CN111879062A - Normal-temperature feeding purification ammonia synthesis gas liquid nitrogen washing device with precooling function - Google Patents

Normal-temperature feeding purification ammonia synthesis gas liquid nitrogen washing device with precooling function Download PDF

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CN111879062A
CN111879062A CN202010627706.6A CN202010627706A CN111879062A CN 111879062 A CN111879062 A CN 111879062A CN 202010627706 A CN202010627706 A CN 202010627706A CN 111879062 A CN111879062 A CN 111879062A
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pipeline
flow channel
liquid nitrogen
ammonia
gas
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曲涛
周启勇
柯云龙
秦燕
梁维好
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Hangzhou Oxygen Plant Group Co Ltd
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Hangzhou Oxygen Plant Group Co Ltd
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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
    • F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
    • F25J3/0204—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream characterised by the feed stream
    • F25J3/0219—Refinery gas, cracking gas, coke oven gas, gaseous mixtures containing aliphatic unsaturated CnHm or gaseous mixtures of undefined nature
    • 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
    • F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
    • F25J3/0204—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream characterised by the feed stream
    • F25J3/0209—Natural gas or substitute natural gas
    • 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
    • F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
    • F25J3/0204—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream characterised by the feed stream
    • F25J3/0223—H2/CO mixtures, i.e. synthesis gas; Water gas or shifted synthesis gas
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
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    • 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
    • F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
    • F25J3/0228—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream characterised by the separated product stream
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    • F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
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    • F25J3/0252—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream characterised by the separated product stream separation of hydrogen
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    • 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
    • F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
    • F25J3/0228—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream characterised by the separated product stream
    • F25J3/0257—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream characterised by the separated product stream separation of nitrogen
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    • 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
    • F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
    • F25J3/0228—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream characterised by the separated product stream
    • F25J3/0276—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream characterised by the separated product stream separation of H2/N2 mixtures, i.e. of ammonia synthesis gas
    • 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
    • F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
    • F25J3/0295—Start-up or control of the process; Details of the apparatus used, e.g. sieve plates, packings
    • 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
    • F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/08—Separating gaseous impurities from gases or gaseous mixtures or from liquefied gases or liquefied gaseous mixtures
    • 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
    • F25J2200/00—Processes or apparatus using separation by rectification
    • F25J2200/02—Processes or apparatus using separation by rectification in a single pressure main column system
    • 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
    • F25J2205/00—Processes or apparatus using other separation and/or other processing means
    • F25J2205/02—Processes or apparatus using other separation and/or other processing means using simple phase separation in a vessel or drum
    • 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
    • F25J2205/00—Processes or apparatus using other separation and/or other processing means
    • F25J2205/30—Processes or apparatus using other separation and/or other processing means using a washing, e.g. "scrubbing" or bubble column for purification purposes
    • 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
    • F25J2210/00—Processes characterised by the type or other details of the feed stream
    • F25J2210/12—Refinery or petrochemical off-gas
    • 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
    • F25J2210/00—Processes characterised by the type or other details of the feed stream
    • F25J2210/42—Nitrogen
    • 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
    • F25J2215/00—Processes characterised by the type or other details of the product stream
    • F25J2215/02—Mixing or blending of fluids to yield a certain product
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    • 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
    • F25J2245/00—Processes or apparatus involving steps for recycling of process streams
    • F25J2245/42—Processes or apparatus involving steps for recycling of process streams the recycled stream being nitrogen
    • 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
    • F25J2270/00—Refrigeration techniques used
    • F25J2270/90—External refrigeration, e.g. conventional closed-loop mechanical refrigeration unit using Freon or NH3, unspecified external refrigeration

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  • Separation By Low-Temperature Treatments (AREA)

Abstract

A normal-temperature feeding purified ammonia synthesis gas liquid nitrogen washing device with precooling comprises a molecular sieve adsorption unit I, an ammonia precooling unit II and a liquid nitrogen washing and cooling box unit III, wherein the molecular sieve adsorption unit I is connected with coal-made synthesis gas from the upstream through a pipeline, a novel molecular sieve is filled in the molecular sieve adsorption unit I to adsorb components which are easy to solidify at low temperature such as carbon dioxide, methanol, water and the like in mixed gas, and the device reduces investment cost; the defect of insufficient cold quantity of the process is avoided by a mode of precooling high-pressure nitrogen by ammonia, the device is prevented from supplementing liquid nitrogen, and the laying of a liquid nitrogen vacuum pipeline is reduced; the hydrogen-nitrogen ratio of the ammonia synthesis gas obtained by separating the liquid nitrogen washing cold box is 3:1, wherein the contents of CO and CH4 are less than 1ppm, 3 heat exchangers in the cold box of the conventional liquid nitrogen washing device are combined into 2 heat exchangers, the complexity of piping in the cold box is reduced, the pressure loss of the process gas in the device is reduced, and the energy consumption is reduced.

