 chloroacetic acid Drugs 0.000 claims description 3
- 230000003197 catalytic effect Effects 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 12
- 238000011084 recovery Methods 0.000 abstract description 3
- 238000004134 energy conservation Methods 0.000 abstract 1
- 230000007613 environmental effect Effects 0.000 abstract 1
- 229960002449 glycine Drugs 0.000 description 20
- 238000005507 spraying Methods 0.000 description 13
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 description 10
- 238000005070 sampling Methods 0.000 description 7
- 239000007921 spray Substances 0.000 description 6
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 4
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 description 4
- 229910052921 ammonium sulfate Inorganic materials 0.000 description 4
- 235000011130 ammonium sulphate Nutrition 0.000 description 4
- 230000009286 beneficial effect Effects 0.000 description 4
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 3
- 238000005406 washing Methods 0.000 description 3
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 235000019270 ammonium chloride Nutrition 0.000 description 2
- 235000011114 ammonium hydroxide Nutrition 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 235000013905 glycine and its sodium salt Nutrition 0.000 description 1
- 235000010299 hexamethylene tetramine Nutrition 0.000 description 1
- 229960004011 methenamine Drugs 0.000 description 1
- 230000003020 moisturizing effect Effects 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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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
- B01D53/14—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
- B01D53/14—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
-
- 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
- B01D53/1406—Multiple stage absorption
-
- 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
- B01D53/54—Nitrogen compounds
- B01D53/58—Ammonia
-
- 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
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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
- B01D53/96—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
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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
- B01J4/00—Feed or outlet devices; Feed or outlet control devices
- B01J4/001—Feed or outlet devices as such, e.g. feeding tubes
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01C—AMMONIA; CYANOGEN; COMPOUNDS THEREOF
- C01C1/00—Ammonia; Compounds thereof
- C01C1/16—Halides of ammonium
- C01C1/164—Ammonium chloride
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C227/00—Preparation of compounds containing amino and carboxyl groups bound to the same carbon skeleton
- C07C227/04—Formation of amino groups in compounds containing carboxyl groups
- C07C227/06—Formation of amino groups in compounds containing carboxyl groups by addition or substitution reactions, without increasing the number of carbon atoms in the carbon skeleton of the acid
- C07C227/08—Formation of amino groups in compounds containing carboxyl groups by addition or substitution reactions, without increasing the number of carbon atoms in the carbon skeleton of the acid by reaction of ammonia or amines with acids containing functional groups
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/20—Air quality improvement or preservation, e.g. vehicle emission control or emission reduction by using catalytic converters
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Abstract
The invention relates to an ammonia tail gas treatment device and a treatment method. The tail gas draught fan is connected with the reaction kettle, the reaction kettle is connected with the first-stage packing tower, the first-stage packing absorption tower is connected with the tail gas first-stage packing absorption tower, the tail gas first-stage packing absorption tower is connected with the tail gas second-stage packing absorption tower, the tail gas second-stage packing absorption tower is connected with the tail gas third-stage packing absorption tower, and the tail gas third-stage packing absorption tower is connected with the draught fan. The method comprises the following specific steps: the ammonia tail gas is conveyed to the reaction kettle through the draught fan for reaction, then conveyed to the packing absorption tower, sprayed and absorbed by the absorption liquid, and then conveyed to the draught fan for closed cycle absorption, and the absorbed absorption liquid is used for production. The method has the advantages of small equipment investment, energy conservation and environmental protection, and is suitable for the recovery process of the ammonia tail gas.
Description
Technical Field
The invention relates to an ammonia tail gas treatment device, in particular to an ammonia tail gas recovery treatment device.
Background
In the processes of aminoacetic acid synthesis production and ammonia water production, because of improper control of reaction conditions, ammonia tail gas is easy to escape, and the ammonia pollutes the environment and increases the production cost. At present, the technology for treating ammonia tail gas mainly comprises water washing absorption and sulfuric acid washing absorption, ammonium sulfate solution is produced after the ammonium sulfate washing absorption, and ammonia tail gas also exists in the process of extracting ammonium sulfate solid, and secondary pollution can be caused if the ammonium sulfate solution is not properly treated.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention provides ammonia tail gas treatment equipment and a recovery method thereof, wherein ammonia tail gas is conveyed to a reaction kettle and a primary filler absorption tower through a draught fan and is sprayed and absorbed by formaldehyde, unabsorbed tail gas is washed and absorbed by a first-stage filler absorption tower, a second-stage filler absorption tower and then is self-circulated, absorption liquid of urotropine produced by absorbing the formaldehyde is used for water for urotropine chemical materials, and ammonia water is washed and absorbed for water for a glycine synthesis process.
