CN109704366B - Pressurized deacidification ammonia distillation heat coupling process and system - Google Patents

Pressurized deacidification ammonia distillation heat coupling process and system Download PDF

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Publication number
CN109704366B
CN109704366B CN201910109557.1A CN201910109557A CN109704366B CN 109704366 B CN109704366 B CN 109704366B CN 201910109557 A CN201910109557 A CN 201910109557A CN 109704366 B CN109704366 B CN 109704366B
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ammonia
tower
inlet
deacidification
gas
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CN109704366A (en
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李昊阳
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Acre Coking and Refractory Engineering Consulting Corp MCC
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Acre Coking and Refractory Engineering Consulting Corp MCC
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Priority to PCT/CN2020/070522 priority patent/WO2020164341A1/en
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01CAMMONIA; CYANOGEN; COMPOUNDS THEREOF
    • C01C1/00Ammonia; Compounds thereof
    • C01C1/02Preparation, purification or separation of ammonia
    • C01C1/10Separation of ammonia from ammonia liquors, e.g. gas liquors
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10KPURIFYING OR MODIFYING THE CHEMICAL COMPOSITION OF COMBUSTIBLE GASES CONTAINING CARBON MONOXIDE
    • C10K1/00Purifying combustible gases containing carbon monoxide
    • C10K1/08Purifying combustible gases containing carbon monoxide by washing with liquids; Reviving the used wash liquors
    • C10K1/10Purifying combustible gases containing carbon monoxide by washing with liquids; Reviving the used wash liquors with aqueous liquids
    • C10K1/12Purifying combustible gases containing carbon monoxide by washing with liquids; Reviving the used wash liquors with aqueous liquids alkaline-reacting including the revival of the used wash liquors
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00Technologies relating to chemical industry
    • Y02P20/10Process efficiency

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Combustion & Propulsion (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Analytical Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Industrial Gases (AREA)
  • Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
  • Physical Water Treatments (AREA)

Abstract

The invention relates to a process and a system for coupling heat of pressurized deacidification and ammonia distillation, wherein the system comprises a deacidification tower, an ammonia distillation tower, a pump, a condenser, a heat exchanger, a reboiler and a valve; the top of the deacidification tower is provided with an acid gas outlet, the upper part is provided with a mixed liquid inlet, the middle part is provided with a lean liquid side line outlet, the lower part is provided with an ammonia vapor inlet and a gas-liquid phase return port, and the bottom is provided with an ammonia water outlet; the top of the ammonia still is provided with an ammonia still gas outlet, the upper part is provided with an ammonia water inlet and a condensate inlet, the middle part is provided with an alkali liquor inlet, and the bottom is provided with a gas-liquid phase inlet and an ammonia still wastewater outlet; according to the invention, the rich liquid desorption pressure is ensured to realize the stepwise desorption to complete the recovery of ammonia products, and meanwhile, the top pressure of the ammonia distillation tower is further increased, so that the top temperature of the ammonia distillation tower is higher than the bottom temperature of the deacidification tower, the heat of the condenser at the top of the ammonia distillation tower is used for supplying heat to the bottom of the deacidification tower, and the purposes of energy conservation and emission reduction are achieved by performing heat coupling through a reasonable temperature system.

