CN211120267U - Device for the cryogenic separation of a multi-component synthesis gas comprising CO/CH4/N2/H2 - Google Patents

Device for the cryogenic separation of a multi-component synthesis gas comprising CO/CH4/N2/H2 Download PDF

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Publication number
CN211120267U
CN211120267U CN201921786845.2U CN201921786845U CN211120267U CN 211120267 U CN211120267 U CN 211120267U CN 201921786845 U CN201921786845 U CN 201921786845U CN 211120267 U CN211120267 U CN 211120267U
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gas
unit
separation
demethanizer
methanol
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刘万洲
杨保江
姜广雨
韩斌
刘学武
宋林军
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Liaoning Datang Power Fuxin Coal To Gas Co ltd
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Liaoning Datang Power Fuxin Coal To Gas 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
    • F25J3/0223—H2/CO mixtures, i.e. synthesis gas; Water gas or shifted synthesis gas
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
    • C01B3/50—Separation of hydrogen or hydrogen containing gases from gaseous mixtures, e.g. purification
    • C01B3/506—Separation of hydrogen or hydrogen containing gases from gaseous mixtures, e.g. purification at low temperatures
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00—Carbon; Compounds thereof
    • C01B32/40—Carbon monoxide
    • 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
    • F25J3/0228—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
    • F25J3/0233—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 CnHm with 1 carbon atom or more
    • 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
    • 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
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
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    • 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
    • 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
    • F25J3/0228—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
    • F25J3/0261—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 carbon monoxide
    • 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
    • F25J2200/00—Processes or apparatus using separation by rectification
    • F25J2200/40—Features relating to the provision of boil-up in the bottom of a column
    • 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
    • F25J2200/74—Refluxing the column with at least a part of the partially condensed overhead 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
    • F25J2220/00—Processes or apparatus involving steps for the removal of impurities
    • F25J2220/02—Separating impurities in general from the feed stream
    • 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
    • F25J2230/00—Processes or apparatus involving steps for increasing the pressure of gaseous process streams
    • F25J2230/32—Compression of the product stream
    • 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
    • F25J2230/00—Processes or apparatus involving steps for increasing the pressure of gaseous process streams
    • F25J2230/42—Processes or apparatus involving steps for increasing the pressure of gaseous process streams the fluid 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
    • F25J2230/00—Processes or apparatus involving steps for increasing the pressure of gaseous process streams
    • F25J2230/60—Processes or apparatus involving steps for increasing the pressure of gaseous process streams the fluid being hydrocarbons or a mixture of hydrocarbons
    • 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
    • F25J2250/00—Details related to the use of reboiler-condensers
    • F25J2250/02—Bath type boiler-condenser using thermo-siphon effect, e.g. with natural or forced circulation or pool boiling, i.e. core-in-kettle heat exchanger
    • 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
    • F25J2270/12—External refrigeration with liquid vaporising loop
    • 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
    • F25J2270/42—Quasi-closed internal or closed external nitrogen refrigeration cycle
    • 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
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00—Technologies relating to chemical industry
    • Y02P20/151—Reduction of greenhouse gas [GHG] emissions, e.g. CO2

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  • Combustion & Propulsion (AREA)
  • Separation By Low-Temperature Treatments (AREA)
  • Separation Of Gases By Adsorption (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

The utility model provides a cryogenic separation contains CO/CH4/N2/H2The multi-component synthesis gas plant of (a), comprising: the device comprises a molecular sieve adsorption unit, a heat exchange unit, a demethanization pre-separation unit, a stripping unit, a demethanization unit and a denitrification unit; the molecular sieve adsorption unit is used for removing methanol and carbon dioxide in raw material gas from the low-temperature methanol washing device to obtain raw material gas from which the methanol and the carbon dioxide are removed; the heat exchange unit is used for cooling the raw material gas subjected to methanol and carbon dioxide removal; the demethanization pre-separation unit is used for separating the gas cooled by the heat exchange unit into hydrogen-rich gas and CO/CH4/N2/H2A liquid; the stripping unit is used for removing CO/CH from the demethanizing pre-separation unit4/N2/H2Separation of liquid into hydrogen flash gas and CO/CH4/N2A liquid; the utility model provides a multicomponent synthetic gas cryrogenic separator energy consumption is low, the security is high.

Description

For cryogenic separation of CO/CH-containing gas4/N2/H2Of a multi-component synthesis gas
Technical Field
The utility model belongs to the chemical industry field. In particular, the present invention relates to a cryogenic separation plant for containing CO/CH4/N2/H2The multi-component synthesis gas plant of (1).