The ammonia tail gas treatment device comprises a draught fan, a reaction kettle, a first-stage packing absorption tower, a first-stage packing tower condenser, a first-stage circulating pump, a tail gas first-stage absorption tower condenser, a tail gas first-stage circulating pump, a tail gas second-stage absorption tower condenser, a tail gas second-stage circulating pump, a tail gas third-stage absorption tower and a tail gas third-stage circulating pump,
the induced draft fan is connected with the reaction kettle, and the top of the reaction kettle is connected with the lower part of the first-stage packing absorption tower;
the top of the first-stage packing absorption tower is connected with a tail gas packing absorption tower, the bottom of the tail gas packing absorption tower is connected with a tail gas circulating pump through a buffer tank, the tail gas circulating pump is connected to the upper part of the tail gas packing absorption tower to form circulation, and the top of the tail gas packing absorption tower is connected with a draught fan.
The tail gas filler absorption tower is at least composed of two stages of absorption towers connected in series, preferably composed of three stages of absorption towers connected in series, namely a tail gas first-stage filler absorption tower, a tail gas second-stage filler absorption tower and a tail gas third-stage filler absorption tower, wherein the top of the first-stage filler absorption tower is connected with the lower part of the tail gas first-stage filler absorption tower, the top of the tail gas first-stage filler absorption tower is connected with the lower part of the tail gas second-stage filler absorption tower, the top of the tail gas second-stage filler absorption tower is connected with the lower part of the tail gas third-stage filler absorption tower, and the top of the tail gas third-stage filler absorption tower is connected with a draught fan.
The bottom of the first-stage packing absorption tower is connected with a first-stage circulating pump through a first buffer tank, the first-stage circulating pump is respectively connected with a first-stage packing tower condenser and a reaction kettle, and the first-stage packing tower condenser is connected with the upper part of the first-stage packing absorption tower to form circulation.
The bottom of the tail gas first-stage packing absorption tower is connected with a tail gas first-stage circulating pump through a second buffer tank, the tail gas first-stage circulating pump is connected with a tail gas first-stage absorption tower condenser, and the tail gas first-stage absorption tower condenser is connected with the upper part of the tail gas first-stage packing absorption tower to form circulation.
The bottom of the tail gas secondary absorption tower is connected with a tail gas secondary circulating pump through a third buffer tank, the tail gas secondary circulating pump is respectively connected with a second buffer tank and a condenser of the tail gas secondary absorption tower, and the condenser of the tail gas secondary absorption tower is connected with the upper part of the tail gas secondary absorption tower to form circulation.
The bottom of the tail gas tertiary filler absorption tower is connected with a tail gas tertiary circulating pump through a buffer tank IV, and the output of the tail gas tertiary circulating pump is respectively connected with a buffer tank III and the upper part of the tail gas tertiary filler absorption tower to form circulation.
And the upper parts of the tail gas first-stage absorption tower, the tail gas second-stage absorption tower and the tail gas third-stage absorption tower are also provided with feed pipes for introducing water.
On the basis of the device, the invention also provides a method for treating ammonia tail gas, wherein the ammonia tail gas is sprayed and absorbed by formaldehyde through a reaction kettle of a draught fan and a first-stage packed tower, and the unabsorbed first-stage, second-stage and third-stage water is absorbed and then circularly absorbed, and the method comprises the following steps:
(1) ammonia tail gas enters a reaction kettle from an induced draft fan, formaldehyde absorption liquid is added into the reaction kettle and a first-stage filler absorption tower, the liquid level of the absorption tower is controlled to be 40-80% (volume fraction), a first-stage circulating pump is started, the absorbed tail gas enters the first-stage filler absorption tower, a part of absorption liquid obtained by absorbing the tail gas in the first-stage filler absorption tower is collected to a first-stage filler tower condenser through the first-stage circulating pump, self-circulation is carried out after temperature reduction, and a part of absorption liquid is collected to the reaction kettle through the first-stage circulating pump;
the ammonia tail gas comes from a glycine synthesis kettle, the glycine synthesis process is characterized in that chloroacetic acid and ammonia gas react under the catalytic action of urotropine to produce glycine and ammonium chloride, the reaction is carried out in the synthesis kettle, and the reaction temperature is controlled to be 70-85 ℃. The ammonia gas does not fully participate in the reaction, so that most of tail gas from the synthesis kettle is ammonia gas, and a small amount of formaldehyde gas (urotropine decomposition) is entrained with water vapor.
Controlling the pressure of the reaction kettle in the step (1) to be 0-2Mpa, controlling the temperature of the reaction kettle to be 20-80 ℃, and controlling the pH value of the reaction kettle to be 7-14;
(2) the unabsorbed tail gas in the first-stage filler absorption tower enters a tail gas absorption tower, the liquid level of the absorption tower is controlled to be 40-80% (volume fraction), water is added into the tail gas absorption tower to serve as absorption liquid, a tail gas circulating pump is started, the tail gas is absorbed and self-circulated after being qualified, in the circulating process, the temperature is reduced to 0-30 ℃ through a condenser for self-circulation, and if the temperature is lower than 30 ℃, condensation can not be carried out;
(3) and conveying the solution absorbed by the reaction kettle to a urotropine dissolving position to be used as material dissolving water, and conveying the solution absorbed by the tail gas absorption tower to a glycine synthesis procedure to be used as process water supplement.