Description

Normal-temperature feeding purification ammonia synthesis gas liquid nitrogen washing device with precooling function
Technical Field
The invention designs a cryogenic separation device and a cryogenic separation method for purifying normal-temperature synthesis gas from upstream and matching the normal-temperature synthesis gas with nitrogen to produce synthesis gas with a hydrogen-nitrogen ratio of 3:1 and providing feed gas for a downstream ammonia synthesis device, and belongs to the field of low-temperature gas separation.
Background
Ammonia has wide application, is one of the most productive inorganic compounds in the world, can be used as a refrigerant, and is widely applied to industries such as nitrogen fertilizers, nitric acid, ammonium salts, soda ash and the like as a basic chemical raw material.
The raw materials of the synthetic ammonia comprise natural gas, naphtha, heavy oil, coal and the like, and the coal is mainly used as the raw material in the current Chinese synthetic ammonia. The ammonia synthesis gas is not converted by gasification, transformation, purification, compression and other devices, and raw material gas is provided for an ammonia synthesis device.
At present, the synthesis ammonia purification process basically adopts a mode of low-temperature methanol washing and liquid nitrogen washing to produce qualified ammonia synthesis gas, wherein a liquid nitrogen washing device adopts a mode of low-temperature liquid nitrogen washing raw material gas from upstream to remove harmful impurities such as CO, Ar, CH4 and the like. The raw material gas of the conventional liquid nitrogen washing process is from low-temperature methanol washing basically in a low-temperature form, and meanwhile, the liquid nitrogen is used for washing ammonia synthesis gas with basically equal temperature and equal cold quantity in the low-temperature methanol washing so as to keep the cold quantity balance of the low-temperature methanol washing and the ammonia synthesis gas.
The liquid nitrogen washing synthesis gas device provided by the invention adopts a front-end ammonia pre-cooling high-pressure nitrogen mode to make up for the situation of insufficient cold energy of a liquid nitrogen washing device aiming at the working condition that the raw material gas from the upstream is at normal temperature, and brings a new process selection route for old plant transformation and peak regulation device construction.
Disclosure of Invention
The invention aims to: a cryogenic separation device and a cryogenic separation method for purifying and mixing nitrogen with normal-temperature coal synthesis gas from upstream to produce synthesis gas with a hydrogen-nitrogen ratio of 3:1 and providing feed gas for a downstream ammonia synthesis device. The raw material gas enters a liquid nitrogen washing boundary area at normal temperature, and equipment, pipelines, switching valves and the like of the molecular sieve part can be made of carbon steel, so that the investment cost of the device is reduced; the defect of insufficient cold quantity of the process is avoided by a mode of precooling high-pressure nitrogen by ammonia, the device is prevented from supplementing liquid nitrogen, and the laying of a liquid nitrogen vacuum pipeline is reduced; the hydrogen-nitrogen ratio of the ammonia synthesis gas obtained by separating the liquid nitrogen washing cold box is 3:1, wherein the contents of CO and CH4 are less than 1ppm, 3 heat exchangers in the cold box of the conventional liquid nitrogen washing device are combined into 2 heat exchangers, the complexity of piping in the cold box is reduced, the pressure loss of the process gas in the device is reduced, and the energy consumption is reduced.