Background
After the economic crisis of the world in the 70 s of the 20 th century, a new coal gasification technology has been developed rapidly, coal gasification research is widely carried out in countries of the world, a batch of novel gasification technologies appears, and so far, less than one hundred kinds of coal gasification technologies are developed or are in research and development. There are many classification methods for coal gasification technology, and there are the following: classification by gas use, classification by gas cause and chinese white index, classification by gasifying agent, classification by heat supply, classification by chemical engineering characteristics of production equipment, classification by operating pressure, classification by residue discharge type, and the like.
Raw gas generated by a gasification device of a first-stage production device of a company is transformed, cooled, washed by low-temperature methanol and recycled by sulfur, then is sent to a methanation device to synthesize methane, and is compressed by a natural gas compressor and then is sent to a natural gas pipe network. The peak regulation project cryogenic separation device utilizes the purified gas sent out by the low-temperature methanol washing device, adopts a cryogenic separation method to carry out deep cooling separation and extract CH4Gas and raw material CO gas for synthesizing ethylene glycol, and simultaneously obtaining hydrogen-rich gas and flash evaporation gas which meet the requirements. CH (CH)4The gas is directly used as a product and is merged into a natural gas pipe network, CO is sent to an ethylene glycol device to be used as raw material gas, one part of hydrogen-rich gas is sent to a PSA unit to be purified to be used as raw material hydrogen for synthesizing ethylene glycol, redundant hydrogen-rich gas and flash evaporation gas are sent to a methanol synthesis device, and nitrogen-containing tail gas is sent to a fuel gas pipe network.
At present, most coal chemical engineering projects adopt a fluidized bed or entrained flow bed technology, the content of methane in the generated crude gas is ppm level, a corresponding matched cryogenic separation device only needs to separate hydrogen-rich gas and CO, most of refrigeration modes in a cold box are CO washing or liquid nitrogen washing, and the process is mature. However, the company gasification device adopts the lurgi crushed coal pressure gasification technology, the reaction temperature is low, the crude gas contains a large amount of methane, and how to separate hydrogen, methane, CO and nitrogen rich gas through the cryogenic separation device and prevent the methane from freezing and blocking in the cold box to become a key problem which restricts the cryogenic separation device of the peak regulation project.
SUMMERY OF THE UTILITY MODEL
The utility model aims at separating four key components in the raw material gas from the outlet of the low-temperature methanol washing device.
In the context of the present invention, pressure is understood to mean gauge pressure unless otherwise specified.
In the present invention, the term "low-temperature methanol washing unit" is generally used to remove acid gases such as CO from raw gas at a temperature of-30 ℃ to-70 ℃2、H2And S.
In the context of the present invention the symbol "/" indicates that substances before and after the symbol are CO-present, such as "CO/CH4/N2/H2"denotes CO, CH4、N2And H2Simultaneously exist.
The above object of the present invention is achieved by the following technical solutions.
In one aspect, the present invention provides a cryogenic separation system for containing CO/CH4/N2/H2The multi-component synthesis gas plant of (a), comprising:
the device comprises a molecular sieve adsorption unit, a heat exchange unit, a demethanization pre-separation unit, a stripping unit, a demethanization unit and a denitrification unit; wherein,
the molecular sieve adsorption unit is used for removing methanol and carbon dioxide in the raw material gas from the low-temperature methanol washing device to obtain raw material gas from which the methanol and the carbon dioxide are removed;
the heat exchange unit is used for cooling the raw material gas subjected to methanol and carbon dioxide removal to obtain a gas cooled by the heat exchange unit;
the demethanization pre-separation unit is used for separating the gas cooled by the heat exchange unit into hydrogen-rich gas and CO/CH4/N2/H2A liquid;
the stripping unit is used for removing CO/CH from the demethanizing pre-separation unit4/N2/H2Separation of liquid into hydrogen flash gas and CO/CH4/N2A liquid;
the demethanization unit is used to convert CO/CH from the stripping unit4/N2Separation of liquids into CO/N2Gas and CH4A liquid;
the denitrification unit is used for removing CO/N from the demethanization unit2Separation of gas into N2Gas and CO liquid.
Preferably, in the device of the present invention, the molecular sieve adsorption unit comprises a regeneration gas heater, a regeneration gas cooler and at least two molecular sieve adsorbers connected in parallel; the molecular sieve adsorber is configured to be at least one molecular sieve adsorber for adsorption and at least one molecular sieve adsorber for regeneration.