Description

Pressurized deacidification ammonia distillation heat coupling process and system
Technical Field
The invention relates to the technical field of coke oven gas purification, in particular to a pressurized deacidification ammonia distillation heat coupling process and a pressurized deacidification ammonia distillation heat coupling system.
Background
The ammonia water desulfurizing process is one common process for eliminating hydrogen sulfide from raw gas. The process takes ammonia in the gas as an alkali source, takes ammonia-containing aqueous solution as a washing medium, and adopts an ammonia-sulfur combined washing (absorption) process to remove hydrogen sulfide in the gas. The method comprises a washing device and a deacidification ammonia distillation device, which form a main process body for absorption and desorption, and the washing and stripping desorption devices for ammonia and hydrogen sulfide are tightly combined together. In the absorption unit, the deacidification ammonia distillation device returns deacidification lean solution with higher ammonia and stripping water to absorb ammonia and hydrogen sulfide in the raw gas to form rich solution containing ammonia and hydrogen sulfide, so as to achieve the purpose of removing the hydrogen sulfide in the raw gas. In the desorption unit, deacidified lean solution and stripping water (part of ammonia distillation wastewater) obtained by desorbing the rich solution through a deacidification ammonia distillation device are returned to the washing device for recycling.
Compared with other desulfurization processes, the ammonia desulfurization process has the advantages of short overall gas purification flow and low investment, and is capable of desulfurizing only by using water as a washing medium and using ammonia in gas as an alkali source in an absorption method without generating desulfurization waste liquid. However, in the prior art, the desorption unit (deacidification and ammonia distillation) desorbs ammonia gas and hydrogen sulfide together, and the desorbed gas is decomposed by ammonia and then is subjected to sulfur recovery. In this process, ammonia, which can be the final chemical product, is directly decomposed as an impurity, and cannot be effectively recovered. Meanwhile, the rich liquid desorption process has larger energy consumption and higher operation cost. Because the heat required by the tower bottom is large, heat is generally supplied by directly connecting steam to the tower bottom, which also causes the defect of large wastewater amount in the process.
The deacidification and ammonia distillation method matched with the ammonia water desulfurization process at present can adopt a pressurized deacidification and ammonia distillation process method for effectively recovering ammonia products and increasing lean liquid ammonia sulfur ratio. The ammonia product is recovered by improving the desorption pressure of the rich liquid and the desorption step by step, so that the lean liquid quality is improved and the desulfurization effect is improved. However, the technology still has the problems of high energy consumption, high operation cost and large wastewater amount.
Disclosure of Invention
The invention provides a pressurized deacidification ammonia distillation heat coupling process and a pressurized deacidification ammonia distillation heat coupling system, which can further improve the top pressure of an ammonia distillation tower while ensuring the desorption pressure of rich liquid to realize the completion of ammonia product recovery by fractional desorption, so that the top temperature of the ammonia distillation tower is higher than the bottom temperature of the deacidification tower, heat of a condenser at the top of the ammonia distillation tower is used for supplying heat to the bottom of the deacidification tower, and heat coupling is carried out through a reasonable temperature system, thereby achieving the purposes of energy conservation and emission reduction.
In order to achieve the above purpose, the invention is realized by adopting the following technical scheme:
a pressurized deacidification ammonia distillation heat coupling process comprises the following steps:
1) Mixing rich liquid from the desulfurizing tower with residual ammonia water, exchanging heat with lean liquid of the deacidification tower through a heat exchanger, and then entering the top of the deacidification tower; the top of the deacidification tower is pressurized to inhibit ammonia gas from escaping, so that the acid gas product at the top of the deacidification tower only contains a small amount of ammonia gas;