In order to achieve the purpose, the invention adopts the following technical scheme:
a normal-temperature feeding purified ammonia synthesis gas liquid nitrogen washing device with precooling comprises a molecular sieve adsorption unit I, an ammonia precooling unit II and a liquid nitrogen washing and cooling box unit III, wherein the molecular sieve adsorption unit I is connected with coal-made synthesis gas from the upstream through a pipeline, a molecular sieve is filled in the molecular sieve adsorption unit I to adsorb carbon dioxide, methanol, water and other components which are easy to solidify at low temperature in mixed gas, so that the substances are prevented from freezing pipelines and equipment, and purified gas is connected with an inlet pipeline of the liquid nitrogen washing and cooling box unit III and introduced into a cooling box III of a cryogenic separation device; the ammonia pre-cooling unit II is connected with high-pressure nitrogen gas obtained by air separation from the upstream through a pipeline, the high-pressure nitrogen gas is pre-cooled to a certain temperature in a liquid ammonia evaporation mode, the pre-cooled high-pressure nitrogen gas is connected with an inlet pipeline of the liquid nitrogen cold washing box unit III, and the liquid nitrogen cold washing box unit III is introduced.
Preferably, the molecular sieve adsorption unit I comprises: the device comprises a molecular sieve adsorber, a regenerated gas heater and a regenerated gas cooler; the molecular sieve adsorber, the regeneration gas heater and the regeneration gas cooler are connected through pipelines, all equipment, pipelines and valves are made of carbon steel, feed gas from the upstream enters a molecular sieve adsorption unit I through the pipelines, and after CO2, methanol and water are adsorbed and removed, the feed gas is discharged out of the molecular sieve adsorption unit I through the pipelines and enters a liquid nitrogen washing cold box unit III;
preferably, the ammonia pre-cooling unit II comprises: an ammonia precooler; liquid ammonia from the ammonia refrigeration unit enters an ammonia precooling unit II through a pipeline, is evaporated and then is discharged out of the ammonia precooling unit II through a pipeline and is sent to an ammonia recovery system; high-pressure nitrogen from air separation enters an ammonia precooling unit II through a pipeline, is discharged out of the ammonia precooling unit II through a pipeline after precooling, and enters a liquid nitrogen washing cold box unit III;
preferably, the liquid nitrogen cold washing box unit III integrally comprises: the system comprises a first main heat exchanger, a second main heat exchanger, a nitrogen scrubber, a hydrogen separator and a gas mixture; the first main heat exchanger is provided with 5 flow channels 1a,1b,1c,1d and 1e, and the second main heat exchanger is provided with 5 flow channels 2a,2b,2c,2d and 2 e.
Preferably, the liquid nitrogen washing cold box unit III receives the feed gas from the molecular sieve adsorption unit I, is communicated with a flow channel 1A of a first main heat exchanger E4 through a pipeline, is cooled in the flow channel 1A, is communicated with a flow channel 2A of a second main heat exchanger through a pipeline, and enters the lower part of the nitrogen washing tower through a pipeline after being cooled in the flow channel 2A.
Preferably, the liquid nitrogen washing cold box unit III receives high-pressure nitrogen from the ammonia pre-cooling unit II, is communicated with a flow channel 1B of the first main heat exchanger through a pipeline, is cooled in the flow channel 1B and then flows out of the first main heat exchanger through the pipeline, and then is divided into two pipelines, wherein one pipeline enters the gas mixer for coarse nitrogen distribution, the other pipeline is communicated with a flow channel 2B of the second main heat exchanger, and after being cooled in the flow channel 2B, the two pipelines enter the upper part of the nitrogen washing tower through the pipeline.
Preferably, the top of the nitrogen washing tower of the liquid nitrogen washing cold box unit III is communicated with a 2D flow channel of the second main heat exchanger through a pipeline, enters a gas mixer through the pipeline after being reheated in the flow channel 2D, is communicated with a 1D flow channel of the first main heat exchanger through the pipeline, and is discharged out of a boundary area through the pipeline after being reheated to normal temperature in the flow channel 1D.
Preferably, a tower kettle of a nitrogen washing tower of the liquid nitrogen washing cold box unit III is communicated with a hydrogen separator through a pipeline, gas and liquid are separated in the hydrogen separator, the top of the hydrogen separator is communicated with a flow channel of the second main heat exchanger through a pipeline, the flow channel is communicated with a 1E flow channel of the first main heat exchanger through a pipeline after reheating in the flow channel, and the flow channel is out of the boundary area through a pipeline after reheating to the normal temperature; the bottom of the hydrogen separator is communicated with a flow channel 2C of the second main heat exchanger through a pipeline, the bottom of the hydrogen separator is communicated with a flow channel 1C of the first main heat exchanger through a pipeline after reheating in the flow channel 2C, and the bottom of the hydrogen separator is communicated with a boundary area through a pipeline after reheating to normal temperature in the flow channel 1C.