In the step (2), the tail gas absorption towers are at least two stages of tail gas absorption towers which are connected in series; after the unabsorbed tail gas in the first-stage filler absorption tower sequentially enters each stage of tail gas absorption tower to be absorbed, part of absorption liquid of each stage of tail gas absorption tower is subjected to self-circulation (in the circulation process, the temperature is reduced to 0-30 ℃ through a condenser to be subjected to self-circulation), and part of absorption liquid is circulated from the last stage of tail gas absorption tower.
In a preferable scheme and a scheme that can be specifically realized, the tail gas absorption tower in the step (2) is a three-stage tail gas absorption tower connected in series, that is, the tail gas that is not absorbed in the first-stage filler absorption tower enters the first-stage tail gas absorption tower, and simultaneously, a top gas phase pipeline of the first-stage tail gas absorption tower from the second-stage tail gas absorption tower is opened, and a top gas phase pipeline of the second-stage tail gas absorption tower from the third-stage tail gas absorption tower from the second-stage tail gas absorption tower;
adding water into a tail gas primary absorption tower, a tail gas secondary absorption tower and a tail gas tertiary absorption tower to serve as absorption liquid, respectively starting a tail gas primary circulating pump, a tail gas secondary circulating pump and a tail gas tertiary circulating pump, wherein part of the absorption liquid obtained after absorption in the tail gas primary absorption tower, the tail gas secondary absorption tower and the tail gas tertiary absorption tower is subjected to self-circulation (in the circulation process, the temperature is reduced to 0-30 ℃ through a condenser for self-circulation), and part of the absorption liquid is stepped on the tail gas secondary filler absorption tower through the tail gas tertiary filler absorption tower and is stepped on the tail gas primary filler absorption tower through the tail gas secondary filler absorption tower;
the ammonia tail gas is respectively absorbed by a reaction and a filler absorption tower, a tail gas primary absorption tower, a tail gas secondary absorption tower and a tail gas tertiary absorption tower, and is self-circulated after being qualified.
Cooling a part of absorption liquid in an absorption tower of the packed tower to 20-80 ℃ by a condenser; conveying a part of the enrichment liquid to a reaction kettle, and simultaneously controlling the treading flow to be 0.5-2m 3 H; the concentration of formaldehyde is 5% -37%.
Cooling a part of absorption liquid in the step (2) to 0-30 ℃ through a condenser; part of the enrichment solution sequentially passes through a tail gas three-stage filler absorption tower, a tail gas two-stage filler absorption tower and a tail gas one-stage filler absorption tower, and the treading flow is controlled to be 0.5-2m 3 /h。
By adopting the technical scheme of the invention, the absorption liquid is completely recycled, the treatment cost of the absorption liquid is reduced, and the production cost is reduced; adding absorption liquid into the filler absorption tower, controlling the liquid level of the absorption tower, starting a spray circulating absorption pump of the absorption tower, cooling a part of absorption liquid by a condenser for self-circulation, replenishing a part of enrichment liquid to the filler absorption tower from back to front, and adopting a continuous treading and continuous replenishing mode; because the absorption amount of the absorption liquid for absorbing ammonia gas is certain, the absorption liquid is used as water for the synthetic process of methenamine and glycine after absorption, and no absorption liquid is used for secondary treatment. The absorbed tail gas is self-circulated without discharge.
The method has the following advantages:
(1) the equipment has high automation degree, can be controlled in a full-automatic way, and realizes unmanned control.
(2) The pressurization is beneficial to the absorption of the ammonia tail gas, and the ammonia tail gas has good treatment effect and no discharge phenomenon.
(3) The recovered ammonia tail gas can be used in the production process, and the production cost is reduced.
Drawings
Fig. 1 is an ammonia tail gas processing apparatus, wherein, draught fan 1, reation kettle 2, one-level filler absorption tower 3, one-level filler tower condenser 4, one-level circulating pump 5, tail gas one-level absorption tower 6, tail gas one-level absorption tower condenser 7, tail gas one-level circulating pump 8, tail gas second grade absorption tower 9, tail gas second grade absorption tower condenser 10, tail gas second grade circulating pump 11, tail gas tertiary absorption tower 12, tail gas tertiary circulating pump 13, buffer tank one 14, buffer tank two 15, buffer tank three 16, buffer tank four 17.
DETAILED DESCRIPTION OF EMBODIMENT (S) OF INVENTION
Example 1
An ammonia tail gas treatment device comprises an induced draft fan 1, a reaction kettle 2, a primary filler absorption tower 3, a primary filler tower condenser 4, a primary circulating pump 5, a tail gas primary absorption tower 6, a tail gas primary absorption tower condenser 7, a tail gas primary circulating pump 8, a tail gas secondary absorption tower 9, a tail gas secondary absorption tower condenser 10, a tail gas secondary circulating pump 11, a tail gas tertiary absorption tower 12 and a tail gas tertiary circulating pump 13, wherein the induced draft fan 1 is connected with the reaction kettle 2, and the top of the reaction kettle 2 is connected with the lower part of the primary filler absorption tower 3;
the top of the first-stage filler absorption tower 3 is connected with the lower part of the tail gas first-stage filler absorption tower 6, the top of the tail gas first-stage filler absorption tower 6 is connected with the lower part of the tail gas second-stage filler absorption tower 9, the top of the tail gas second-stage filler absorption tower 9 is connected with the lower part of the tail gas third-stage filler absorption tower 12, and the top of the tail gas third-stage filler absorption tower 12 is connected with the draught fan 1.