Preferably, in the plant of the present invention, the demethanizer unit comprises a demethanizer, a demethanizer bottom reboiler and a demethanizer overhead condenser; the stripping unit comprises a stripping tower and a stripping tower bottom reboiler; the demethanizing pre-separation unit comprises a demethanizing pre-separation tower and a demethanizing pre-separation tower top condenser; the denitrification unit comprises a denitrification tower and a denitrification tower top condenser.
Preferably, in the device of the present invention, the heat exchange unit includes a first main heat exchanger and a second main heat exchanger connected in series;
preferably, the first main heat exchanger and the second main heat exchanger are plate-fin heat exchangers;
preferably, the pipeline used for conveying the raw material gas for removing methanol and carbon dioxide passes through the first main heat exchanger, the demethanizer bottom reboiler and the second main heat exchanger in sequence.
Preferably, in the device of the present invention, the device further comprises a methane compressor for compressing CH of the demethanization unit4。
Preferably, the device of the present invention further comprises a nitrogen compressor; the nitrogen compressor is used for providing cold for the demethanizer pre-separation tower top condenser, the demethanizer tower top condenser, the denitrogenation tower top condenser and the heat exchange unit, and the nitrogen can circulate in a reciprocating manner.
Preferably, in the device of the utility model, the demethanizer pre-separation tower, the denitrogenation tower and the demethanizer are packed towers, and the stripping tower is a packed tower and a float valve tower which are designed in a segmented mode.
On the other hand, the utility model also provides a method for cryogenic separation contains CO/CH4/N2/H2The method for multi-component synthesis gas, which uses the device of the utility model, comprises the following steps:
(1) removing methanol and carbon dioxide in the raw material gas from the low-temperature methanol washing device through a molecular sieve adsorption unit to obtain raw material gas from which the methanol and the carbon dioxide are removed;
(2) cooling the raw material gas without methanol and carbon dioxide by a heat exchange unit, and separating the raw material gas into hydrogen-rich gas and CO/CH by a demethanization pre-separation unit4/N2/H2A liquid;
(3) reacting the CO/CH4/N2/H2The liquid is passed to a stripping unit and separated into hydrogen flash gas and CO/CH4/N2A liquid;
(4) reacting the CO/CH4/N2The liquid is passed to a demethanizer unit and separated into CO/N2Gas and CH4A liquid;
(5) mixing the CO/N2The gas is passed to a denitrification unit and separated into N2Gas and CO liquid.
Preferably, in the method of the present invention, the demethanizer unit comprises a demethanizer, a demethanizer bottom reboiler, and a demethanizer overhead condenser; the stripping unit comprises a stripping tower and a stripping tower bottom reboiler; the demethanizing pre-separation unit comprises a demethanizing pre-separation tower and a demethanizing pre-separation tower top condenser; the denitrification unit comprises a denitrification tower and a condenser at the top of the denitrification tower;
the tower top temperature of the demethanizer pre-separation tower is-180 ℃ to-178 ℃, the tower top pressure is 2.9MPa to 3.3MPa, the tower bottom temperature is-168 ℃ to-166 ℃, and the tower bottom pressure is 2.9MPa to 3.3 MPa;
the temperature of the top of the stripping tower is-168 ℃ to-166 ℃, the pressure of the top of the stripping tower is 0.7MPa to 1.1MPa, the temperature of the bottom of the stripping tower is-149 ℃ to-147 ℃, and the pressure of the bottom of the stripping tower is 0.8MPa to 1.2 MPa;
the top temperature of the demethanizer is-167 ℃ to-166 ℃, the top pressure is 0.7MPa to 0.8MPa, the bottom temperature is-129 ℃ to-127 ℃, and the bottom pressure is 0.5MPa to 0.9 MPa;
the temperature of the top of the denitrogenation tower is-168 ℃ to-166 ℃, the pressure of the top of the denitrogenation tower is 0.5MPa to 0.9MPa, the temperature of the bottom of the denitrogenation tower is-167 ℃ to-165 ℃, and the pressure of the bottom of the denitrogenation tower is 0.5MPa to 0.9 MPa.