2) The acid gas escapes from the top of the deacidification tower, and the lean solution extracted from the side line of the deacidification tower exchanges heat with the rich solution of the desulfurization tower and the residual ammonia water and returns to the desulfurization tower for recycling;
3) The pressure at the top of the ammonia distillation column is greater than the pressure at the bottom of the deacidification column, after the pressure of the liquid phase at the bottom of the deacidification column is increased by a pump, one part of the liquid phase enters the top of the ammonia distillation column to carry out ammonia distillation treatment, and the other part of the liquid phase enters a condenser at the top of the ammonia distillation column to be heated, and the heated liquid phase returns to the bottom of the deacidification column;
4) Part of the ammonia gas evaporated from the top of the ammonia distillation tower escapes into a tower top condenser to be condensed and concentrated, and the other part of the ammonia gas is returned to the bottom of the deacidification tower through valve adjustment to be used as a heat source at the bottom of the deacidification tower;
5) Concentrating the ammonia gas evaporated from the top of the ammonia distillation tower through a condenser, allowing the gas phase to escape to form an ammonia product, and returning the liquid phase to the ammonia distillation tower as reflux;
6) And adding alkali liquor into the middle part of the ammonia distillation tower to remove fixed ammonia, providing heat at the bottom of the ammonia distillation tower through a reboiler, returning part of ammonia distillation wastewater discharged from the bottom of the ammonia distillation tower to the desulfurization section to be used as stripping water for desulfurizing and washing ammonia, and simultaneously supplying heat to the desulfurization tower.
A system for coupling heat of pressurizing deacidification and ammonia distillation comprises a deacidification tower, an ammonia distillation tower, a pump, a condenser, a heat exchanger, a reboiler and a valve; the top of the deacidification tower is provided with an acid gas outlet, the upper part is provided with a mixed liquid inlet, the middle part is provided with a lean liquid side line outlet, the lower part is provided with an ammonia vapor inlet and a gas-liquid phase return port, and the bottom is provided with an ammonia water outlet; the mixed liquor inlet is connected with a first heat exchange medium outlet of the heat exchanger, and the first heat exchange medium inlet of the heat exchanger is connected with a rich liquor conveying pipeline of the desulfurizing tower and a residual ammonia water conveying pipeline; the lean liquid side outlet of the deacidification tower is connected with the second heat exchange medium inlet of the heat exchanger, and the second heat exchange medium outlet of the heat exchanger is connected with a lean liquid conveying pipeline; the top of the ammonia still is provided with an ammonia still gas outlet, the upper part is provided with an ammonia water inlet and a condensate inlet, the middle part is provided with an alkali liquor inlet, and the bottom is provided with a gas-liquid phase inlet and an ammonia still wastewater outlet; the ammonia water outlet of the deacidification tower is connected with the inlet of the pump, the outlet of the pump is respectively connected with the ammonia water inlet of the ammonia distillation tower and the first heat exchange medium inlet of the condenser, and the first heat exchange medium outlet of the condenser is connected with the gas-liquid phase return port of the deacidification tower; the ammonia evaporation gas outlet of the ammonia evaporation tower is connected with the second heat exchange medium inlet of the condenser through one pipeline, is connected with the ammonia evaporation gas inlet of the deacidification tower through the other pipeline, and is provided with a valve on a pipeline connected with the ammonia evaporation gas inlet; the second heat exchange medium outlet of the condenser is connected with an ammonia product pipeline, and the condensate outlet of the condenser is connected with the condensate inlet of the ammonia distillation tower; the ammonia distillation wastewater outlet of the ammonia distillation tower is connected with an ammonia distillation wastewater pipeline, the ammonia distillation wastewater pipeline is connected with the inlet of a reboiler through a branch pipeline, the outlet of the reboiler is connected with the gas-liquid phase inlet of the ammonia distillation tower, and the ammonia distillation wastewater pipeline at the downstream of the branch pipeline is additionally connected with a stripping water conveying pipeline.
