CN113144812A - Hydrogen chloride dry purification method and system - Google Patents

Hydrogen chloride dry purification method and system Download PDF

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Publication number
CN113144812A
CN113144812A CN202110485956.5A CN202110485956A CN113144812A CN 113144812 A CN113144812 A CN 113144812A CN 202110485956 A CN202110485956 A CN 202110485956A CN 113144812 A CN113144812 A CN 113144812A
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hydrogen chloride
gas
condenser
liquid
heat exchanger
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黄奕平
仇晓丰
童新洋
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Hangzhou Dongri Energy Efficient Technology Co ltd
HANGZHOU ZHONGHAO TECHNOLOGY CO LTD
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Hangzhou Dongri Energy Efficient Technology Co ltd
HANGZHOU ZHONGHAO TECHNOLOGY CO LTD
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D53/00Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/002Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by condensation
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D53/00Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/26Drying gases or vapours
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B7/00Halogens; Halogen acids
    • C01B7/01Chlorine; Hydrogen chloride
    • C01B7/07Purification ; Separation
    • C01B7/0706Purification ; Separation of hydrogen chloride
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D2257/00Components to be removed
    • B01D2257/20Halogens or halogen compounds
    • B01D2257/204Inorganic halogen compounds
    • B01D2257/2045Hydrochloric acid
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D2257/00Components to be removed
    • B01D2257/80Water

Abstract

The invention relates to a hydrogen chloride dry purification method and a system, wherein the method comprises the following steps: 1) drying the hydrogen chloride gas containing the impurity gas to remove water vapor in the hydrogen chloride gas; 2) pressurizing the hydrogen chloride gas obtained in the step 1), cooling and condensing to liquefy the hydrogen chloride gas to form high-purity hydrogen chloride liquid, keeping impurity gas in a gaseous state, and carrying out gas-liquid separation on the high-purity hydrogen chloride liquid and the impurity gas; 3) the hydrogen chloride liquid is decompressed and gasified by a pressure reducing valve, and the hydrogen chloride gas is output; the invention can also utilize low-temperature hydrogen chloride gas to cool and condense the pressurized hydrogen chloride gas containing impurities, then output the purified hydrogen chloride gas, and cool and condense the pressurized hydrogen chloride gas by utilizing the principle of hydrogen chloride gas gasification and heat absorption. The energy consumed by the method is the electric energy used by the compressor and the refrigerant used by the second condenser, and compared with the steam used by wet purification, the cost is reduced; the invention can also be additionally provided with a rectifying tower to improve the purification purity of the hydrogen chloride gas through gas stripping.

Description

Hydrogen chloride dry purification method and system
Technical Field
The invention relates to the field of hydrogen chloride production, in particular to a hydrogen chloride dry purification system and a hydrogen chloride dry purification method.
Background
The synthesis of hydrogen chloride gas is to fully combust chlorine and hydrogen in a synthesis furnace to obtain hydrogen chloride gas, and excess hydrogen must be filled in the combustion process, so that the synthesized hydrogen chloride gas contains about 6 percent of hydrogen; in addition, the hydrogen chloride gas output by the synthesis furnace is also mixed with water and other gas impurities. In the use process of the hydrogen chloride gas, if the hydrogen chloride gas is not purified, the use effect is poor, the hydrogen chloride gas is continuously consumed in the use process, the included hydrogen is continuously accumulated, and when the hydrogen is accumulated to a certain amount, explosion can be caused. Therefore, the hydrogen chloride gas must be purified before use.
The existing hydrogen chloride gas purification mainly adopts an analytic method, namely, the hydrogen chloride gas is firstly introduced into a solution, then the hydrogen chloride gas is analyzed, analytic equipment such as a device for producing hydrogen chloride from hydrochloric acid through concentration and analysis disclosed in Chinese patent CN110606470A comprises a hydrogen chloride analytic system and a calcium chloride concentration and evaporation system, wherein the hydrogen chloride analytic system comprises a jet mixer, an analytic tower, a hydrogen chloride primary condenser, a hydrogen chloride secondary condenser, a demister, a condensed acid tank, an analytic reboiler and an analytic condensed water tank; the calcium chloride concentration and evaporation system comprises a first-effect evaporator, a first-effect flash evaporation tank, a first-effect condensed water tank, a second-effect evaporator, a second-effect flash evaporation tank, a second-effect condensed water tank, a third-effect evaporator, a third-effect flash evaporation tank, a third-effect condensed water tank, a third-effect discharge preheater, an evaporation condenser, a vacuum buffer tank and a water flow injection pump vacuum unit. The solution falls from the top of the desorption tower, and the high-temperature hydrogen chloride and the water vapor are introduced from the bottom of the desorption tower, so that the solution and the water vapor exchange heat in the tower, and the hydrogen chloride gas in the concentrated hydrochloric acid is desorbed and removed.
When the high-purity hydrogen chloride gas is obtained through analysis, a large amount of steam is needed to heat the solution, statistics shows that 1.5t of steam is needed for continuously purifying 1t of hydrogen chloride gas, the price of the steam in the current market is about 150 yuan/t, and the cost for purifying the hydrogen chloride gas is relatively high.
Disclosure of Invention
The invention aims to provide a hydrogen chloride production device and a hydrogen chloride production method, which aim to solve the problem of high cost required by the existing hydrogen chloride gas purification.
In order to achieve the purpose, the technical scheme provided by the invention is as follows:
the invention relates to a hydrogen chloride dry purification method, which comprises the following steps:
1) drying the hydrogen chloride gas containing the impurity gas to remove water vapor in the hydrogen chloride gas;
2) pressurizing the hydrogen chloride gas obtained in the step 1) to 0.4-1.0MpaG, cooling and condensing to liquefy the hydrogen chloride gas therein to form high-purity hydrogen chloride liquid, keeping impurity gas in a gaseous state, and separating the gas from the liquid;
3) the liquid hydrogen chloride is sent to a first condenser through a control valve, and the liquid hydrogen chloride is vaporized into gas to be output.
Preferably, the step 3) is specifically:
3) and (2) decompressing the hydrogen chloride liquid through a control valve, allowing the hydrogen chloride liquid to enter a shell pass of a first condenser, vaporizing the high-purity hydrogen chloride liquid to form low-temperature hydrogen chloride gas under the combined action of decompression and heat exchange with hydrogen chloride gas containing impurity gas in a tube pass of the first condenser, simultaneously cooling and condensing the hydrogen chloride gas pressurized in the step 1) by utilizing the principle of vaporization and heat absorption of the high-purity hydrogen chloride liquid, and then outputting the hydrogen chloride gas.
Preferably, the hydrogen chloride dry purification method comprises the following steps:
(1) drying the hydrogen chloride gas containing impurities by a drying device to remove water vapor in the hydrogen chloride gas;
(2) the hydrogen chloride gas enters a compressor to be compressed to 0.4-1.0MpaG, and the boiling point of the hydrogen chloride gas is increased;
(3) introducing the compressed hydrogen chloride gas containing impurities into a first condenser, introducing the hydrogen chloride gas containing impurities in the first condenser into a second condenser through a fourth gas outlet of the first condenser and an eighth gas inlet of the second condenser, reducing the temperature of the hydrogen chloride gas containing impurities by the second condenser through a refrigerant, liquefying the hydrogen chloride gas to form high-purity hydrogen chloride liquid, and outputting the impurity gas from an eighth gas outlet of the second condenser; the high-purity hydrogen chloride liquid is decompressed by a control valve and enters the shell pass of a first condenser, and under the combined action of decompression and heat exchange with the impurity-containing hydrogen chloride gas introduced into the first condenser from a compressor, the high-purity hydrogen chloride liquid is vaporized to form low-temperature hydrogen chloride gas;
(4) the high-purity hydrogen chloride liquid absorbs heat in the vaporization process, the high-purity hydrogen chloride in the vaporization process is used as a refrigerant to cool the hydrogen chloride gas containing impurities in the first condenser, the high-pressure hydrogen chloride gas in the first condenser is liquefied to form high-purity hydrogen chloride liquid, the high-purity hydrogen chloride liquid returns to the first condenser through the control valve to carry out heat exchange, and part of non-liquefied gas in the hydrogen chloride gas containing impurities enters the second condenser in a gas form to be cooled and condensed continuously;
(5) the hydrogen chloride vaporized after returning to the first condenser is output from the first condenser in the form of a gas.