Preferably, in the method of the present invention, the heat exchange unit includes a first main heat exchanger and a second main heat exchanger connected in series; the raw material gas subjected to methanol and carbon dioxide removal sequentially passes through the first main heat exchanger, the demethanizer bottom reboiler and the second main heat exchanger;
the raw material gas from which the methanol and the carbon dioxide are removed passes through the first main heat exchanger, the temperature is between 106 ℃ below zero and 104 ℃ below zero, and the pressure is between 2.9MPa and 3.3 MPa;
the raw material gas without methanol and carbon dioxide passes through a reboiler at the bottom of the demethanizer, the temperature is between 127 ℃ below zero and 125 ℃, and the pressure is between 2.9MPa and 3.3 MPa;
and the raw material gas after methanol and carbon dioxide removal passes through the second main heat exchanger, the temperature is-168 ℃ to-166 ℃, and the pressure is 2.9MPa to 3.3 MPa.
Preferably, in the method of the present invention, the molecular sieve adsorption unit comprises a regeneration gas heater, a regeneration gas cooler and at least two molecular sieve adsorbers connected in parallel; wherein the molecular sieve adsorber is configured to be at least one molecular sieve adsorber for adsorption and at least one molecular sieve adsorber for regeneration; the regeneration gas used by the regeneration gas heater and the regeneration gas cooler is the hydrogen-rich gas.
The utility model discloses following beneficial effect has:
(1) through right the utility model discloses a multicomponent cryogenic separation device's technology and parameter selection and equipment lectotype can greatly reduced project investment, energy consumption to it is significant to define the stage in earlier stage to the project, can provide theory and data support for other similar projects simultaneously.
(2) The utility model provides a multicomponent synthetic gas cryrogenic separator energy consumption is lower, the security is higher. Through the utility model discloses a multicomponent synthetic gas cryogenic separation method has solved the technological problem of multicomponent separation in the raw gas.
(3) The prior art mostly adopts two-component or three-component gas deep cooling separation. Compared with the prior art, the utility model discloses a multicomponent synthetic gas cryrogenic separator is applicable to high CH4Gas separation of crude gas with a content of particularly four components (H)2、CO、CH4、N2) And (5) gas separation. The utility model discloses filled the technological blank of multicomponent gaseous cryogenic separation, provided corresponding theory and data support from aspects such as device investment, energy consumption, steady operation. Technical support can be provided for other multi-component gas cryogenic separation projects.
Drawings
Embodiments of the present invention are described in detail below with reference to the attached drawing figures, wherein:
FIG. 1 shows an embodiment of the present invention for cryogenic separation of CO/CH-containing gas4/N2/H2The multi-component synthesis gas plant of (1).
Detailed Description
The present invention will be described in further detail with reference to specific embodiments, which are given for the purpose of illustration only and are not intended to limit the scope of the invention.
FIG. 1 shows an embodiment of the present invention for cryogenic separation of a CO/CH containing stream4/N2/H2The multi-component synthesis gas plant of (a), comprising: the device comprises a molecular sieve adsorption unit, a heat exchange unit, a demethanization pre-separation unit, a stripping unit, a demethanization unit and a denitrification unit; the molecular sieve adsorption unit is used for removing methanol and carbon dioxide in raw material gas from the low-temperature methanol washing device to obtain raw material gas with methanol and carbon dioxide removed; the heat exchange unit is used for cooling the raw material gas subjected to methanol and carbon dioxide removal to obtain a gas cooled by the heat exchange unit; the demethanization pre-separation unit is used for separating the gas cooled by the heat exchange unit into hydrogen-rich gas and CO/CH4/N2/H2A liquid; the stripping unit is used for removing CO/CH from the demethanizing pre-separation unit4/N2/H2Separation of liquid into hydrogen flash gas and CO/CH4/N2A liquid; the demethanization unit is used to convert CO/CH from the stripping unit4/N2Separation of liquids into CO/N2Gas and CH4A liquid; the denitrification unit is used for removing CO/N from the demethanization unit2Separation of gas into N2Gas and CO liquid.
In the device shown in fig. 1, the heat exchange unit is used for cooling the raw material gas subjected to methanol and carbon dioxide removal to-168 ℃ to-166 ℃.
In the apparatus shown in fig. 1, the molecular sieve adsorption unit comprises two molecular sieve adsorbers connected in parallel, and the regeneration gas can be heated and cooled by a regeneration gas heater and a regeneration gas cooler (not shown in the figure); the molecular sieve adsorber is configured into a molecular sieve adsorber for adsorption, and the other molecular sieve adsorber is used for regeneration.