The deacidification tower is characterized in that a plurality of layers of packing or trays are respectively arranged in the 2-section tower body between the mixed liquor inlet and the lean liquor side line extraction outlet and between the lean liquor side line extraction outlet and the distilled gas inlet.
The ammonia still is characterized in that a plurality of layers of fillers or trays are respectively arranged in the 2-section tower body between the ammonia water inlet and the alkali liquor inlet and between the alkali liquor inlet and the gas-liquid phase inlet.
Compared with the prior art, the invention has the beneficial effects that:
1) The top temperature of the ammonia distillation tower is higher than the bottom temperature of the deacidification tower by increasing the top pressure of the ammonia distillation tower, and the ammonia distillation tower condenser is used for heating the desulfurizing tower as a reboiler of the desulfurizing tower while concentrating ammonia;
2) The steam consumption of the system is reduced in a heat coupling mode, and meanwhile, the required area of a reboiler at the bottom of the ammonia distillation tower is reduced; and the waste water discharge capacity is reduced by adopting a steam indirect heating mode.
Drawings
FIG. 1 is a flow chart of a process for pressurized deacidification and ammonia distillation heat coupling according to the present invention.
In the figure: 1. the deacidification tower 11, the acid gas discharge port 12, the mixed liquor inlet 13, the lean liquid side extraction port 14, the ammonia vapor gas inlet 15, the gas-liquid phase return port 16, the ammonia water discharge port 2, the ammonia vapor tower 21, the ammonia vapor gas outlet 22, the ammonia water inlet 23, the condensate inlet 24, the alkali liquor inlet 25, the gas-liquid phase inlet 26, the ammonia vapor waste water outlet 3, the heat exchanger 4, the pump 5, the condenser 6, the reboiler 7, the valve
Detailed Description
The following is a further description of embodiments of the invention, taken in conjunction with the accompanying drawings:
as shown in FIG. 1, the process for coupling heat of pressurizing deacidification and ammonia distillation comprises the following steps:
1) Mixing rich liquid from the desulfurizing tower with residual ammonia water, exchanging heat with lean liquid of the deacidification tower through a heat exchanger 3, and then entering the top of the deacidification tower 1; the top of the deacidification tower 1 is pressed to inhibit ammonia gas from escaping, so that the acid gas product at the top of the deacidification tower 1 only contains a small amount of ammonia gas;
2) The acid gas escapes from the top of the deacidification tower 1, and the lean solution extracted from the side line of the deacidification tower 1 exchanges heat with the rich solution of the desulfurization tower and the residual ammonia water and returns to the desulfurization tower for recycling;
3) The pressure at the top of the ammonia distillation tower 2 is greater than the pressure at the bottom of the deacidification tower 1, after the liquid phase at the bottom of the deacidification tower 1 is pressurized by a pump 4, one part of the liquid phase enters the top of the ammonia distillation tower 2 for ammonia distillation treatment, and the other part of the liquid phase enters a condenser 5 at the top of the ammonia distillation tower 2 for heating, and the heated gas-liquid phase returns to the bottom of the deacidification tower 1;
4) Part of the gas evaporated from the top of the ammonia distillation tower 2 enters a tower top condenser 5 for condensation and concentration treatment, and the other part of the gas is regulated by a valve 7 and returns to the bottom of the deacidification tower 1 to be used as a heat source at the bottom of the deacidification tower 1;