Preferably, in the step (2), in the compression process, the temperature of the hydrogen chloride gas containing impurities is increased to generate heat, and part of the compressed hydrogen chloride gas containing impurities is firstly introduced into the first heat exchanger and part of the compressed hydrogen chloride gas containing impurities is introduced into the second heat exchanger;
in the step (3), the compressed hydrogen chloride gas containing impurities in the first heat exchanger and the second heat exchanger is introduced into a first condenser;
returning the impurity gas output from the eighth gas outlet of the second condenser in the step (3) to the second heat exchanger from the seventh gas inlet of the second heat exchanger, performing heat exchange with the impurity-containing hydrogen chloride gas compressed in the second heat exchanger, heating the impurity gas, and sending the heated impurity gas into the synthesis furnace from the seventh gas outlet of the second heat exchanger for reuse;
and (5) returning the high-purity hydrogen chloride gas output from the fifth gas outlet of the first condenser to the first heat exchanger from the third gas inlet of the first heat exchanger, performing heat exchange with the impurity-containing hydrogen chloride gas compressed in the first heat exchanger, heating the high-purity hydrogen chloride gas to reach the temperature required by industrial use, and outputting the high-purity hydrogen chloride gas from the third gas outlet of the first heat exchanger.
The hydrogen chloride gas is required to be heated when being used industrially, and the impurity gas is also required to be heated when the impurity gas enters the synthesis furnace for reuse, so that the high-pressure impurity-containing hydrogen chloride gas is respectively heated with the purified high-purity hydrogen chloride gas and the impurity gas, the heat generated when the gas is pressurized is fully utilized, and the energy consumption required by the subsequent use of the hydrogen chloride gas and the recovery of the impurity-containing gas is reduced.
Preferably, the hydrogen chloride gas containing impurities in the first heat exchanger and the second heat exchanger in the step (3) is firstly introduced into the rectifying tower before being introduced into the first condenser; and (3) the hydrogen chloride liquefied in the step (3) and the step (4) also passes through the rectifying tower before entering the control valve for pressure reduction, and impurities dissolved in the hydrogen chloride liquid are stripped by the hydrogen chloride gas containing the impurities, so that the purity of the hydrogen chloride liquid is higher.
Preferably, the part of the hydrogen chloride gas containing impurities after partial compression is introduced into a third heat exchanger in the step (2), the refrigerant used for performing heat exchange on the second condenser in the step (3) is introduced into the third heat exchanger before being recovered, and performs heat exchange with the hydrogen chloride gas containing impurities in the third heat exchanger, so that part of the hydrogen chloride in the third heat exchanger is liquefied, the hydrogen chloride liquid, the hydrogen chloride gas without condensation and the impurities enter a rectifying tower, the liquefied hydrogen chloride gas is output from a liquid outlet of the rectifying tower, and is decompressed by a control valve and enters a shell pass of the first condenser for vaporization, so that low-temperature hydrogen chloride gas is formed; outputting the uncondensed hydrogen chloride gas and the impurity gas from a gas outlet of a rectifying tower of the rectifying tower, entering the first condenser from a fourth gas inlet of the first condenser, and continuously liquefying in the manner of the steps (3) and (4).
Preferably, in the step (3) and the step (4), before the hydrogen chloride liquid enters the control valve from the rectifying tower for pressure reduction, the temperature of the hydrogen chloride liquid is also raised through a reboiler, and impurities dissolved in the hydrogen chloride liquid are separated and returned to the rectifying tower.
Preferably, the step 1) of drying the hydrogen chloride gas containing the impurity gas comprises the following specific steps:
(1.1) introducing the hydrogen chloride gas containing the impurity gas into a drying cooler, and cooling the hydrogen chloride gas containing the impurity gas to ensure that part of water vapor is liquefied due to cooling and separated from the hydrogen chloride gas containing the impurity gas;
(1.2) introducing the hydrogen chloride gas containing the impurity gas obtained in the step (1.1) into a sulfuric acid drying tower, and absorbing water vapor by using concentrated sulfuric acid in the sulfuric acid drying tower;
and (1.3) introducing the hydrogen chloride gas containing the impurity gas obtained in the step (1.2) into a gas demister to remove sulfuric acid mist generated when a sulfuric acid drying tower absorbs water vapor.
The invention also relates to a hydrogen chloride dry purification system, which comprises a drying device, a compressor, a first heat exchanger, a first condenser, a second heat exchanger and a second condenser; the compressor is provided with a first air inlet and a first air outlet which are communicated with each other, and the first air inlet is connected with the drying device;
the first heat exchanger is provided with a second air inlet and a second air outlet which are communicated with each other, and a third air inlet and a third air outlet which are communicated with each other, wherein the second air inlet is communicated with the first air outlet of the compressor;
the first condenser is provided with a fourth air inlet, a fourth air outlet and a first liquid outlet which are communicated with each other, and a fifth liquid inlet and a fifth air outlet which are communicated with each other, the fourth air inlet is communicated with the second air outlet of the first heat exchanger, the first liquid outlet is communicated with the fifth liquid inlet through a pipeline and a control valve arranged on the pipeline, and the fifth air outlet is communicated with the third air inlet of the first heat exchanger;
the second heat exchanger is provided with a sixth air inlet and a sixth air outlet which are communicated with each other, and a seventh air inlet and a seventh air outlet which are communicated with each other, the sixth air inlet is communicated with the first air outlet of the compressor, and the sixth air outlet is communicated with the fourth air inlet of the first condenser;
the second condenser is provided with an eighth air inlet, an eighth air outlet and a second liquid outlet which are communicated with each other, and a refrigerant feeding hole and a refrigerant discharging hole which are used for inputting and outputting external refrigerants;
the third gas outlet is used for outputting the purified hydrogen chloride gas, and the seventh gas outlet is used for outputting the processed impurity gas.
Preferably, the drying device comprises a drying cooler, a sulfuric acid drying tower and a gas demister which are connected in sequence. The drying cooler liquefies water vapor through the mode of cooling, and sulphuric acid drying tower passes through sulphuric acid absorption water vapor, produces a large amount of heats and produces the sulfuric acid fog after sulphuric acid absorbs water vapor, and gas demister is used for cleaing away the sulfuric acid fog.
Preferably, the bottom of the drying cooler is connected with a condensed acid tank, and the sulfuric acid drying tower is provided with a cooler for reducing the temperature. After the water vapor is liquefied, part of hydrogen chloride gas is dissolved in water to form hydrochloric acid, and the condensed acid tank is used for collecting the part of hydrochloric acid; the sulfuric acid drying tower generates a large amount of heat when absorbing water, and the sulfuric acid drying tower is cooled by the cooler, so that the sulfuric acid drying tower is protected.
Preferably, a plurality of cooling condensers are arranged between the gas demister and the sulfuric acid drying tower. The cooling condenser is used for cooling the hydrogen chloride gas containing impurities, and the temperature of the compressor is prevented from being overhigh.
Preferably, the device further comprises a rectifying tower, the rectifying tower comprises a rectifying tower air inlet, a rectifying tower air outlet, a rectifying tower liquid inlet and a rectifying tower liquid outlet, the second air outlet of the first heat exchanger and the sixth air outlet of the second heat exchanger are communicated with the rectifying tower air inlet, the rectifying tower air outlet is communicated with the fourth air inlet of the first condenser, the first liquid outlet of the first condenser and the second liquid outlet of the second condenser are communicated with the rectifying tower liquid inlet, and the rectifying tower liquid outlet is communicated with the fifth liquid inlet of the first condenser through a pipeline and a control valve arranged on the pipeline. The impurity gas dissolved in the hydrogen chloride liquid is extracted by the rectifying tower in a gas stripping mode, so that the purity of the hydrogen chloride liquid is higher, and the purity of the hydrogen chloride gas obtained after pressure reduction and heat exchange is also higher.
Preferably, the heat exchanger further comprises a third heat exchanger, the third heat exchanger comprises a first channel and a second channel, two ends of the first channel are respectively communicated with the compressor and the rectifying tower, one end of the second channel is connected with a refrigerant discharge port of the second condenser, and the other end of the second channel is used for recovering the refrigerant.