The bottom of the first-stage packed absorption tower 3 is connected with a first-stage circulating pump 5 through a first buffer tank 14, the first-stage circulating pump 5 is respectively connected with a first-stage packed tower condenser 4 and a reaction kettle 2, and the first-stage packed tower condenser 4 is connected with the upper part of the first-stage packed absorption tower 3 to form circulation.
The bottom of the tail gas first-stage packing absorption tower 6 is connected with a tail gas first-stage circulating pump 8 through a second buffer tank 15, the tail gas first-stage circulating pump 8 is connected with a tail gas first-stage absorption tower condenser 7, and the tail gas first-stage absorption tower condenser 7 is connected with the upper part of the tail gas first-stage packing absorption tower 6 to form circulation.
The bottom of the tail gas secondary absorption tower 9 is connected with a tail gas secondary circulating pump 11 through a third buffer tank 16, the output of the tail gas secondary circulating pump 11 is respectively connected with the third buffer tank 16 and a tail gas secondary absorption tower condenser 10, and the tail gas secondary absorption tower condenser 10 is connected with the upper part of the tail gas secondary absorption tower 9 to form circulation.
The bottom of the tail gas tertiary packing absorption tower 12 is connected with a tail gas tertiary circulating pump 13 through a buffer tank IV 17, and the output of the tail gas tertiary circulating pump 13 is respectively connected with the buffer tank IV 17 and the upper part of the tail gas tertiary packing absorption tower 12 to form circulation.
Example 2
The glycine synthesis process is that chloroacetic acid and ammonia gas react under the catalysis of urotropine to produce glycine and ammonium chloride, the reaction is carried out in the synthesis kettle, and the reaction temperature is controlled to 70-85 ℃. As ammonia gas does not sufficiently participate in the reaction, 94.5 percent (volume fraction) of ammonia gas, 0.5 percent (volume fraction) of formaldehyde gas and 5 percent (volume fraction) of water vapor are carried in tail gas from the synthesis kettle. Specifically, the ammonia treatment process was carried out by using the apparatus of example 1, adding 10% by mass of formaldehyde into a reactor, controlling the pressure of the reactor to 0.3Mpa, automatically releasing the pressure by overpressure to a subsequent tail gas absorption tower, controlling the temperature of the reactor to 60 ℃, controlling the pH of the reactor to 12, adding 10% of formaldehyde into a first-stage packed absorption tower, controlling the liquid level of the absorption tower to 40%, and starting the packed tower to spray for cyclic absorptionPump, carrying out self-circulation by cooling 97% volume fraction formaldehyde absorption liquid to 50 ℃ through a condenser at 30 m/h, carrying out self-circulation by absorbing 3% volume fraction formaldehyde (enrichment liquid) to a urotropine removal material pond through a reaction kettle at 1 m/h, and controlling the flow of the urotropine removal material pond at the bottom of the reaction kettle to be 1m 3 H is used as the reference value. Unabsorbed tail gas gets into tail gas one-level absorption tower, tail gas second grade absorption tower, the tertiary absorption tower of tail gas, to tail gas one, two, add water in the tertiary absorption tower that packs, control tail gas one, two, tertiary absorption tower liquid level is 40%, open the tower that packs separately and spray the circulation absorption pump, after absorbing, 97% volume fraction's absorption liquid with 30m thin year/h through the condenser cooling to 15 ℃ carry out the self-loopa, 3% volume fraction's enrichment liquid with 1m year/h get into tail gas second grade absorption tower through the tertiary absorption tower of tail gas in proper order, get into the glycine synthesis technology moisturizing from tail gas second grade absorption tower that packs. Conveying the tail gas to a reaction kettle and a first-stage filler absorption tower through a draught fan, spraying and absorbing the tail gas by formaldehyde, and performing self-circulation after the unabsorbed tail gas is washed and absorbed by the first-stage filler absorption tower, the second-stage filler absorption tower and the third-stage filler absorption tower. In the tank for removing urotropine, the content of urotropine is 5.5 percent, and the ammonia content is 0.15 percent by sampling at the top of the tail gas three-level filler absorption tower.
In another example of this case, it is found that effective absorption of ammonia tail gas can be achieved when the concentration of formaldehyde in the feeding process is 5%, 10%, 15%, 20%, 25%, 30%, 35%, 37%, while too low concentration of formaldehyde, such as 3%, has too high absorption pressure to the first, second, and third packing absorption towers of tail gas, which makes it difficult to achieve water absorption, and finally, the top of the third packing absorption tower of tail gas has a large ammonia taste, which proves that the absorption is incomplete. The concentration is higher, such as 40 percent of formaldehyde concentration, the cost is too high, and the tail gas treatment link is not facilitated.