5) Concentrating the ammonia gas evaporated from the top of the ammonia distillation tower 2 through a condenser 5, allowing the gas phase to escape to form an ammonia product, and returning the liquid phase to the ammonia distillation tower 2 as reflux;
6) The middle part of the ammonia still 2 is added with alkali liquor for removing fixed ammonia, the bottom of the ammonia still 2 provides heat through a reboiler 6, and a part of ammonia still wastewater discharged from the bottom of the ammonia still 2 returns to the desulfurization section to be used as stripping water for desulfurizing and washing ammonia, and simultaneously, heat is supplied to the desulfurization tower.
A system for coupling heat of pressurizing deacidification and ammonia distillation comprises a deacidification tower 1, an ammonia distillation tower 2, a pump 4, a condenser 5, a heat exchanger 3, a reboiler 6 and a valve 7; the top of the deacidification tower 1 is provided with an acid gas outlet 11, the upper part is provided with a mixed liquid inlet 12, the middle part is provided with a lean liquid side line outlet 13, the lower part is provided with an ammonia gas inlet 14 and a gas-liquid phase return port 15, and the bottom is provided with an ammonia water outlet 16; the mixed liquor inlet 12 is connected with a first heat exchange medium outlet of the heat exchanger 3, and the first heat exchange medium inlet of the heat exchanger 3 is connected with a rich liquor conveying pipeline of the desulfurizing tower and a residual ammonia water conveying pipeline; the lean solution side outlet 13 of the deacidification tower 1 is connected with the second heat exchange medium inlet of the heat exchanger 3, and the second heat exchange medium outlet of the heat exchanger 3 is connected with a lean solution conveying pipeline; the top of the ammonia still 2 is provided with an ammonia still gas outlet 21, the upper part is provided with an ammonia water inlet 22 and a condensate inlet 23, the middle part is provided with an alkali liquor inlet 24, and the bottom is provided with a gas-liquid phase inlet 25 and an ammonia still wastewater outlet 26; the ammonia water outlet 16 of the deacidification tower 1 is connected with the inlet of the pump 4, the outlet of the pump 4 is respectively connected with the ammonia water inlet 22 of the ammonia distillation tower 2 and the first heat exchange medium inlet of the condenser 5, and the first heat exchange medium outlet of the condenser 5 is connected with the gas-liquid phase return port 15 of the deacidification tower 1; the ammonia vapor outlet 21 of the ammonia vapor tower 2 is connected with the second heat exchange medium inlet of the condenser 5 through one pipeline, is connected with the ammonia vapor inlet 14 of the deacidification tower 1 through the other pipeline, and is provided with a valve 7 on a pipeline connected with the ammonia vapor inlet 14; the second heat exchange medium outlet of the condenser 5 is connected with an ammonia product pipeline, and the condensate outlet of the condenser 5 is connected with the condensate inlet 23 of the ammonia distillation tower 2; the ammonia distillation wastewater outlet 26 of the ammonia distillation tower 2 is connected with an ammonia distillation wastewater pipeline, the ammonia distillation wastewater pipeline is connected with the inlet of the reboiler 6 through a branch pipeline, the outlet of the reboiler 6 is connected with the gas-liquid phase inlet 25 of the ammonia distillation tower 2, and the ammonia distillation wastewater pipeline downstream of the branch pipeline is additionally connected with a stripping water conveying pipeline.
The deacidification tower 1 is provided with a plurality of layers of packing or trays respectively in a 2-stage tower body positioned between the mixed liquor inlet 12 and the lean liquor side stream extraction outlet 13 and between the lean liquor side stream extraction outlet 13 and the ammonia vapor gas inlet 14.
The ammonia still 2 is provided with a plurality of layers of packing or trays in the 2-section tower body between the ammonia water inlet 22 and the alkali liquor inlet 24 and between the alkali liquor inlet 24 and the gas-liquid phase inlet 25 respectively.
The foregoing is only a preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art, who is within the scope of the present invention, should make equivalent substitutions or modifications according to the technical scheme of the present invention and the inventive concept thereof, and should be covered by the scope of the present invention.