Preferably, the rectifying tower is also provided with a reboiler, the bottom of the reboiler is connected with a liquid outlet of the rectifying tower, and the top of the reboiler is communicated with the inside of the rectifying tower through a gas pipeline. The reboiler passes through the high principle of hydrogen chloride boiling point than the boiling point of impurity gas, with hydrogen chloride liquid heating to between impurity boiling point and the hydrogen chloride boiling point for impurity gas vaporizes and separates with the hydrogen chloride liquid, and then makes the purity of hydrogen chloride liquid higher.
Compared with the prior art, the technical scheme provided by the invention has the following beneficial effects:
1. the invention relates to a hydrogen chloride dry purification system and a hydrogen chloride dry purification method, which compress hydrogen chloride gas containing impurity gas through a compressor to raise the boiling point of the hydrogen chloride gas, then cool the gas to liquefy the hydrogen chloride, finally decompress the system through a control valve to vaporize hydrogen chloride liquid due to the lowering of the boiling point to form high-purity hydrogen chloride gas, wherein the energy consumed in the whole process mainly comprises electric energy and a small amount of refrigerant used when the compressor compresses the hydrogen chloride gas containing impurity, the refrigerant is from a refrigerating unit, 150-degree electricity is needed for purifying 1t of hydrogen chloride gas (the refrigerant is converted into electricity), the cost of the 150-degree electricity is 0.6 yuan, and the cost is lower than the cost of steam used by an analytic method, so the invention can reduce the cost of hydrogen chloride purification.
2. When the hydrogen chloride gas is purified by adopting the hydrogen chloride dry purification method, the purified hydrogen chloride liquid absorbs heat in the process of decompression and vaporization, the just vaporized hydrogen chloride gas is used for cooling the first condenser, and then the hydrogen chloride gas containing impurities in the first condenser is liquefied, so that the cold energy of the vaporized hydrogen chloride liquid is fully utilized, and the using amount of a refrigerant is further reduced.
3. In the process of purifying the hydrogen chloride gas by adopting the hydrogen chloride dry purification method, the heat is generated when the hydrogen chloride gas containing the impurity gas is compressed, and the heat exchange is respectively carried out on the compressed hydrogen chloride gas containing the impurity gas, the purified hydrogen chloride gas and the separated impurity gas, so that the purified hydrogen chloride gas reaches the industrial use temperature, the impurity gas meets the temperature requirement of recycling, and the energy consumption of heating the purified hydrogen chloride gas and the separated impurity gas in the follow-up process is reduced.
4. According to the invention, the noncondensable hydrogen chloride gas output from the first condenser is subjected to cooling treatment by the second condenser, so that the hydrogen chloride is extracted as much as possible, the hydrogen chloride extraction efficiency is increased, and the waste of the hydrogen chloride is reduced.
5. According to the invention, in the rectifying tower, the hydrogen chloride gas is used for stripping gas impurities in the hydrogen chloride liquid, the reboiler is used for vaporizing the gas impurities in the hydrogen chloride liquid, so that the purity of the hydrogen chloride liquid is further ensured, and then the high-purity hydrogen chloride liquid is subjected to reduced pressure vaporization, so that the purity of the obtained hydrogen chloride gas is higher.
Drawings
FIG. 1 is a schematic diagram of a hydrogen chloride dry purification system according to example 1;
FIG. 2 is a structural view of a hydrogen chloride dry purification system according to example 2;
FIG. 3 is a schematic view of the compressor;
FIG. 4 is a schematic view of the structure of the first heat exchanger;
FIG. 5 is a schematic structural view of a first condenser;
FIG. 6 is a schematic view of the structure of a second heat exchanger;
FIG. 7 is a schematic structural view of a second condenser;
FIG. 8 is a schematic view of the structure of a rectifying column;
fig. 9 is a structural diagram of a hydrogen chloride dry purification system according to example 3.
Description of the drawings: 1-a drying cooler, 11-a condensed acid tank, 2-a sulfuric acid drying tower, 21-a cooler, 3-a temperature reduction condenser, 4-a gas demister, 5-a compressor, 51-a first gas outlet, 52-a first gas outlet, 6-a first heat exchanger, 61-a second gas inlet, 62-a second gas outlet, 63-a third gas inlet, 64-a third gas outlet, 7-a first condenser, 71-a fourth gas inlet, 72-a fourth gas outlet, 73-a fifth liquid inlet, 74-a fifth gas outlet, 75-a first liquid outlet, 8-a second heat exchanger, 81-a sixth gas inlet, 82-a sixth gas outlet, 83-a seventh gas inlet, 84-a seventh gas outlet, 9-a second condenser, 91-eighth gas inlet, 92-eighth gas outlet, 93-refrigerant feed inlet, 94-refrigerant discharge outlet, 95-second liquid outlet, 10-rectifying tower, 101-rectifying tower gas inlet, 102-rectifying tower gas outlet, 103-rectifying tower liquid inlet, 104-rectifying tower liquid outlet, 11-control valve, 12-reboiler and 13-third heat exchanger.
Detailed Description
For further understanding of the present invention, the present invention will be described in detail with reference to examples, which are provided for illustration of the present invention but are not intended to limit the scope of the present invention.
Example 1
The hydrogen chloride gas in this embodiment is obtained by burning chlorine and hydrogen in a synthesis furnace, and since excess hydrogen needs to be introduced in the process of synthesizing the hydrogen chloride gas, the impurity gas in the synthesized hydrogen chloride gas mainly refers to hydrogen, and the hydrogen content is about 6%, and of course, the hydrogen chloride gas also contains a trace amount of water vapor and other gases. This example illustrates the present invention by taking the removal of hydrogen and water vapor from the synthesis hydrogen chloride gas as an example. It should be noted that, when removing other impurity gases, only the temperature and pressure parameters need to be changed, and the method can also be realized.
Referring to fig. 1, a hydrogen chloride dry purification system of the present embodiment includes a drying device, a compressor 5, a first heat exchanger 6, a first condenser 7, a second heat exchanger 8, and a second condenser 9.
The drying device is used for removing trace water vapor in the synthetic hydrogen chloride gas and comprises a drying cooler 1, a sulfuric acid drying tower 2 and a gas demister 4 which are sequentially connected. The drying cooler 1 liquefies the water vapor by cooling to form water drops, and part of hydrogen chloride gas is dissolved in the water to form hydrochloric acid, so that the bottom of the drying cooler 1 is connected with a condensed acid tank 11 for collecting the part of hydrochloric acid; the sulfuric acid drying tower 2 absorbs water vapor through sulfuric acid, and the sulfuric acid absorbs the water vapor to generate a large amount of heat and generate sulfuric acid mist, so that the sulfuric acid drying tower 2 is provided with a cooler 21 for cooling, the sulfuric acid drying tower 2 is cooled through the cooler 21, the sulfuric acid drying tower 2 is protected, and the gas demister 4 can be used for removing the sulfuric acid mist; the temperature of the gas output from the top of the sulfuric acid drying tower 2 reaches about 18 ℃, and a 2-stage cooling condenser 3 is arranged between the sulfuric acid drying tower 2 and the gas demister 4 for protecting the gas demister 4 and the compressor 5 and is used for cooling the hydrogen chloride gas containing impurities.
Referring to fig. 1 and 3, the compressor 5 is provided with a first gas inlet 51 and a first gas outlet 52 which are communicated with each other, the first gas inlet 51 is connected with a drying device, hydrogen chloride gas containing impurity gas enters the compressor 5 from the first gas inlet 51 after being dried, and the compressor 5 compresses the gas to 0.9 Mpa.
Referring to fig. 1 and 4, the first heat exchanger 6 is provided with a second inlet 61 and a second outlet 62 which are communicated with each other, and a third inlet 63 and a third outlet 64 which are communicated with each other, wherein the second inlet 61 is communicated with the first outlet 52 of the compressor 5.
Referring to fig. 1 and 5, the first condenser 7 is provided with a fourth air inlet 71, a fourth air outlet 72 and a first liquid outlet 75 which are communicated with each other, and a fifth liquid inlet 73 and a fifth air outlet 74 which are communicated with each other, the fourth air inlet 71 is communicated with the second air outlet 62 of the first heat exchanger 6, the first liquid outlet 75 is communicated with the fifth liquid inlet 73 through a pipeline and a control valve 11 arranged on the pipeline, and the fifth air outlet 74 is communicated with the third air inlet 63 of the first heat exchanger 6.