In another embodiment of the present application, it is found that, in the process of adding water to the first, second, and third stages of filler absorption towers for absorption, after absorption, the respective circulation amounts are circulated in volume fractions of 95%, 96%, 97%, 98%, and 98.5%, which is beneficial to absorption of ammonia in the tail gas, and since ammonia is very soluble in water, the ammonia is more beneficial to absorption in the process of circulating and condensing to within 15 ℃, and the enrichment liquid is also beneficial to supplement from the rear to the front filler absorption tower, so that a continuous treading and continuous supplement process is realized. If the circulation amount is less than 95%, for example, less than 94% and less, the ammonia content tends to be higher than 2.5% by sampling the top of the tail gas tertiary packed absorption column.
Example 3
An ammonia treatment process is performed by using the apparatus in embodiment 1, synthesis tail gas in glycine production (synthesis tail gas in example 2) is added into a reaction kettle, the mass fraction of formaldehyde is 14%, the pressure of the reaction kettle is controlled to 0.5Mpa, overpressure is automatically released to remove a subsequent tail gas absorption tower, the temperature of the reaction kettle is controlled to 65 ℃, the pH value of the reaction kettle is controlled to 11.8, 14% of formaldehyde is added into a first-stage filler absorption tower, the liquid level of the absorption tower is controlled to 60%, a filler tower spraying circulating absorption pump is started, 98.3% of formaldehyde absorption liquid with volume fraction is cooled to 53 ℃ through a condenser by 20m and/h for self-circulation, 1.7% of formaldehyde (enrichment liquid) with volume fraction is absorbed by the reaction kettle by 0.5m and/h for removing urotroping material pool, and the flow rate of the urotroping material pool is controlled to 0.5m and is controlled to be 0.5m 3 H is used as the reference value. Unabsorbed tail gas enters a tail gas first-stage absorption tower, a tail gas second-stage absorption tower and a tail gas third-stage absorption tower, water is added into the tail gas first-stage absorption tower, water is added into the tail gas second-stage absorption tower and the tail gas third-stage absorption tower, the liquid levels of the tail gas first-stage absorption tower, the liquid levels of the tail gas second-stage absorption tower and the tail gas third-stage absorption tower are controlled to be 60%, a spraying circulating absorption pump of a packed tower is started, after absorption, absorption liquid with the volume fraction of 98.3% is subjected to self circulation after being cooled to 15 ℃ through a condenser at the speed of 30 m/h, enrichment liquid with the volume fraction of 1.7% sequentially passes through the tail gas third-stage absorption tower at the speed of 0.5 m/h and enters the tail gas second-stage absorption tower, and then enters the tail gas first-stage packed absorption tower from the tail gas second-stage packed absorption tower to remove water in the glycine synthesis process. Conveying the tail gas to a reaction kettle and a first-stage filler absorption tower through a draught fan, spraying and absorbing the tail gas by formaldehyde, and performing self-circulation after the unabsorbed tail gas is washed and absorbed by the first-stage filler absorption tower, the second-stage filler absorption tower and the third-stage filler absorption tower. The content of urotropine in the urotropine removal pond is 6.3 percent, and the ammonia content is 0.12 percent by sampling at the top of a tail gas three-level filler absorption tower.
Example 4
The ammonia treatment process was carried out using the apparatus of example 1, the synthesis tail gas from the glycine production (example 2 synthesis tail gas) was added to a reaction vessel with a mass fraction of 15% formaldehyde, the pressure of the reaction vessel was controlled to 0.3Mpa and overpressureThe automatic pressure relief subsequent tail gas removal absorption tower is realized, the temperature of a reaction kettle is controlled to 65 ℃, the pH value of the reaction kettle is controlled to 12, 15% of formaldehyde is added into a first-stage packing absorption tower, the liquid level of the absorption tower is controlled to 50%, a packing tower spraying circulating absorption pump is started, 96.2% of formaldehyde absorption liquid with volume fraction is cooled to 50 ℃ through a condenser for self-circulation through 15m of methane/h, 3.8% of formaldehyde (enrichment liquid) with volume fraction is cooled to 50 ℃ through the reaction kettle through 0.6m of methane/h, and the flow of the urotropine removal material pool is controlled to be 0.6m 3 H is used as the reference value. Unabsorbed tail gas enters a tail gas first-stage absorption tower, a tail gas second-stage absorption tower and a tail gas third-stage absorption tower, water is added into the tail gas first-stage absorption tower, water is added into the tail gas second-stage absorption tower and a tail gas third-stage absorption tower, the liquid levels of the tail gas first-stage absorption tower, the tail gas second-stage absorption tower and the tail gas third-stage absorption tower are controlled to be 50%, a packed tower spraying circulating absorption pump is started, after absorption, absorption liquid with the volume fraction of 98.3% is subjected to self circulation after being cooled to 15 ℃ through a condenser at the speed of 30m and subjected to self-cultivation/h, enrichment liquid with the volume fraction of 1.7% is subjected to self-cultivation at the speed of 0.5m and is sequentially subjected to tail gas third-stage absorption tower entering the tail gas second-stage absorption tower, and then entering the tail gas first-stage packed absorption tower from the tail gas second-stage absorption tower to remove glycine synthesis process water supplement. Conveying the tail gas to a reaction kettle and a first-stage filler absorption tower through a draught fan, spraying and absorbing the tail gas by formaldehyde, and performing self-circulation after the unabsorbed tail gas is washed and absorbed by the first-stage filler absorption tower, the second-stage filler absorption tower and the third-stage filler absorption tower. In the tank for removing urotropine, the content of urotropine is 7.2 percent, and the ammonia content is 0.13 percent by sampling at the top of a tail gas three-level filler absorption tower.