The invention has the positive effects that: the raw material gas in the molecular sieve adsorption unit I is at normal temperature, the operating conditions of the molecular sieve adsorption unit I become mild, laying of low-temperature pipelines is reduced, all equipment, pipelines (including pipe fittings), valves and the like can be made of carbon steel, and investment cost of the device is reduced.
The invention has the positive effects that: according to the liquid nitrogen washing cold box unit III, the raw material gas enters the plate-fin heat exchanger in the liquid nitrogen washing cold box unit III at normal temperature, the risk that the heat exchanger is damaged due to the fact that the temperature difference of the end face of the plate-fin heat exchanger is too large in the operation process (particularly in the driving process) is reduced, meanwhile, compared with a liquid nitrogen washing device cold box of a conventional low-temperature raw material gas, 3 plate-fin heat exchangers in the heat exchanger are combined into 2 plate-fin heat exchangers, the complexity of piping in the cold box is reduced, the pressure loss of process gas in equipment is reduced, and the energy consumption is indirectly reduced.
The invention has the positive effects that: according to the liquid nitrogen cold washing box unit III, when the feed gas enters the liquid nitrogen cold washing box unit III at normal temperature, the cold energy of the device is insufficient, and a certain amount of liquid nitrogen (-about 180 ℃) is normally led to the cold box from air separation through the vacuum pipeline to supplement the cold energy.
Drawings
Fig. 1 is a schematic structural view of the present invention.
Detailed Description
The invention will be described in detail below with reference to the following figures: as shown in fig. 1, the ammonia synthesis gas liquid nitrogen washing device for purifying normal temperature feeding of the present invention can purify normal temperature coal from upstream to produce synthesis gas, produce ammonia synthesis gas with 3:1 hydrogen-nitrogen ratio and CO content lower than 1ppm, and provide feed gas for the downstream ammonia synthesis device, the device includes three parts of a molecular sieve adsorption unit i, an ammonia precooling unit ii, and a liquid nitrogen washing cold box unit iii, the molecular sieve adsorption unit i is connected with the coal synthesis gas from upstream through a pipeline, the molecular sieve adsorption unit includes: molecular sieve adsorber S1, regeneration gas heater E1, E2 regeneration gas cooler; the molecular sieve adsorber S1, the regeneration gas heater E1 and the regeneration gas cooler E2 are mainly used for adsorbing easily-solidified components such as carbon dioxide, methanol, water and the like in the mixed gas at low temperature and preventing the substances from freezing pipelines and equipment; the ammonia precooling unit II is integrated with: the ammonia precooler E3 is mainly used for precooling high-pressure nitrogen gas obtained by air separation by utilizing liquid ammonia evaporation; the liquid nitrogen washing and cooling box unit III is integrated and comprises: the first main heat exchanger E4 is provided with 5 channels of 1a,1b,1c,1D and 1E, the second main heat exchanger E5 is provided with 5 channels of 2a,2b,2c,2D and 2E, the nitrogen scrubber T1, the hydrogen separator D1 and the mixed gas M1, and the main functions of purifying the CO content in the raw material gas to be less than 1ppm and simultaneously carrying out nitrogen distribution on the purified synthesis gas are realized.
Raw material gas containing H2 more than or equal to 90% from an upstream device enters a molecular sieve adsorption unit I through a pipeline 01, after CO2, methanol and water are adsorbed and removed, the raw material gas is discharged out of the molecular sieve adsorption unit I through a pipeline 02 and enters a liquid nitrogen washing and cooling box unit III.
Liquid ammonia from the ammonia refrigeration unit enters an ammonia precooling unit II through a pipeline 03, is evaporated and then is discharged out of the ammonia precooling unit II through a pipeline 04 and is sent to an ammonia recovery system; high-pressure nitrogen from air separation enters an ammonia pre-cooling unit II through a pipeline 05, is discharged out of the ammonia pre-cooling unit II through a pipeline 06 after pre-cooling, and enters a liquid nitrogen washing cold box unit III.