Referring to fig. 1 and 6, the second heat exchanger 8 is provided with a sixth gas inlet 81 and a sixth gas outlet 82 which are communicated with each other, and a seventh gas inlet 83 and a seventh gas outlet 84 which are communicated with each other, the sixth gas inlet 81 is communicated with the first gas outlet 52 of the compressor 5, and the sixth gas outlet 82 is communicated with the fourth gas inlet 71 of the first condenser 7.
Referring to fig. 1 and 7, the second condenser 9 is provided with an eighth air inlet 91, an eighth air outlet 92 and a second liquid outlet 95 which are communicated with each other, and a refrigerant inlet 93 and a refrigerant outlet 94 for inputting and outputting an external refrigerant, the eighth air inlet 91 is communicated with the fourth air outlet 72 of the first condenser 7, the second liquid outlet 95 is connected to a pipeline between the first liquid outlet 75 and the control valve 11 through a pipeline, and the eighth air outlet 92 is communicated with the seventh air inlet 83 of the second heat exchanger 8.
Referring to fig. 1, the third gas outlet 64 is used for outputting purified hydrogen chloride gas, and the seventh gas outlet 84 is used for outputting treated tail gas, i.e. hydrogen gas and a small amount of non-condensable hydrogen chloride gas.
The hydrogen chloride dry purification method based on the system comprises the following steps:
(1) the temperature of the synthesized hydrogen chloride gas containing impurities is 45-55 ℃, the hydrogen chloride gas containing impurities is dried by a drying cooler 1 and a sulfuric acid drying tower 2 in sequence, the temperature of the hydrogen chloride gas containing impurities after drying is 16 ℃, the air pressure is 0.052MPaG, and the drying treatment comprises the following specific steps:
(1.1) introducing hydrogen chloride gas containing impurity gas into a drying cooler 1, separating part of water vapor from the hydrogen chloride gas containing impurity gas due to temperature reduction and liquefaction of the drying cooler 1 in a cooling mode, and allowing liquid water to flow into a condensed acid tank 11 along the inner wall of the drying cooler 1;
(1.2) introducing the hydrogen chloride gas containing the impurity gas obtained in the step (1.1) into a sulfuric acid drying tower 2, wherein the sulfuric acid drying tower 2 absorbs water vapor through sulfuric acid, and a large amount of heat and sulfuric acid mist are generated in the process that the sulfuric acid absorbs the water vapor, so that the sulfuric acid drying tower 2 is cooled by matching with a cooler 21, and the dried gas is cooled by matching with a 2-stage cooling condenser;
and (1.3) introducing the hydrogen chloride gas containing the impurity gas obtained in the step (1.2) into a gas demister 4 to remove sulfuric acid mist generated when the sulfuric acid drying tower 2 absorbs water vapor.
(2) The hydrogen chloride gas containing the impurities after being dried by the drying device enters a compressor 5 for compression treatment, the air pressure of the hydrogen chloride gas containing the impurities is increased from 0.05-0.06 Mpa to 0.9MpaG, and the boiling point of the hydrogen chloride gas is further increased, at the moment, the boiling point of the hydrogen chloride gas is increased from-85 ℃ to-33 ℃, and the boiling point of the hydrogen gas is-259.2 ℃; in the process of compressing the hydrogen chloride gas containing impurities, the temperature of the hydrogen chloride gas containing impurities is raised to 42 ℃;
(3) the compressed hydrogen chloride gas containing impurities is output from the first gas outlet 51, part of the hydrogen chloride gas containing impurities is introduced into the first heat exchanger 6 from the second gas inlet 61, part of the hydrogen chloride gas containing impurities is introduced into the second heat exchanger 8 from the sixth gas inlet 81, and the proportion of the hydrogen chloride gas containing impurities introduced into the first heat exchanger 6 and the second heat exchanger 8 is about 85%; the hydrogen chloride gas containing impurities in the first heat exchanger 6 and the second heat exchanger 8 is respectively output through the second gas outlet 62 and the sixth gas outlet 82, enters the first condenser 7 from the fourth gas inlet 71, the hydrogen chloride gas containing impurities in the first condenser 7 is completely output from the fourth gas outlet 72 because the first condenser 7 does not introduce the refrigerant, and is introduced into the second condenser 9 from the eighth gas inlet 91, the second condenser 9 inputs the refrigerant from the refrigerating unit from the refrigerant inlet 93, the temperature of the refrigerant is-80 ℃, the refrigerant is recycled to the refrigerating unit from the refrigerant outlet 94, the high-pressure hydrogen chloride gas containing impurities in the second condenser 9 is cooled through the refrigerant, so that the hydrogen chloride gas in the hydrogen chloride gas is liquefied to form hydrogen chloride liquid, the temperature of the hydrogen chloride liquid is-57 ℃, the pressure is 0.879MpaG, and the impurity gases such as hydrogen gas still exist in a gas form (the hydrogen gas contains a small amount of non-condensable hydrogen chloride gas), the temperature of the impurity gas is-40.8 ℃, the air pressure is 0.885MpaG, the impurity gas in the second condenser 9 is output to the second heat exchanger 8 from the eighth gas outlet 92, the impurity gas exchanges heat with the hydrogen chloride gas containing the impurities after being compressed in the second heat exchanger 8, the impurity gas is heated and decompressed, the impurity gas is sent into the synthesis furnace for recycling from the seventh gas outlet of the second heat exchanger 8 after being heated and decompressed, the temperature of the output impurity gas is 25 ℃, the air pressure is 0.878MpaG, and simultaneously, the hydrogen chloride gas containing the impurities entering the second heat exchanger 8 from the compressor is cooled, so that the temperature of the hydrogen chloride gas containing the impurities entering the first condenser from the second heat exchanger 8 is reduced to-33.95 ℃; the hydrogen chloride liquid in the second condenser 9 is output from a second liquid outlet 95, is decompressed by the control valve 11 and then returns to the shell side of the first condenser 7 from a fifth liquid inlet 73 of the first condenser 7, and under the combined action of decompression and heat exchange with the hydrogen chloride gas containing impurities and introduced into the first condenser 7 from the compressor, the high-purity hydrogen chloride liquid is vaporized to form low-temperature hydrogen chloride gas, the temperature of the low-temperature hydrogen chloride gas is-33.99 ℃, and the air pressure is 0.89 MpaG;
(4) the high-purity hydrogen chloride liquid absorbs heat in the vaporization process, the high-purity hydrogen chloride in the vaporization process is used as a refrigerant to cool the high-pressure impurity-containing hydrogen chloride gas in the first condenser 7, the hydrogen chloride gas is liquefied, the high-purity hydrogen chloride liquid is output from the first liquid outlet 75, is decompressed through the control valve 11 and then returns to the first condenser 7 for heat exchange, and the steps are repeated, and the first condenser 7 is continuously cooled; part of the unliquefied gas in the hydrogen chloride gas containing impurities enters a second condenser 9 for continuous cooling and condensation;
(5) the vaporized high-purity hydrogen chloride gas returned from the fifth liquid inlet 73 to the first condenser 7 is output from the fifth gas outlet 74, returned from the third gas inlet 63 of the first heat exchanger 6 to the first heat exchanger 6, subjected to heat exchange with the hydrogen chloride gas containing impurities compressed in the first heat exchanger 6, heated to a temperature required for industrial use, and output from the third gas outlet 64 of the first heat exchanger 6, wherein the temperature of the high-purity hydrogen chloride gas is 48 ℃ and the gas pressure is 0.8789 MpaG.
The energy consumed in the whole purification process mainly comprises electric energy and a small amount of refrigerant which are used when the compressor compresses the hydrogen chloride gas containing impurities, the refrigerant is from a refrigerating unit, the refrigerating unit also consumes the electric energy, according to statistics, the purification of 1t of hydrogen chloride gas probably needs 150 degrees of electricity, the cost of the 150 degrees of electricity is 90 yuan, and the cost is lower than that of steam used by an analytic method, so the invention can reduce the purification cost of the hydrogen chloride.
Example 2
The hydrogen chloride gas in this embodiment is obtained by burning chlorine and hydrogen in a synthesis furnace, and since excess hydrogen needs to be introduced in the process of synthesizing the hydrogen chloride gas, the impurity gas in the synthesized hydrogen chloride gas mainly refers to hydrogen, and the hydrogen content is about 6%, and of course, the hydrogen chloride gas also contains a trace amount of water vapor and other gases. This example illustrates the present invention by taking the removal of hydrogen and water vapor from the synthesis hydrogen chloride gas as an example. It should be noted that, when removing other impurity gases, only the temperature and pressure parameters need to be changed, and the method can also be realized.