In the plant shown in fig. 1, the demethanizer unit comprises a demethanizer, a demethanizer bottom reboiler, and a demethanizer overhead condenser; the stripping unit comprises a stripping tower and a stripping tower bottom reboiler; the demethanizing pre-separation unit comprises a demethanizing pre-separation tower and a demethanizing pre-separation tower top condenser; the denitrification unit comprises a denitrification tower and a denitrification tower top condenser.
In the apparatus shown in fig. 1, the heat exchange unit comprises a first main heat exchanger and a second main heat exchanger which are connected in series; the first main heat exchanger and the second main heat exchanger are plate-fin heat exchangers, and heat exchange of multiple streams of material flows can be realized; and pipelines used for conveying the qualified raw material gas are sequentially connected in series through the first main heat exchanger, the demethanizer bottom reboiler and the second main heat exchanger so as to achieve the purpose of cooling. The plate-fin heat exchanger has high heat transfer efficiency, can realize the mutual heat exchange of a plurality of streams of materials in one device, and has the advantages of compact structure, light weight, material saving and the like, thereby being widely applied to the heat exchange occasions with phase change at low temperature and in a plurality of streams. According to the characteristics of the cryogenic separation process, plate-fin heat exchangers are selected as heat exchangers in the cold box.
In the plant shown in fig. 1, a methane compressor is further included for compressing the CH of the demethanizer unit4. The device of the utility model can also comprise a nitrogen compressor; the nitrogen compressor is used for providing cold for the demethanizer pre-separation tower top condenser, the demethanizer tower top condenser, the denitrogenation tower top condenser and the heat exchange unit, and the nitrogen can circulate in a reciprocating manner.
In the apparatus shown in FIG. 1, the demethanizer pre-separation column is a packed column, and the packing is in the form of structured packing; the stripping tower is designed by sections of a packed tower and a float valve tower, and the tower trays are in the forms of regular packing and the float valve tower; the denitrification tower is a packed tower, and the packing form is regular packing; the demethanizer is a packed column, and the packing form is regular packing. The material selection aluminum alloy in the design of denitrogenation tower and demethanizer, its advantage lies in light in weight, and the aluminum product low temperature ductility is good, and equipment barrel, head are easy to make.
Example 1
This example serves to illustrate in detail the cryogenic separation process of multi-component syngas of the present invention.
The utility model adopts the raw material gas parameters of the raw gas from the low-temperature methanol washing device
Figure BDA0002244471720000061
Figure BDA0002244471720000071
Molecular sieve adsorption unit
For preventing CO from raw material gas2Free methanol, water and the like enter the cold box to be frozen and blocked, and a molecular sieve adsorption system is arranged in front of the cold box. The cryogenic feed gas fed into the low-temperature methanol washing device contains trace CO2And methanol, the solidification points of the two components are far higher than the internal operation temperature of the cold box, so that CO is arranged at the outlet of the molecular sieve adsorption unit2Content analyzer (methanol prior to CO)2Is adsorbed as long as CO2Not exceeding the standard, methanol not exceeding the standard, so a methanol analyzer is not arranged), and CO is monitored2The content and the control index are CO2≤1PPM。
In the regeneration stage of the molecular sieve adsorber, the regeneration gas is required to heat and cool the molecular sieve. The utility model discloses a copious cooling separator demethanization preseparation tower top hydrogen-rich gas 3.06MPa, the single series output is 143000Nm3The highest temperature of hydrogen-rich gas regeneration can be heated to 160 ℃, the consumption of heating steam is greatly reduced, and the pressure difference between the hydrogen-rich gas and the raw material gas is about 0.1MPa, so that the system pressure fluctuation during the switching of the molecular sieve can be reduced. Therefore, the utility model selects the hydrogen-rich gas as the regeneration gas source of the molecular sieve adsorber.
206000Nm of raw material gas from low-temperature methanol washing device3The/h first enters a molecular sieve adsorber, where the traces of methanol and carbon dioxide contained therein are removed to avoid them freezing in the cold box and causing plugging of cryogenic equipment and piping. The molecular sieve adsorber consists of two molecular sieves, one molecular sieve is used and the other molecular sieve is regenerated, automatic switching is realized by a program controller, the total period is 24 hours, wherein the adsorption time is 12 hours, and the regeneration time is 12 hours; the gas for regenerating the molecular sieve is rich hydrogen from a cold box, and a regeneration gas heater and a regeneration gas generator are neededThe system comprises a regeneration gas cooler and a complete set of switching part instrument valves, wherein the main switching valve adopts an inlet hard sealing triple eccentric butterfly valve.