Claims (4)

1. The process for coupling the heat of pressurizing deacidification and ammonia distillation is characterized by comprising the following steps of:
1) Mixing rich liquid from the desulfurizing tower with residual ammonia water, exchanging heat with lean liquid of the deacidification tower through a heat exchanger, and then entering the top of the deacidification tower; the top of the deacidification tower is pressurized to inhibit ammonia gas from escaping, so that the acid gas product at the top of the deacidification tower only contains a small amount of ammonia gas;
2) The acid gas escapes from the top of the deacidification tower, and the lean solution extracted from the side line of the deacidification tower exchanges heat with the rich solution of the desulfurization tower and the residual ammonia water and returns to the desulfurization tower for recycling;
3) The pressure at the top of the ammonia distillation column is greater than the pressure at the bottom of the deacidification column, after the pressure of the liquid phase at the bottom of the deacidification column is increased by a pump, one part of the liquid phase enters the top of the ammonia distillation column to carry out ammonia distillation treatment, and the other part of the liquid phase enters a condenser at the top of the ammonia distillation column to be heated, and the heated liquid phase returns to the bottom of the deacidification column;
4) Part of the ammonia gas evaporated from the top of the ammonia distillation tower escapes into a tower top condenser to be condensed and concentrated, and the other part of the ammonia gas is returned to the bottom of the deacidification tower through valve adjustment to be used as a heat source at the bottom of the deacidification tower;
5) Concentrating the ammonia gas evaporated from the top of the ammonia distillation tower through a condenser, allowing the gas phase to escape to form an ammonia product, and returning the liquid phase to the ammonia distillation tower as reflux;
6) And adding alkali liquor into the middle part of the ammonia distillation tower to remove fixed ammonia, providing heat at the bottom of the ammonia distillation tower through a reboiler, returning part of ammonia distillation wastewater discharged from the bottom of the ammonia distillation tower to the desulfurization section to be used as stripping water for desulfurizing and washing ammonia, and simultaneously supplying heat to the desulfurization tower.
2. The system is characterized by comprising a deacidification tower, an ammonia distillation tower, a pump, a condenser, a heat exchanger, a reboiler and a valve; the top of the deacidification tower is provided with an acid gas outlet, the upper part is provided with a mixed liquid inlet, the middle part is provided with a lean liquid side line outlet, the lower part is provided with an ammonia vapor inlet and a gas-liquid phase return port, and the bottom is provided with an ammonia water outlet; the mixed liquor inlet is connected with a first heat exchange medium outlet of the heat exchanger, and the first heat exchange medium inlet of the heat exchanger is connected with a rich liquor conveying pipeline of the desulfurizing tower and a residual ammonia water conveying pipeline; the lean liquid side outlet of the deacidification tower is connected with the second heat exchange medium inlet of the heat exchanger, and the second heat exchange medium outlet of the heat exchanger is connected with a lean liquid conveying pipeline; the top of the ammonia still is provided with an ammonia still gas outlet, the upper part is provided with an ammonia water inlet and a condensate inlet, the middle part is provided with an alkali liquor inlet, and the bottom is provided with a gas-liquid phase inlet and an ammonia still wastewater outlet; the ammonia water outlet of the deacidification tower is connected with the inlet of the pump, the outlet of the pump is respectively connected with the ammonia water inlet of the ammonia distillation tower and the first heat exchange medium inlet of the condenser, and the first heat exchange medium outlet of the condenser is connected with the gas-liquid phase return port of the deacidification tower; the ammonia evaporation gas outlet of the ammonia evaporation tower is connected with the second heat exchange medium inlet of the condenser through one pipeline, is connected with the ammonia evaporation gas inlet of the deacidification tower through the other pipeline, and is provided with a valve on a pipeline connected with the ammonia evaporation gas inlet; the second heat exchange medium outlet of the condenser is connected with an ammonia product pipeline, and the condensate outlet of the condenser is connected with the condensate inlet of the ammonia distillation tower; the ammonia distillation wastewater outlet of the ammonia distillation tower is connected with an ammonia distillation wastewater pipeline, the ammonia distillation wastewater pipeline is connected with the inlet of a reboiler through a branch pipeline, the outlet of the reboiler is connected with the gas-liquid phase inlet of the ammonia distillation tower, and the ammonia distillation wastewater pipeline at the downstream of the branch pipeline is additionally connected with a stripping water conveying pipeline.
3. The system for coupling heat for pressurizing, deacidifying and distilling ammonia according to claim 2, wherein the deacidification tower is provided with a plurality of layers of packing or trays respectively in the 2-stage tower body between the mixed liquor inlet and the lean liquor side offtake outlet and between the lean liquor side offtake outlet and the distilled ammonia gas inlet.
4. The system for coupling heat of pressurizing, deacidifying and distilling ammonia according to claim 2, wherein the ammonia distilling tower is provided with a plurality of layers of packing or trays respectively in the 2-section tower body between the ammonia water inlet and the alkali liquid inlet and between the alkali liquid inlet and the gas-liquid inlet.
CN201910109557.1A 2019-02-11 2019-02-11 Pressurized deacidification ammonia distillation heat coupling process and system Active CN109704366B (en)

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CN201910109557.1A CN109704366B (en) 2019-02-11 2019-02-11 Pressurized deacidification ammonia distillation heat coupling process and system
PCT/CN2020/070522 WO2020164341A1 (en) 2019-02-11 2020-01-06 Process and system for thermal coupling of pressurized deacidification and ammonia distillation

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CN113150837B (en) * 2021-04-23 2022-07-26 济南冶金化工设备有限公司 Coke oven gas desulfurization process
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CN115367943B (en) * 2022-08-22 2024-02-02 吴嘉 Energy-saving salt-containing heavy ammonia nitrogen-containing wastewater treatment system and process
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