Referring to fig. 2, the hydrogen chloride dry purification system includes a drying device, a compressor 5, a first heat exchanger 6, a first condenser 7, a second heat exchanger 8, a second condenser 9, and a rectifying tower 10.
The drying device is used for removing trace water vapor in the synthetic hydrogen chloride gas and comprises a drying cooler 1, a sulfuric acid drying tower 2 and a gas demister 4 which are sequentially connected. The drying cooler 1 liquefies the water vapor by cooling to form water drops, and part of hydrogen chloride gas is dissolved in the water to form hydrochloric acid, so that the bottom of the drying cooler 1 is connected with a condensed acid tank 11 for collecting the part of hydrochloric acid; the sulfuric acid drying tower 2 absorbs water vapor through sulfuric acid, and the sulfuric acid absorbs the water vapor to generate a large amount of heat and generate sulfuric acid mist, so that the sulfuric acid drying tower 2 is provided with a cooler 21 for cooling, the sulfuric acid drying tower 2 is cooled through the cooler 21, the sulfuric acid drying tower 2 is protected, and the gas demister 4 can be used for removing the sulfuric acid mist; the temperature of the gas output from the top of the sulfuric acid drying tower 2 reaches about 18 ℃, and a 2-stage cooling condenser 3 is arranged between the sulfuric acid drying tower 2 and the gas demister 4 for protecting the gas demister 4 and the compressor 5 and is used for cooling the hydrogen chloride gas containing impurities.
Referring to fig. 2 and 3, the compressor 5 is provided with a first gas inlet 51 and a first gas outlet 52 which are communicated with each other, the first gas inlet 51 is connected with a drying device, hydrogen chloride gas containing impurity gas enters the compressor 5 from the first gas inlet 51 after being dried, and the compressor 5 compresses the gas to 0.9 Mpa.
Referring to fig. 2 and 4, the first heat exchanger 6 is provided with a second inlet 61 and a second outlet 62 which are communicated with each other, and a third inlet 63 and a third outlet 64 which are communicated with each other, wherein the second inlet 61 is communicated with the first outlet 52 of the compressor 5.
Referring to fig. 2 and 6, the second heat exchanger 8 is provided with a sixth gas inlet 81 and a sixth gas outlet 82 which are communicated with each other, and a seventh gas inlet 83 and a seventh gas outlet 84 which are communicated with each other, wherein the sixth gas inlet 81 is communicated with the first gas outlet 52 of the compressor 5.
Referring to fig. 2 and 8, the rectifying tower 10 includes a rectifying tower gas inlet 101, a rectifying tower gas outlet 102, a rectifying tower liquid inlet 103 and a rectifying tower liquid outlet 104, the second gas outlet 62 of the first heat exchanger 6 and the sixth gas outlet 82 of the second heat exchanger 8 are both communicated with the rectifying tower gas inlet 101, and the rectifying tower gas outlet 102 is communicated with the fourth gas inlet 71 of the first condenser 7.
Referring to fig. 2 and 5, the first condenser 7 is provided with a fourth gas inlet 71, a fourth gas outlet 72 and a first liquid outlet 75 which are communicated with each other, and a fifth liquid inlet 73 and a fifth gas outlet 74 which are communicated with each other, the first liquid outlet 75 is communicated with the liquid inlet 103 of the rectifying tower through a liquid pipeline, and the fifth gas outlet 74 is communicated with the third gas inlet 63 of the first heat exchanger 6.
Referring to fig. 2 and 7, the second condenser 9 is provided with an eighth air inlet 91, an eighth air outlet 92 and a second liquid outlet 95 which are communicated with each other, and a refrigerant inlet 93 and a refrigerant outlet 94 for inputting and outputting an external refrigerant, the eighth air inlet 91 is communicated with the fourth air outlet 72 of the first condenser 7, the second liquid outlet 95 is communicated with the liquid inlet 103 of the rectifying tower through a liquid pipeline, and the eighth air outlet 92 is communicated with the seventh air inlet 83 of the second heat exchanger 8.
Referring to fig. 2, the rectification column outlet 104 is connected to the fifth inlet 74 of the first condenser 7 via a pipe and a control valve 11 provided on the pipe. The principle of the rectifying tower 10 is that the components in the mixture have different volatilities, that is, the vapor pressure of each component at the same temperature is different, so that the light component in the liquid phase is transferred to the gas phase, and the heavy component in the gas phase is transferred to the liquid phase, thereby realizing the separation of the rectifying tower. Rectifying column 10 is still furnished with reboiler 12, the bottom and the rectifying column liquid outlet 104 of reboiler 12 are connected, the inside intercommunication of gas pipeline and rectifying column 10 is passed through at the top of reboiler 12, reboiler 12 passes through the high principle of hydrogen chloride boiling point than gaseous boiling point of impurity, with hydrogen chloride liquid heat-up to between impurity boiling point and the hydrogen chloride boiling point for gaseous impurity vaporizes and with hydrogen chloride liquid separation, and then makes the purity of hydrogen chloride liquid higher.
The third gas outlet 64 is used for outputting purified hydrogen chloride gas, and the seventh gas outlet 84 is used for outputting treated tail gas, i.e. hydrogen gas and a small amount of noncondensable hydrogen chloride gas.
The hydrogen chloride dry purification method based on the system comprises the following steps:
(1) the temperature of the synthesized hydrogen chloride gas containing impurities is 45-55 ℃, the hydrogen chloride gas containing impurities is dried by a drying cooler 1 and a sulfuric acid drying tower 2 in sequence, the temperature of the hydrogen chloride gas containing impurities after drying is 16 ℃, the air pressure is 0.052MPaG, and the drying treatment comprises the following specific steps:
(1.1) introducing hydrogen chloride gas containing impurity gas into a drying cooler 1, separating part of water vapor from the hydrogen chloride gas containing impurity gas due to temperature reduction and liquefaction of the drying cooler 1 in a cooling mode, and allowing liquid water to flow into a condensed acid tank 11 along the inner wall of the drying cooler 1;
(1.2) introducing the hydrogen chloride gas containing the impurity gas obtained in the step (1.1) into a sulfuric acid drying tower 2, wherein the sulfuric acid drying tower 2 absorbs water vapor through sulfuric acid, and a large amount of heat and sulfuric acid mist are generated in the process that the sulfuric acid absorbs the water vapor, so that the sulfuric acid drying tower 2 is cooled by matching with a cooler 21, and the dried gas is cooled by matching with a 2-stage cooling condenser;
and (1.3) introducing the hydrogen chloride gas containing the impurity gas obtained in the step (1.2) into a gas demister 4 to remove sulfuric acid mist generated when the sulfuric acid drying tower 2 absorbs water vapor.