The regeneration process of molecular sieve adsorption units is generally divided into two main stages:
a heating stage: the hydrogen-rich gas from the cold box is heated to 100 ℃ by 1.5MPa water vapor in a regeneration gas heater, the hot regeneration gas is sent out after passing through an adsorber, and CO2And methanol are released and carried away by the regeneration gas; heating for about 2.5 hr, heating hydrogen-rich gas to 160 deg.C with 1.5MPa steam in a regeneration gas heater, delivering hot regeneration gas through the adsorber for 4.5 hr, and collecting residual CO2And methanol is completely released and carried away by the regeneration gas.
And (3) a cooling stage: after the heating phase, the hot adsorbent is cooled down by hydrogen rich gas from the cold box (bypassing the regeneration gas heater). The regenerated gas is sent to a regenerated gas cooler. After the regeneration step, the regenerated adsorber may be allowed to adsorb again.
Cryogenic separation system
Cryogenic separation, also known as cryogenic rectification, is essentially a gas liquefaction process. The process principle is that hydrogen, carbon monoxide, nitrogen, methane, argon and the like contained in the process gas are cooled and then rectified by utilizing the characteristic of different volatility of each component in the gas, so that different gases are separated.
Since the cryogenic separation process is operated at a low temperature, trace amounts of carbon dioxide and methanol in the feed gas are frozen at a low temperature to block the channels of the plate-fin heat exchanger in the cold box, and thus the trace amounts of carbon dioxide and methanol must be removed in a molecular sieve adsorber before the feed gas enters the cold box. After entering the cold box, the raw material gas is cooled to a certain temperature and enters the demethanizing pre-separation tower. The hydrogen is more volatile than other gases, so that the hydrogen-rich gas is obtained at the top of the demethanization pre-separation tower and is discharged out of the cold box after cold energy is recovered. Liquid mainly containing carbon monoxide, methane and nitrogen from the bottom of the demethanizer pre-separation tower enters a stripping tower for mass transfer separation after throttling. Because the volatility of the carbon monoxide, the nitrogen and the methane is lower than that of the hydrogen, flash steam containing more hydrogen is obtained at the top of the stripping tower, and liquid containing no hydrogen is obtained at the bottom of the stripping tower, so that the separation of the hydrogen from the feed gas is realized. The liquid at the bottom of the stripping tower enters a demethanizer after throttling and reheating, and the methane liquid is obtained at the bottom of the demethanizer because the volatility of nitrogen and carbon monoxide is higher than that of methane, and the liquid is discharged from a cold box after cold energy is recovered. And the carbon monoxide gas rich in nitrogen at the top of the demethanizer enters a denitrification tower for separation. Similarly, because the volatility of nitrogen is higher than that of carbon monoxide, high-purity carbon monoxide liquid is obtained at the bottom of the denitrification tower, and nitrogen-containing waste gas is obtained at the top of the denitrification tower, so that the separation of hydrogen, carbon monoxide, nitrogen and methane is finally realized. And finally reheating the carbon monoxide liquid out of the cold box to obtain a high-purity product carbon monoxide.
The demethanizer pre-separation tower, the demethanizer and the denitrogenation tower are provided with tower top condensers, and the circulating liquid nitrogen is used for throttling to provide the required cold energy; the stripping tower and the demethanizer are both provided with a tower bottom reboiler, and the feed gas is used as a heat source to provide heat.
The cold volume that the cold box needs is got rid of and is provided outside by partial component self throttle in the feed gas, still can be extra to it provide cryogen closed circulation system, the utility model discloses a mode of nitrogen compression, cooling, liquefaction, throttle provides cold volume for the system.