Example 5
Adopt embodiment 1's device to carry out ammonia processing technology, with synthetic tail gas in glycine production (example 2 synthetic tail gas), add mass fraction into reation kettle for 15% formaldehyde, reation kettle's pressure control is to 0.5Mpa, the superpressure is automatic to be decompressed and is removed follow-up tail gas absorption tower, reation kettle's temperature control is to 70 ℃, reation kettle's pH value controls 12, add 15% formaldehyde to one-level filler absorption tower, control absorption tower liquid level is 60%, open filler tower spraying circulation absorption pump, 95.2% volume fraction's formaldehyde absorption liquid is with 10m year/h through the condenser cooling to 55 ℃ and carry out self-loopa, 4.8% volume fraction's formaldehyde (enrichment liquid) absorbs the material pond that goes urotroping with 0.5m year/h reation kettle in proper order, control goes urotroping material pond to goThe flow rate is 0.5m 3 H is used as the reference value. Unabsorbed tail gas enters a tail gas first-stage absorption tower, a tail gas second-stage absorption tower and a tail gas third-stage absorption tower, water is added into the tail gas first-stage absorption tower, the tail gas second-stage absorption tower and the tail gas third-stage absorption tower, the liquid levels of the tail gas first-stage absorption tower, the tail gas second-stage absorption tower and the tail gas third-stage absorption tower are controlled to be 60%, a packed tower spraying circulating absorption pump is started, after absorption is carried out, absorption liquid with the volume fraction of 98.3% is sent out at 30 m/h and cooled to 15 ℃ through a condenser for self circulation, enrichment liquid with the volume fraction of 1.7% sequentially passes through the tail gas third-stage absorption tower and enters the tail gas second-stage absorption tower from the tail gas second-stage absorption tower, and then enters the tail gas first-stage packed absorption tower for glycine removal synthesis process water supplement. Conveying the tail gas to a reaction kettle and a first-stage filler absorption tower through a draught fan, spraying and absorbing the tail gas by formaldehyde, and performing self-circulation after the unabsorbed tail gas is washed and absorbed by the first-stage filler absorption tower, the second-stage filler absorption tower and the third-stage filler absorption tower. In the tank for removing urotropine, the content of urotropine is 8.9 percent, and the ammonia content is 0.09 percent by sampling at the top of a tail gas three-level filler absorption tower.
Example 6
An ammonia treatment process was performed by using the apparatus of example 1, using the synthesis tail gas from glycine production (example 2 synthesis tail gas), adding 10% by mass of formaldehyde into a reactor, controlling the pressure of the reactor to 0.3Mpa, automatically releasing pressure at overpressure to a subsequent tail gas absorption tower, controlling the temperature of the reactor to 60 ℃, controlling the pH of the reactor to 12, adding 10% of formaldehyde into a first-stage packed absorption tower, controlling the liquid level of the absorption tower to 40%, starting a packed tower spray circulation absorption pump, cooling 66.7% by volume of formaldehyde absorption liquid from 10 mn/h of formaldehyde to 50 ℃ by a condenser, performing self-circulation, absorbing 33.3% by volume of formaldehyde (enrichment liquid) from 5 mn/h of the reactor sequentially to a urotroping material removal pool, and controlling the flow of the urotroping material removal pool to 5m 3 H is used as the reference value. Unabsorbed tail gas gets into tail gas one-level absorption tower, tail gas second grade absorption tower, tertiary absorption tower of tail gas, to tail gas one, two, add water in the three filler absorption towers, control tail gas one, two, three filler absorption tower liquid level is 40%, open the filled tower and spray the circulation absorption pump, after absorbing, 97% volume fraction's absorption liquid with 30m thin year of a year/h through the condenser cooling to 15 ℃ carry out the self-loopa, 3% volume fraction's enrichment liquid follows year by year/h through the tertiary absorption tower of tail gas in proper order with 1mThe absorption tower enters a tail gas secondary filler absorption tower, and then enters a tail gas primary filler absorption tower from the tail gas secondary filler absorption tower to remove water supplement of a glycine synthesis process. Conveying the tail gas to a reaction kettle and a first-stage filler absorption tower through a draught fan, spraying and absorbing the tail gas by formaldehyde, and performing self-circulation after the unabsorbed tail gas is washed and absorbed by the first-stage filler absorption tower, the second-stage filler absorption tower and the third-stage filler absorption tower. In the tank for removing urotropine, the content of urotropine is 2.0 percent, and the ammonia content is 1.1 percent by sampling at the top of a tail gas three-level filler absorption tower.