(2) The hydrogen chloride gas containing the impurities after being dried by the drying device enters a compressor 5 for compression treatment, the air pressure of the hydrogen chloride gas containing the impurities is increased from 0.05-0.06 Mpa to 0.9MpaG, and the boiling point of the hydrogen chloride gas is further increased, at the moment, the boiling point of the hydrogen chloride gas is increased from-85 ℃ to-33 ℃, and the boiling point of the hydrogen gas is-259.2 ℃; in the process of compressing the hydrogen chloride gas containing impurities, the temperature of the hydrogen chloride gas containing impurities is raised to 42 ℃;
(3) the compressed hydrogen chloride gas containing impurities is output from the first air outlet 51, part of the hydrogen chloride gas containing impurities is introduced into the first heat exchanger 6 from the second air inlet 61, part of the hydrogen chloride gas containing impurities is introduced into the second heat exchanger 8 from the sixth air inlet 81, and the proportion of the hydrogen chloride gas containing impurities introduced into the first heat exchanger 6 and the second heat exchanger 8 is 85%; the hydrogen chloride gas containing impurities in the first heat exchanger 6 and the second heat exchanger 8 is respectively output through the second air outlet 62 and the sixth air outlet 82, is introduced into the rectifying tower 10 from the rectifying tower air inlet 101, is output from the rectifying tower air outlet 102, enters the first condenser 7 from the fourth air inlet 71 of the first condenser 7, because the first condenser 7 does not introduce the refrigerant, the hydrogen chloride gas containing impurities in the first condenser 7 is completely output from the fourth air outlet 72, is introduced into the second condenser 9 from the eighth air inlet 91 of the second condenser 9, the second condenser 9 inputs the refrigerant from the refrigerating unit from the refrigerant inlet 93, the temperature of the refrigerant is-80 ℃, the refrigerant is recovered to the refrigerating unit from the refrigerant outlet 94, and then the high-pressure hydrogen chloride gas containing impurities in the second condenser 9 is cooled through the refrigerant, so that the hydrogen chloride gas therein is liquefied, forming hydrogen chloride liquid, wherein the temperature of the hydrogen chloride liquid is-57 ℃, the pressure is 0.879MpaG, while impurity gases such as hydrogen gas and the like still exist in the form of gas (the hydrogen gas contains a small amount of non-condensable hydrogen chloride gas), the temperature of the impurity gases is-40.8 ℃, the air pressure is 0.885MpaG, the impurity gases in the second condenser 9 are output from an eighth air outlet 92, enter the second heat exchanger 8 from a seventh air inlet 83 of the second heat exchanger 8, carry out heat exchange with the impurity-containing hydrogen chloride gas compressed in the second heat exchanger 8, heat the impurity gases, the impurity gases after heating and pressure reduction are sent into the synthesis furnace for recycling from a seventh air outlet 84 of the second heat exchanger 8, the temperature of the output impurity gases is 25 ℃, the air pressure is 0.878MpaG, and simultaneously, the temperature of the impurity-containing hydrogen chloride gas entering the second heat exchanger 8 from the compressor is reduced, so that the temperature of the impurity-containing hydrogen chloride gas entering the first condenser from the second heat exchanger 8 is reduced to-33.95 DEG C (ii) a The hydrogen chloride liquid in the second condenser 9 is output from the second liquid outlet 95 and enters the rectifying tower 10 from the liquid inlet 103 of the rectifying tower, the hydrogen chloride liquid is contacted with the hydrogen chloride gas containing impurities, the hydrogen chloride gas in the gas phase is transferred into the hydrogen chloride liquid, the hydrogen dissolved in the hydrogen chloride liquid in the liquid phase is transferred into the gas phase, the hydrogen chloride liquid is output from the liquid outlet 104 of the rectifying tower after being stripped, the temperature of the hydrogen chloride liquid is raised through the reboiler 12, the hydrogen dissolved in the hydrogen chloride liquid is separated and returned to the rectifying tower 10, the hydrogen chloride liquid is decompressed through the control valve 11 and returns to the shell pass of the first condenser 7 from the fifth liquid inlet 73 of the first condenser 7, and the high-purity hydrogen chloride liquid is vaporized to form low-temperature hydrogen chloride gas under the combined action of decompression and the hydrogen chloride gas containing impurities and introduced into the first condenser 7 from the compressor, the temperature of the low-temperature hydrogen chloride gas is-33.99 ℃, and the air pressure is 0.89 MpaG;
(4) the high-purity hydrogen chloride liquid absorbs heat in the vaporization process, the high-purity hydrogen chloride in the vaporization process is used as a refrigerant to cool the high-pressure impurity-containing hydrogen chloride gas in the first condenser 7, the hydrogen chloride gas is liquefied, the high-purity hydrogen chloride liquid is output from the first liquid outlet 75 and enters the rectifying tower 10 from the liquid inlet 103 of the rectifying tower, the impurity-containing hydrogen chloride gas is used for carrying out gas treatment on the hydrogen chloride liquid (the principle is the same as that in the step (3), the step is not elaborated in detail), the impurity gas dissolved in the hydrogen chloride liquid is further removed through the reboiler 12, the high-purity hydrogen chloride liquid is decompressed through the control valve 11 and returns to the first condenser 7 from the fifth liquid inlet 73 for heat exchange, and the steps are repeated, and the first condenser 7 is continuously cooled; part of the unliquefied gas in the hydrogen chloride gas containing impurities enters a second condenser 9 for continuous cooling and condensation;
(5) the high-purity hydrogen chloride gas obtained by vaporizing the high-purity hydrogen chloride for the refrigerant, which is returned to the first condenser 7 from the fifth liquid inlet 73, is output from the fifth gas outlet 74, is returned to the first heat exchanger 6 from the third gas inlet 63 of the first heat exchanger 6, exchanges heat with the hydrogen chloride gas containing impurities compressed in the first heat exchanger 6, heats the high-purity hydrogen chloride gas to reach the temperature required for industrial use, and is output from the third gas outlet 64 of the first heat exchanger 6, wherein the temperature of the high-purity hydrogen chloride gas is 48 ℃ and the gas pressure is 0.8789 MpaG; meanwhile, the low-temperature high-purity hydrogen chloride gas cools the high-pressure impurity-containing hydrogen chloride gas in the first condenser 7 to-33.95 ℃, and the air pressure of the impurity-containing hydrogen chloride gas is 0.894 MpaG.
In this example, the rectifying column 10 and the reboiler 12 are added to example 1, and this example can reduce the cost of purifying hydrogen chloride and contribute to improving the purity of hydrogen chloride as compared with example 1.
Example 3
The hydrogen chloride gas in this embodiment is obtained by burning chlorine and hydrogen in a synthesis furnace, and since excess hydrogen needs to be introduced in the process of synthesizing the hydrogen chloride gas, the impurity gas in the synthesized hydrogen chloride gas mainly refers to hydrogen, and the hydrogen content is about 6%, and of course, the hydrogen chloride gas also contains a trace amount of water vapor and other gases. This example illustrates the present invention by taking the removal of hydrogen and water vapor from the synthesis hydrogen chloride gas as an example. It should be noted that, when removing other impurity gases, only the temperature and pressure parameters need to be changed, and the method can also be realized.
Referring to fig. 9, the hydrogen chloride dry purification system according to the present embodiment includes a drying device, a compressor 5, a first heat exchanger 6, a first condenser 7, a second heat exchanger 8, a second condenser 9, a rectifying tower 10, and a third heat exchanger 13.
The drying device is used for removing trace water vapor in the synthetic hydrogen chloride gas and comprises a drying cooler 1, a sulfuric acid drying tower 2 and a gas demister 4 which are sequentially connected. The drying cooler 1 liquefies the water vapor by cooling to form water drops, and part of hydrogen chloride gas is dissolved in the water to form hydrochloric acid, so that the bottom of the drying cooler 1 is connected with a condensed acid tank 11 for collecting the part of hydrochloric acid; the sulfuric acid drying tower 2 absorbs water vapor through sulfuric acid, and the sulfuric acid absorbs the water vapor to generate a large amount of heat and generate sulfuric acid mist, so that the sulfuric acid drying tower 2 is provided with a cooler 21 for cooling, the sulfuric acid drying tower 2 is cooled through the cooler 21, the sulfuric acid drying tower 2 is protected, and the gas demister 4 can be used for removing the sulfuric acid mist; the temperature of the gas output from the top of the sulfuric acid drying tower 2 reaches about 18 ℃, and a 2-stage cooling condenser 3 is arranged between the sulfuric acid drying tower 2 and the gas demister 4 for protecting the gas demister 4 and the compressor 5 and is used for cooling the hydrogen chloride gas containing impurities.
Referring to fig. 2 and 3, the compressor 5 is provided with a first gas inlet 51 and a first gas outlet 52 which are communicated with each other, the first gas inlet 51 is connected with a drying device, hydrogen chloride gas containing impurity gas enters the compressor 5 from the first gas inlet 51 after being dried, and the compressor 5 compresses the gas to 0.9 Mpa.
Referring to fig. 2 and 4, the first heat exchanger 6 is provided with a second inlet 61 and a second outlet 62 which are communicated with each other, and a third inlet 63 and a third outlet 64 which are communicated with each other, wherein the second inlet 61 is communicated with the first outlet 52 of the compressor 5.
Referring to fig. 2 and 6, the second heat exchanger 8 is provided with a sixth gas inlet 81 and a sixth gas outlet 82 which are communicated with each other, and a seventh gas inlet 83 and a seventh gas outlet 84 which are communicated with each other, wherein the sixth gas inlet 81 is communicated with the first gas outlet 52 of the compressor 5.