In this embodiment, the raw material gas from the molecular sieve adsorption unit, from which methanol and carbon dioxide are removed, enters a cold box, and the raw material gas from which methanol and carbon dioxide are removed passes through the first main heat exchanger, and then is at-105.8 ℃ and a pressure of 3.14 MPa; the raw material gas without methanol and carbon dioxide passes through a reboiler at the bottom of the demethanizer, the temperature is-126.5 ℃, and the pressure is 3.132 MPa; after the raw material gas from which the methanol and the carbon dioxide are removed passes through the second main heat exchanger, the temperature is-167 ℃, and the pressure is 3.112 MPa; then the hydrogen-rich gas enters a reboiler at the bottom of the demethanizing preseparator, and the hydrogen-rich gas is obtained at the top of the demethanizing preseparator and reheated to 31.4 ℃ by a second main heat exchanger and a first main heat exchanger. The hydrogen-rich gas thus obtained can be divided, for example, into two streams, one stream of 53000Nm3H PSA removal to produce hydrogenOne strand of 53000Nm3The regenerated gas as the molecular sieve completely regenerates the adsorbent and then sends the adsorbent to a methanol synthesis device;
in this example, the temperature at the top of the demethanizer pre-separation column was-179.4 ℃, the pressure at the top of the column was 3.102MPa, the temperature at the bottom of the column was-167 ℃ and the pressure at the bottom of the column was 3.112 MPa; the temperature at the top of the stripping tower is-167.1 ℃, the pressure at the top of the stripping tower is 0.9MPa, the temperature at the bottom of the stripping tower is-148 ℃ and the pressure at the bottom of the stripping tower is 1.031 MPa; the temperature of the top of the demethanizer is-166.5 ℃, the pressure of the top of the demethanizer is 0.731MPa, the temperature of the bottom of the demethanizer is-128 ℃, and the pressure of the bottom of the demethanizer is 0.741 MPa; the temperature of the top of the denitrogenation tower is-167.3 ℃, the pressure of the top of the denitrogenation tower is 0.711MPa, the temperature of the bottom of the denitrogenation tower is-166.7 ℃ and the pressure of the bottom of the denitrogenation tower is 0.721 MPa.
Obtaining CO/CH at the bottom of the demethanizer pre-separation tower4/N2/H2The mixed liquid is throttled and then sent to a stripping tower for dehydrogenation, and H is mainly obtained at the top of the stripping tower2/CO flashed gas 2637Nm3And h, reheating to 31.4 ℃ through a second main heat exchanger and a first main heat exchanger in the cold box. The flash gas thus obtained can be sent to a methanol synthesis apparatus, for example. CO/CH is obtained at the bottom of the stripping tower4/N2Sending the mixed liquid to a demethanizer for rectification;
obtaining CH at the bottom of the demethanizer4And throttling the liquid, and reheating the liquid to 31.4 ℃ through a second main heat exchanger and a first main heat exchanger in the cold box. CH thus obtained4For example, the natural gas can enter a compressor, and enters a natural gas pipeline network after being compressed to 8.2 MPa. The tower top of the demethanizer obtains CO-rich gas (mainly containing N)2Ar, etc.) which is denitrified by a denitrogenation tower to obtain 970Nm at the top of the denitrogenation tower3The nitrogen-containing waste gas is reheated to 31.4 ℃ by the second main heat exchanger and the first main heat exchanger in the cold box. The nitrogen-containing gas thus obtained can be fed, for example, to a fuel gas pipeline network. And obtaining CO liquid without methanol and carbon dioxide at the bottom of the denitrification tower, and reheating the CO liquid to 31.4 ℃ through a second main heat exchanger and a first main heat exchanger in the cold box. The CO thus obtained can be sent to, for example, an ethylene glycol plant as a feed gas.
Selection of methane recovery: the investment and energy consumption were compared as follows at different methane recovery rates:
investment and energy consumption comparison table under different methane recovery rates
Figure BDA0002244471720000101
The utility model discloses a set up methane in methane removal methane preseparation tower top of the tower condenser to rich hydrogen and carry out the condensation and retrieve, control methane removal methane preseparation tower top of the tower temperature and pressure to control the methane rate of recovery.
By integrating the overall investment and income, the annual operating cost of the scheme 1 (96%) is 327 ten thousand yuan higher than that of the scheme 3 (99%), the annual operating cost of the scheme 2 (98%) is about 32 ten thousand yuan higher than that of the scheme 3, and the operating mode of the scheme 3 is optimal. In the methanol synthesis device, if the methane recovery rate is improved from 96% to 99%, the tail gas of the membrane separation is reduced by about 8000Nm3And/h, a methanation recovery device is not added, and the methanol is directly returned to a low-temperature methanol inlet, so that the investment of about 3000 ten thousand yuan is reduced.
More than synthesizing, the utility model discloses a control demethanization preseparation tower top temperature and pressure to with methane recovery rate control for 99%.
In this embodiment, a nitrogen compressor and a natural gas compressor may be further employed, wherein high-pressure nitrogen from the nitrogen compressor enters the cold box, is cooled to-167 ℃ by the first main heat exchanger and the second main heat exchanger in the cold box, is throttled to respectively provide cold energy for the demethanizer pre-separation tower, the demethanizer, the top condenser of the denitrogenation tower and the main heat exchanger, and is reheated to 31.4 ℃ by the second main heat exchanger and the first main heat exchanger in the cold box, and is returned to the nitrogen compressor for cyclic reciprocation; a methane compressor: and the low-pressure methane gas from the cold box enters a methane compressor, is compressed to the required pressure of 8.2MPa, and then is discharged from a boundary area.