The raw material gas from the molecular sieve adsorption unit I is communicated with a flow channel 1A of a first main heat exchanger E4 through a pipeline 02, is cooled in the flow channel 1A and then communicated with a flow channel 2A of a second main heat exchanger E5 through a pipeline 07, and enters the lower part of a nitrogen washing tower T1 through a pipeline 08 after being cooled in the flow channel 2A; high-pressure nitrogen from the ammonia pre-cooling unit II is communicated with a flow channel 1B of a first main heat exchanger E4 through a pipeline 06, is cooled in the flow channel 1B and then flows out of an E4 through a pipeline 13, and then is divided into two pipelines 14 and 15, wherein one pipeline 14 enters a gas mixer M1, the other pipeline 15 is communicated with a flow channel 2B of a second main heat exchanger E5, and after being cooled in the flow channel 2B, the high-pressure nitrogen enters the upper part of a nitrogen washing tower T1 through a pipeline 16.
The top of the nitrogen scrubber T1 is communicated with a 2D flow channel of a second main heat exchanger E5 through a pipeline 09, enters a gas mixer M1 through a pipeline 10 after being reheated in the flow channel 2D, is communicated with a 1D flow channel of a first main heat exchanger E4 through a pipeline 11, and is discharged out of a boundary area through a pipeline 12 after being reheated to normal temperature in the flow channel 1D; the nitrogen scrubber T1 has a tower kettle communicated with a hydrogen separator D1 through a pipeline 17, and gas-liquid separation is carried out in the hydrogen separator D1, wherein the top of the hydrogen separator D1 is communicated with a flow channel 2E of a second main heat exchanger E5 through a pipeline 18, the top of the flow channel 2E is communicated with a flow channel 1E of a first main heat exchanger E4 through a pipeline 19 after reheating is carried out in the flow channel 2E, and the top of the flow channel 19 is discharged from a boundary area through a pipeline 20 after reheating is carried out to normal temperature; the bottom of the hydrogen separator D1 is communicated with the flow channel 2C of the second main heat exchanger E5 through a pipeline 21, is communicated with the flow channel 1C of the first main heat exchanger E4 through a pipeline 22 after reheating in the flow channel 2C, and is discharged out of the boundary area through a pipeline 23 after reheating to the normal temperature in the flow channel 1C.
The above examples are specific embodiments of the present invention. The liquid nitrogen washing device with precooling and normal-temperature feeding for purifying ammonia synthesis gas and the method can be combined or changed in a plurality of ways, and all belong to the protection scope of the invention.

Claims (8)

1. A normal-temperature feeding purified ammonia synthesis gas liquid nitrogen washing device with precooling comprises a molecular sieve adsorption unit I, an ammonia precooling unit II and a liquid nitrogen washing and cooling box unit III, and is characterized in that the molecular sieve adsorption unit I is connected with coal-made synthesis gas from the upstream through a pipeline, a molecular sieve is filled in the molecular sieve adsorption unit I to adsorb carbon dioxide, methanol, water and other components which are easy to solidify at low temperature in mixed gas, the substances are prevented from freezing pipelines and equipment, purified gas is connected with an inlet pipeline of the liquid nitrogen washing and cooling box unit III, and a cold box III of a cryogenic separation device is introduced; the ammonia pre-cooling unit II is connected with high-pressure nitrogen gas obtained by air separation from the upstream through a pipeline, the high-pressure nitrogen gas is pre-cooled to a certain temperature in a liquid ammonia evaporation mode, the pre-cooled high-pressure nitrogen gas is connected with an inlet pipeline of the liquid nitrogen cold washing box unit III, and the liquid nitrogen cold washing box unit III is introduced.
2. The liquid nitrogen washing device with precooling for normal-temperature feeding purified ammonia synthesis gas according to claim 1, wherein the molecular sieve adsorption unit I integrally comprises: a molecular sieve adsorber (S1), a regeneration gas heater (E1), a regeneration gas cooler (E2); the molecular sieve adsorber (S1), the regenerated gas heater (E1) and the regenerated gas cooler (E2) are connected through pipelines, all equipment, pipelines and valves are made of carbon steel, feed gas from upstream enters the molecular sieve adsorption unit (I) through the pipeline (01), and after CO2, methanol and water are adsorbed and removed, the feed gas exits the molecular sieve adsorption unit (I) through the pipeline (02) and enters the liquid nitrogen washing and cooling box unit III.