Referring to fig. 2 and 8, the rectifying tower 10 includes a rectifying tower gas inlet 101, a rectifying tower gas outlet 102, a rectifying tower liquid inlet 103 and a rectifying tower liquid outlet 104, the second gas outlet 62 of the first heat exchanger 6 and the sixth gas outlet 82 of the second heat exchanger 8 are both communicated with the rectifying tower gas inlet 101, and the rectifying tower gas outlet 102 is communicated with the fourth gas inlet 71 of the first condenser 7.
The third heat exchanger 13 includes a first channel and a second channel, two ends of the first channel are respectively communicated with the compressor 5 and the rectifying tower 10, one end of the second channel is connected with a refrigerant discharge port 94 of the second condenser 9, and the other end is used for recovering the refrigerant and is connected with the refrigerating unit.
Referring to fig. 2 and 5, the first condenser 7 is provided with a fourth gas inlet 71, a fourth gas outlet 72 and a first liquid outlet 75 which are communicated with each other, and a fifth liquid inlet 73 and a fifth gas outlet 74 which are communicated with each other, the first liquid outlet 75 is communicated with the liquid inlet 103 of the rectifying tower through a liquid pipeline, and the fifth gas outlet 74 is communicated with the third gas inlet 63 of the first heat exchanger 6.
Referring to fig. 2 and 7, the second condenser 9 is provided with an eighth air inlet 91, an eighth air outlet 92 and a second liquid outlet 95 which are communicated with each other, and a refrigerant inlet 93 and a refrigerant outlet 94 for inputting and outputting an external refrigerant, the eighth air inlet 91 is communicated with the fourth air outlet 72 of the first condenser 7, the second liquid outlet 95 is communicated with the liquid inlet 103 of the rectifying tower through a liquid pipeline, and the eighth air outlet 92 is communicated with the seventh air inlet 83 of the second heat exchanger 8.
Referring to fig. 2, the rectification column outlet 104 is connected to the fifth inlet 74 of the first condenser 7 via a pipe and a control valve 11 provided on the pipe. The principle of the rectifying tower 10 is that the components in the mixture have different volatilities, that is, the vapor pressure of each component at the same temperature is different, so that the light component in the liquid phase is transferred to the gas phase, and the heavy component in the gas phase is transferred to the liquid phase, thereby realizing the separation of the rectifying tower. Rectifying column 10 is still furnished with reboiler 12, the bottom and the rectifying column liquid outlet 104 of reboiler 12 are connected, the inside intercommunication of gas pipeline and rectifying column 10 is passed through at the top of reboiler 12, reboiler 12 passes through the high principle of hydrogen chloride boiling point than gaseous boiling point of impurity, with hydrogen chloride liquid heat-up to between impurity boiling point and the hydrogen chloride boiling point for gaseous impurity vaporizes and with hydrogen chloride liquid separation, and then makes the purity of hydrogen chloride liquid higher.
The third gas outlet 64 is used for outputting purified hydrogen chloride gas, and the seventh gas outlet 84 is used for outputting treated tail gas, i.e. hydrogen gas and a small amount of noncondensable hydrogen chloride gas.
The hydrogen chloride dry purification method based on the system comprises the following steps:
(1) the temperature of the synthesized hydrogen chloride gas containing impurities is 45-55 ℃, the hydrogen chloride gas containing impurities is dried by a drying cooler 1 and a sulfuric acid drying tower 2 in sequence, the temperature of the hydrogen chloride gas containing impurities after drying is 16 ℃, the air pressure is 0.052MPaG, and the drying treatment comprises the following specific steps:
(1.1) introducing hydrogen chloride gas containing impurity gas into a drying cooler 1, separating part of water vapor from the hydrogen chloride gas containing impurity gas due to temperature reduction and liquefaction of the drying cooler 1 in a cooling mode, and allowing liquid water to flow into a condensed acid tank 11 along the inner wall of the drying cooler 1;
(1.2) introducing the hydrogen chloride gas containing the impurity gas obtained in the step (1.1) into a sulfuric acid drying tower 2, wherein the sulfuric acid drying tower 2 absorbs water vapor through sulfuric acid, and a large amount of heat and sulfuric acid mist are generated in the process that the sulfuric acid absorbs the water vapor, so that the sulfuric acid drying tower 2 is cooled by matching with a cooler 21, and the dried gas is cooled by matching with a 2-stage cooling condenser;
and (1.3) introducing the hydrogen chloride gas containing the impurity gas obtained in the step (1.2) into a gas demister 4 to remove sulfuric acid mist generated when the sulfuric acid drying tower 2 absorbs water vapor.
(2) The hydrogen chloride gas containing the impurities after being dried by the drying device enters a compressor 5 for compression treatment, the air pressure of the hydrogen chloride gas containing the impurities is increased from 0.05-0.06 Mpa to 0.9MpaG, and the boiling point of the hydrogen chloride gas is further increased, at the moment, the boiling point of the hydrogen chloride gas is increased from-85 ℃ to-33 ℃, and the boiling point of the hydrogen gas is-259.2 ℃; in the process of compressing the hydrogen chloride gas containing impurities, the temperature of the hydrogen chloride gas containing impurities is raised to 42 ℃;
(3) the compressed hydrogen chloride gas containing impurities is output from the first gas outlet 51, part of the hydrogen chloride gas containing impurities is introduced into the first heat exchanger 6 from the second gas inlet 61, part of the hydrogen chloride gas containing impurities is introduced into the second heat exchanger 8 from the sixth gas inlet 81, and part of the hydrogen chloride gas containing impurities is introduced into the third heat exchanger; the hydrogen chloride gas containing impurities in the first heat exchanger 6, the second heat exchanger 8 and the third heat exchanger 13 is all introduced into the rectifying tower 10, the hydrogen chloride gas containing impurities is output from a gas outlet 102 of the rectifying tower and enters the first condenser 7 from a fourth gas inlet 71 of the first condenser 7, the hydrogen chloride gas containing impurities in the first condenser 7 is completely output from a fourth gas outlet 72 because the first condenser 7 is not introduced with a refrigerant, the hydrogen chloride gas containing impurities in the first condenser 7 is introduced into the second condenser 9 from an eighth gas inlet 91 of the second condenser 9, the refrigerant from a refrigerating unit is input from a refrigerant inlet 93 into the second condenser 9, the temperature of the refrigerant is-80 ℃, the refrigerant is output from a refrigerant outlet 94, the output refrigerant is introduced into the third heat exchanger 13 again to carry out heat exchange with the hydrogen chloride gas containing impurities in the third heat exchanger 13, so that part of the hydrogen chloride gas subsequently introduced into the third heat exchanger 13 is liquefied, the liquefied hydrogen chloride liquid enters a rectifying tower 10 and then flows downwards, and is output from a rectifying tower liquid outlet 104, impurity gas and uncondensed hydrogen chloride gas are output to a first condenser 7 from a rectifying tower gas outlet 102, and a refrigerant is recovered to a refrigerating unit; further, the high-pressure hydrogen chloride gas containing impurities in the second condenser 9 and the third heat exchanger 13 is cooled through a refrigerant, so that the hydrogen chloride gas in the high-pressure hydrogen chloride gas is liquefied to form hydrogen chloride liquid, wherein the temperature of the hydrogen chloride liquid is-57 ℃, and the pressure is 0.879 MpaG; the impurity gas such as hydrogen in the second condenser 9 still exists in the form of gas (the hydrogen contains a small amount of noncondensable hydrogen chloride gas), the temperature of the impurity gas is-40.8 ℃, the air pressure is 0.885MpaG, the impurity gas in the second condenser 9 is output from the eighth air outlet 92, enters the second heat exchanger 8 from the seventh air inlet 83 of the second heat exchanger 8, exchanges heat with the impurity-containing hydrogen chloride gas compressed in the second heat exchanger 8, heats the impurity gas, the heated and decompressed impurity gas is sent into the synthesis furnace for recycling from the seventh air outlet 84 of the second heat exchanger 8, the temperature of the output impurity gas is 25 ℃, and the air pressure is 0.878 MpaG; meanwhile, the temperature of the hydrogen chloride gas containing impurities entering the second heat exchanger 8 from the compressor is reduced, so that the temperature of the hydrogen chloride gas containing impurities entering the first condenser from the second heat exchanger 8 is reduced to-33.95 ℃. The hydrogen chloride liquid in the second condenser 9 is output from the second liquid outlet 95, enters the rectifying tower 10 from the liquid inlet 103 of the rectifying tower, and is merged with the hydrogen chloride liquid output from the third heat exchanger 13, in the rectifying tower 10, the hydrogen chloride liquid is contacted with the hydrogen chloride gas containing impurities, the hydrogen chloride gas in the gas phase is transferred into the hydrogen chloride liquid, the hydrogen dissolved in the hydrogen chloride liquid in the liquid phase is transferred into the gas phase, the hydrogen chloride liquid is output from the liquid outlet 104 of the rectifying tower after being stripped, the temperature of the hydrogen chloride liquid is raised through the reboiler 12, the hydrogen dissolved in the hydrogen chloride liquid is separated and returned to the rectifying tower 10, the hydrogen chloride liquid is decompressed through the control valve 11 and then returned to the shell pass of the first condenser 7 from the fifth liquid inlet 73 of the first condenser 7, under the combined action of decompression and heat exchange with the hydrogen chloride gas containing impurities and introduced into the first condenser 7 from the compressor, vaporizing the high-purity hydrogen chloride liquid to form low-temperature hydrogen chloride gas, wherein the temperature of the low-temperature hydrogen chloride gas is-33.99 ℃, and the air pressure is 0.89 MpaG;