Example 7
An ammonia treatment process was performed by using the apparatus of example 1, using the synthesis tail gas from glycine production (example 2 synthesis tail gas), adding 15% by mass of formaldehyde into a reactor, controlling the pressure of the reactor to 0.3Mpa, automatically releasing pressure at overpressure to a subsequent tail gas absorption tower, controlling the temperature of the reactor to 65 ℃, controlling the pH of the reactor to 12, adding 15% by mass of formaldehyde into a first-stage packed absorption tower, controlling the liquid level of the absorption tower to 50%, starting a packed tower spray circulation absorption pump, cooling 33.3% by volume of formaldehyde absorption liquid to 50 ℃ by a condenser at 15m and a rack/h, performing self-circulation, absorbing 16.7% by volume of formaldehyde (enrichment liquid) to a urotroping removal pool at 3m and a rack/h by the reactor, and controlling the flow of the urotroping removal pool to 3m 3 H is used as the reference value. Unabsorbed tail gas enters a tail gas first-stage absorption tower, a tail gas second-stage absorption tower and a tail gas third-stage absorption tower, water is added into the tail gas first-stage absorption tower, water is added into the tail gas second-stage absorption tower and a tail gas third-stage absorption tower, the liquid levels of the tail gas first-stage absorption tower, the tail gas second-stage absorption tower and the tail gas third-stage absorption tower are controlled to be 50%, a packed tower spraying circulating absorption pump is started, after absorption, absorption liquid with the volume fraction of 98.3% is subjected to self circulation after being cooled to 15 ℃ through a condenser at the speed of 30m and subjected to self-cultivation/h, enrichment liquid with the volume fraction of 1.7% is subjected to self-cultivation at the speed of 0.5m and is sequentially subjected to tail gas third-stage absorption tower entering the tail gas second-stage absorption tower, and then entering the tail gas first-stage packed absorption tower from the tail gas second-stage absorption tower to remove glycine synthesis process water supplement. Conveying the tail gas to a reaction kettle and a first-stage filler absorption tower through a draught fan, spraying and absorbing the tail gas by formaldehyde, and performing self-circulation after the unabsorbed tail gas is washed and absorbed by the first-stage filler absorption tower, the second-stage filler absorption tower and the third-stage filler absorption tower. Removing urotropine from urotropine pond with urotropine content of 3.5%, sampling at the top of tail gas three-stage packing absorption tower to obtain ammonia contentIs 0.85%.
Claims (10)
1. An ammonia tail gas treatment device, which comprises a draught fan (1), a reaction kettle (2), a first-stage packing absorption tower (3), a first-stage packing tower condenser (4) and a first-stage circulating pump (5),
the induced draft fan (1) is connected with the reaction kettle (2), and the top of the reaction kettle (2) is connected with the lower part of the first-stage packing absorption tower (3);
the top of the first-stage packing absorption tower (3) is connected with a tail gas packing absorption tower, the bottom of the tail gas packing absorption tower is connected with a tail gas circulating pump through a buffer tank, the tail gas circulating pump is connected to the upper part of the tail gas packing absorption tower to form circulation, and the top of the tail gas packing absorption tower is connected with a draught fan (1).
2. The ammonia tail gas treatment device according to claim 1, wherein the tail gas filler absorption tower is composed of at least two absorption towers connected in series, preferably three absorption towers connected in series, namely a tail gas first-stage filler absorption tower (6), a tail gas second-stage filler absorption tower (9) and a tail gas third-stage filler absorption tower (12), then the top of the first-stage filler absorption tower (3) is connected with the lower part of the tail gas first-stage filler absorption tower (6), the top of the tail gas first-stage filler absorption tower (6) is connected with the lower part of the tail gas second-stage filler absorption tower (9), the top of the tail gas second-stage filler absorption tower (9) is connected with the lower part of the tail gas third-stage filler absorption tower (12), and the top of the tail gas third-stage filler absorption tower (12) is connected with the induced draft fan (1).
3. The ammonia off-gas treatment device according to claim 1,
the bottom of the first-stage packing absorption tower (3) is connected with a first-stage circulating pump (5) through a first buffer tank (14), the first-stage circulating pump (5) is respectively connected with a first-stage packing tower condenser (4) and a reaction kettle (2), and the first-stage packing tower condenser (4) is connected with the upper part of the first-stage packing absorption tower (3) to form circulation.
4. The ammonia off-gas treatment device according to claim 1,
the bottom of the tail gas first-level packing absorption tower (6) is connected with a tail gas first-level circulating pump (8) through a second buffer tank (15), the tail gas first-level circulating pump (8) is connected with a tail gas first-level absorption tower condenser (7), and the tail gas first-level absorption tower condenser (7) is connected with the upper part of the tail gas first-level packing absorption tower (6) to form circulation.