This embodiment may also employ a safety vent system (not shown in fig. 1). Because the cold box operates at low temperature, materials can not be directly discharged into the torch system under the condition of parking or abnormity, an emergency discharge system is required to be arranged and comprises a liquid discharge tank and a torch gas heater, and cold materials enter the torch system after being gasified by the two devices.
Through the method of the utility model, the obtained main product performance guaranteed value
Figure BDA0002244471720000111
It is thus clear that through right the utility model discloses a technology and parameter selection and equipment lectotype of multicomponent cryogenic separation device can greatly reduced project investment, energy consumption. The utility model discloses a multicomponent synthetic gas cryrogenic separator is applicable to high CH4Gas separation of crude gas with a content of particularly four components (H)2、CO、CH4、N2) And (5) gas separation. The utility model discloses filled the technological blank of multicomponent gaseous cryogenic separation, provided corresponding theory and data support from aspects such as device investment, energy consumption, steady operation. Technical support can be provided for other multi-component gas cryogenic separation projects.

Claims (9)

1. For cryogenic separation of CO/CH-containing gas4/N2/H2The multi-component synthesis gas plant of (a), comprising:
the device comprises a molecular sieve adsorption unit, a heat exchange unit, a demethanization pre-separation unit, a stripping unit, a demethanization unit and a denitrification unit; wherein,
the molecular sieve adsorption unit is used for removing methanol and carbon dioxide in the raw material gas from the low-temperature methanol washing device to obtain raw material gas from which the methanol and the carbon dioxide are removed;
the heat exchange unit is used for cooling the raw material gas subjected to methanol and carbon dioxide removal to obtain a gas cooled by the heat exchange unit;
the demethanization pre-separation unit is used for separating the gas cooled by the heat exchange unit into hydrogen-rich gas and CO/CH4/N2/H2A liquid;
the stripping unit is used for removing CO/CH from the demethanizing pre-separation unit4/N2/H2Separation of liquid into hydrogen flash gas and CO/CH4/N2A liquid;
the demethanization unit is used for removing the methanol from the stripping unitCO/CH of4/N2Separation of liquids into CO/N2Gas and CH4A liquid;
the denitrification unit is used for removing CO/N from the demethanization unit2Separation of gas into N2Gas and CO liquid.
2. The apparatus of claim 1, wherein the molecular sieve adsorption unit comprises a regeneration gas heater, a regeneration gas cooler, and at least two molecular sieve adsorbers in parallel; the molecular sieve adsorber is configured to be at least one molecular sieve adsorber for adsorption and at least one molecular sieve adsorber for regeneration.
3. The apparatus of claim 1, wherein the demethanizer unit comprises a demethanizer, a demethanizer bottom reboiler, and a demethanizer overhead condenser; the stripping unit comprises a stripping tower and a stripping tower bottom reboiler; the demethanizing pre-separation unit comprises a demethanizing pre-separation tower and a demethanizing pre-separation tower top condenser; the denitrification unit comprises a denitrification tower and a denitrification tower top condenser.
4. The apparatus of claim 1, wherein the heat exchange unit comprises a first primary heat exchanger, a second primary heat exchanger in series.
5. The apparatus of claim 4, wherein the first and second primary heat exchangers are plate-fin heat exchangers.
6. The apparatus according to claim 4, wherein a line for transporting the methanol and carbon dioxide-removed raw gas passes through the first main heat exchanger, the demethanizer bottom reboiler, and the second main heat exchanger in this order.
7. The plant of claim 1, further comprising a methane compressor for compressing the demethanizerCH of unit4。
8. The apparatus of claim 3, wherein the apparatus further comprises a nitrogen compressor; the nitrogen compressor is used for providing cold for the demethanizer pre-separation tower top condenser, the demethanizer tower top condenser, the denitrogenation tower top condenser and the heat exchange unit, and the nitrogen can circulate in a reciprocating manner.
9. The apparatus of claim 3 wherein the demethanizer preseparator, denitrogenation column and demethanizer are packed columns and the stripper is a packed and float valve column staged design column.
CN201921786845.2U 2019-10-23 2019-10-23 Device for the cryogenic separation of a multi-component synthesis gas comprising CO/CH4/N2/H2 Expired - Fee Related CN211120267U (en)

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