3. The liquid nitrogen wash apparatus with precooling and normal-temperature feed purification of ammonia synthesis gas as claimed in claim 1, wherein the ammonia precooling unit II is integrated with: an ammonia precooler (E3); liquid ammonia from the ammonia refrigeration unit enters an ammonia precooling unit (II) through a pipeline (03), is evaporated and then is discharged out of the ammonia precooling unit (II) through a pipeline (04) and is sent to an ammonia recovery system; high-pressure nitrogen from air separation enters an ammonia precooling unit (II) through a pipeline (05), is discharged out of the ammonia precooling unit (II) through a pipeline (06) after precooling, and enters a liquid nitrogen washing cold box unit (III).
4. The apparatus for liquid nitrogen scrubbing of ammonia synthesis gas with precooling, normal-temperature feed purification as claimed in claim 1, 2 or 3, wherein the liquid nitrogen scrubbing cold box unit III integrally comprises: the system comprises a first main heat exchanger (E4), a second main heat exchanger (E5), a nitrogen scrubber (T1), a hydrogen separator (D1) and a gas mixture (M1); the first main heat exchanger (E4) has 5 flow paths (1 a,1b,1c,1d, 1E), and the second main heat exchanger (E5) has 5 flow paths (2 a,2b,2c,2d, 2E).
5. The device for washing the ammonia synthesis gas with precooling and purified at normal temperature according to claim 4, wherein the liquid nitrogen washing and cooling box unit III receives the raw material gas from the molecular sieve adsorption unit I, is communicated with the flow channel (1A) of the first main heat exchanger (E4) through a pipeline (02), is communicated with the flow channel (2A) of the second main heat exchanger (E5) through a pipeline (07) after being cooled in the flow channel (1A), and enters the lower part of the nitrogen washing tower (T1) through a pipeline (08) after being cooled in the flow channel (2A).
6. The device for washing ammonia synthesis gas with precooling and normal-temperature feeding purification of the ammonia synthesis gas as claimed in claim 5, wherein the liquid nitrogen washing cold box unit (III) receives the high-pressure nitrogen gas from the ammonia precooling unit (II), is communicated with the flow channel (1B) of the first main heat exchanger (E4) through a pipeline (06), and is cooled in the flow channel (1B) and then is discharged out of the first main heat exchanger (E4) through a pipeline (13), and then is divided into two pipelines (14) and (15), one pipeline (14) enters the gas mixer M1 for crude nitrogen distribution, the other pipeline (15) is communicated with the flow channel (2B) of the second main heat exchanger (E5), and after being cooled in the flow channel (2B), the cooled high-pressure nitrogen gas enters the upper part of the nitrogen washing tower (T1) through a pipeline (16).
7. The device for washing ammonia synthesis gas with precooling and normal-temperature feeding purification of claim 6, wherein the top of the nitrogen washing tower (T1) of the liquid nitrogen washing and cooling box unit III is communicated with the flow channel (2D) of the second main heat exchanger (E5) through a pipeline (09), enters the gas mixer (M1) through a pipeline (10) after being reheated in the flow channel (2D), is communicated with the flow channel (1D) of the first main heat exchanger (E4) through a pipeline (11), and exits the boundary area through a pipeline (12) after being reheated to normal temperature in the flow channel (1D).
8. The liquid nitrogen washing device with precooling normal-temperature feeding purified ammonia synthesis gas as claimed in claim 7, characterized in that the bottom of the nitrogen washing tower (T1) of the liquid nitrogen washing cold box unit III is communicated with a hydrogen separator (D1) through a pipeline (17), gas and liquid are separated in the hydrogen separator (D1), wherein the top of the hydrogen separator (D1) is communicated with a flow channel (2E) of the second main heat exchanger (E5) through a pipeline (18), the flow channel (2E) is communicated with a flow channel (1E) of the first main heat exchanger (E4) through a pipeline (19) after reheating in the flow channel (2E), and the flow channel (19) is discharged out of a boundary area through a pipeline (20) after reheating to normal temperature; the bottom of the hydrogen separator (D1) is communicated with the flow channel (2C) of the second main heat exchanger (E5) through a pipeline (21), the heat is reheated in the flow channel (2C), then the heat is communicated with the flow channel (1C) of the first main heat exchanger (E4) through a pipeline (22), and the heat is reheated in the flow channel (1C) to the normal temperature and then the heat is discharged out of the boundary area through a pipeline (23).
CN202010627706.6A 2020-07-02 2020-07-02 Normal-temperature feeding purification ammonia synthesis gas liquid nitrogen washing device with precooling function Pending CN111879062A (en)

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