5. The ammonia off-gas treatment device according to claim 1,
the bottom of the tail gas secondary absorption tower (9) is connected with a tail gas secondary circulating pump (11) through a third buffer tank (16), the output of the tail gas secondary circulating pump (11) is respectively connected with a second buffer tank (15) and a condenser (10) of the tail gas secondary absorption tower, and the condenser (10) of the tail gas secondary absorption tower is connected with the upper part of the tail gas secondary absorption tower (9) to form circulation;
the bottom of the tail gas tertiary packing absorption tower (12) is connected with a tail gas tertiary circulating pump (13) through a buffer tank IV (17), and the output of the tail gas tertiary circulating pump (13) is respectively connected with a buffer tank III (16) and the upper part of the tail gas tertiary packing absorption tower (12) to form circulation.
6. The ammonia tail gas treatment method is characterized by comprising the following steps:
(1) ammonia tail gas enters a reaction kettle from a draught fan, formaldehyde absorption liquid is added into the reaction kettle and a first-stage filler absorption tower, a first-stage circulating pump is started, the absorbed tail gas enters a first-stage filler absorption tower, a part of absorption liquid obtained by absorbing the tail gas in the first-stage filler absorption tower is collected to a first-stage filler tower condenser through the first-stage circulating pump, self-circulation is carried out after temperature reduction, and a part of absorption liquid is collected to the reaction kettle through the first-stage circulating pump;
(2) the tail gas which is not absorbed in the first-stage filler absorption tower enters a tail gas absorption tower, water is added into the tail gas absorption tower to serve as absorption liquid, a tail gas circulating pump is started, and the tail gas is absorbed and self-circulated after being qualified;
(3) and conveying the solution absorbed by the reaction kettle to a urotropine dissolving position to be used as material dissolving water, and conveying the solution absorbed by the tail gas absorption tower to a glycine synthesis procedure to be used as process water supplement.
7. The ammonia off-gas treatment method according to claim 6,
the ammonia tail gas is tail gas from a synthesis kettle, most of the tail gas is ammonia gas, and a small amount of formaldehyde gas and entrained water vapor are generated in the synthesis kettle due to insufficient participation of the ammonia gas in the reaction process of chloroacetic acid and the ammonia gas at 70-85 ℃ under the catalytic action of urotropine;
in the step (2), the tail gas absorption towers are at least two stages of tail gas absorption towers which are connected in series; after unabsorbed tail gas in the first-stage packing absorption tower enters each stage of tail gas absorption tower in sequence to be absorbed, a part of absorption liquid of each stage of tail gas absorption tower is subjected to self-circulation, and a part of absorption liquid is circulated from the tail gas absorption tower of the previous stage by the next stage.
8. The ammonia tail gas treatment method according to claim 6, wherein the tail gas absorption tower in the step (2) is a three-stage tail gas absorption tower connected in series, that is, the unabsorbed tail gas in the first-stage packing absorption tower enters the first-stage tail gas absorption tower, and simultaneously a top gas phase pipeline of the first-stage tail gas absorption tower from the second-stage tail gas absorption tower is opened, and the second-stage tail gas absorption tower from a top gas phase pipeline of the third-stage tail gas absorption tower;
adding water serving as absorption liquid into a tail gas primary absorption tower, a tail gas secondary absorption tower and a tail gas tertiary absorption tower, respectively starting a tail gas primary circulating pump, a tail gas secondary circulating pump and a tail gas tertiary circulating pump, wherein a part of absorption liquid obtained after absorption in the tail gas primary absorption tower, the tail gas secondary absorption tower and the tail gas tertiary absorption tower is subjected to self-circulation, and a part of absorption liquid is stepped on the tail gas secondary filler absorption tower through the tail gas tertiary filler absorption tower and is stepped on the tail gas primary filler absorption tower through the tail gas tertiary filler absorption tower;
the ammonia tail gas is respectively absorbed by a reaction and a filler absorption tower, a tail gas primary absorption tower, a tail gas secondary absorption tower and a tail gas tertiary absorption tower, and is self-circulated after being qualified.
9. The method for treating ammonia off-gas according to claim 8, wherein the pressure of the reaction kettle in the step (1) is controlled to be 0-2Mpa, the temperature of the reaction kettle is controlled to be 20-80 ℃, and the pH value of the reaction kettle is controlled to be 7-14;
cooling a part of absorption liquid in an absorption tower of the packed tower to 20-80 ℃ by a condenser; conveying a part of the enrichment liquid to a reaction kettle, and simultaneously controlling the treading flow to be 0.5-2m 3/h; the concentration of formaldehyde is 5% -37%.
10. The method for treating ammonia off-gas according to claim 8, wherein the temperature of the part of the absorption liquid in the step (2) is reduced to 0-30 ℃ by a condenser; part of the enrichment solution sequentially passes through a tail gas three-stage filler absorption tower, a tail gas two-stage filler absorption tower and a tail gas one-stage filler absorption tower, and the treading flow is controlled to be 0.5-2m 3 /h。
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| CN115350573A (en) * | 2022-09-20 | 2022-11-18 | 威海市正大环保设备股份有限公司 | High-sulfur flue gas desulfurization method |
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