(4) the high-purity hydrogen chloride liquid absorbs heat in the vaporization process, the high-purity hydrogen chloride in the vaporization process is used as a refrigerant to cool the high-pressure impurity-containing hydrogen chloride gas in the first condenser 7, the hydrogen chloride gas is liquefied, the high-purity hydrogen chloride liquid is output from the first liquid outlet 75 and enters the rectifying tower 10 from the liquid inlet 103 of the rectifying tower, the impurity-containing hydrogen chloride gas is used for carrying out gas treatment on the hydrogen chloride liquid (the principle is the same as that in the step (3), the step is not elaborated in detail), the impurity gas dissolved in the hydrogen chloride liquid is further removed through the reboiler 12, the high-purity hydrogen chloride liquid is decompressed through the control valve 11 and returns to the first condenser 7 from the fifth liquid inlet 73 for heat exchange, and the steps are repeated, and the first condenser 7 is continuously cooled; part of the unliquefied gas in the hydrogen chloride gas containing impurities enters a second condenser 9 for continuous cooling and condensation;
(5) the high-purity hydrogen chloride gas obtained by vaporizing the high-purity hydrogen chloride for the refrigerant, which is returned to the first condenser 7 from the fifth liquid inlet 73, is output from the fifth gas outlet 74, is returned to the first heat exchanger 6 from the third gas inlet 63 of the first heat exchanger 6, exchanges heat with the hydrogen chloride gas containing impurities compressed in the first heat exchanger 6, heats the high-purity hydrogen chloride gas to reach the temperature required for industrial use, and is output from the third gas outlet 64 of the first heat exchanger 6, wherein the temperature of the high-purity hydrogen chloride gas is 48 ℃ and the gas pressure is 0.8789 MpaG; meanwhile, the low-temperature high-purity hydrogen chloride gas cools the high-pressure impurity-containing hydrogen chloride gas in the first condenser 7 to-33.95 ℃, and the air pressure of the impurity-containing hydrogen chloride gas is 0.894 MpaG.
The present invention has been described in detail with reference to the embodiments, but the description is only for the preferred embodiments of the present invention and should not be construed as limiting the scope of the present invention. All equivalent changes and modifications made within the scope of the present invention shall fall within the scope of the present invention.

Claims (15)

1. A hydrogen chloride dry purification method is characterized in that: which comprises the following steps:
1) drying the hydrogen chloride gas containing the impurity gas to remove water vapor in the hydrogen chloride gas;
2) pressurizing the hydrogen chloride gas obtained in the step 1) to 0.4-1.0MpaG, cooling and condensing to liquefy the hydrogen chloride gas therein to form high-purity hydrogen chloride liquid, keeping impurity gas in a gaseous state, and separating the gas from the liquid;
3) the liquid hydrogen chloride is sent to a first condenser through a control valve, and the liquid hydrogen chloride is vaporized into gas to be output.
2. The dry purification process of hydrogen chloride according to claim 1, characterized in that: the step 3) is specifically as follows:
3) and (2) decompressing the hydrogen chloride liquid through a control valve, allowing the hydrogen chloride liquid to enter a shell pass of a first condenser, vaporizing the high-purity hydrogen chloride liquid to form low-temperature hydrogen chloride gas under the combined action of decompression and heat exchange with hydrogen chloride gas containing impurity gas in a tube pass of the first condenser, simultaneously cooling and condensing the hydrogen chloride gas pressurized in the step 1) by utilizing the principle of vaporization and heat absorption of the high-purity hydrogen chloride liquid, and then outputting the hydrogen chloride gas.
3. The dry purification process of hydrogen chloride according to claim 2, characterized in that: which comprises the following steps:
(1) drying the hydrogen chloride gas containing impurities by a drying device to remove water vapor in the hydrogen chloride gas;
(2) the hydrogen chloride gas enters a compressor to be compressed to 0.4-1.0MpaG, and the boiling point of the hydrogen chloride gas is increased;
(3) introducing the compressed hydrogen chloride gas containing impurities into a first condenser, introducing the hydrogen chloride gas containing impurities in the first condenser into a second condenser through a fourth gas outlet of the first condenser and an eighth gas inlet of the second condenser, reducing the temperature of the hydrogen chloride gas containing impurities by the second condenser through a refrigerant, liquefying the hydrogen chloride gas to form high-purity hydrogen chloride liquid, and outputting the impurity gas from an eighth gas outlet of the second condenser; the high-purity hydrogen chloride liquid is decompressed by a control valve and enters the shell pass of a first condenser, and under the combined action of decompression and heat exchange with the impurity-containing hydrogen chloride gas introduced into the first condenser from a compressor, the high-purity hydrogen chloride liquid is vaporized to form low-temperature hydrogen chloride gas;
(4) the high-purity hydrogen chloride liquid absorbs heat in the vaporization process, the high-purity hydrogen chloride in the vaporization process is used as a refrigerant to cool the hydrogen chloride gas containing impurities in the first condenser, the high-pressure hydrogen chloride gas in the first condenser is liquefied to form high-purity hydrogen chloride liquid, the high-purity hydrogen chloride liquid returns to the first condenser through the control valve to carry out heat exchange, and part of non-liquefied gas in the hydrogen chloride gas containing impurities enters the second condenser in a gas form to be cooled and condensed continuously;
(5) the hydrogen chloride vaporized after returning to the first condenser is output from the first condenser in the form of a gas.
4. The dry purification process of hydrogen chloride according to claim 3, characterized in that: in the step (2), in the compression process, the temperature of the hydrogen chloride gas containing impurities is raised to generate heat, and part of the compressed hydrogen chloride gas containing impurities is firstly introduced into the first heat exchanger and part of the compressed hydrogen chloride gas containing impurities is introduced into the second heat exchanger;
in the step (3), the compressed hydrogen chloride gas containing impurities in the first heat exchanger and the second heat exchanger is introduced into a first condenser;
returning the impurity gas output from the eighth gas outlet of the second condenser in the step (3) to the second heat exchanger from the seventh gas inlet of the second heat exchanger, performing heat exchange with the impurity-containing hydrogen chloride gas compressed in the second heat exchanger, heating the impurity gas, and sending the heated impurity gas into the synthesis furnace from the seventh gas outlet of the second heat exchanger for reuse;
and (5) returning the high-purity hydrogen chloride gas output from the fifth gas outlet of the first condenser to the first heat exchanger from the third gas inlet of the first heat exchanger, performing heat exchange with the impurity-containing hydrogen chloride gas compressed in the first heat exchanger, heating the high-purity hydrogen chloride gas to reach the temperature required by industrial use, and outputting the high-purity hydrogen chloride gas from the third gas outlet of the first heat exchanger.
5. The dry purification process of hydrogen chloride according to claim 4, characterized in that: introducing the hydrogen chloride gas containing impurities in the first heat exchanger and the second heat exchanger in the step (3) into a rectifying tower before introducing the hydrogen chloride gas into the first condenser; and (3) the hydrogen chloride liquefied in the step (3) and the step (4) also passes through the rectifying tower before entering the control valve for pressure reduction, and impurities dissolved in the hydrogen chloride liquid are stripped by the hydrogen chloride gas containing the impurities, so that the purity of the hydrogen chloride liquid is higher.
6. The dry purification process of hydrogen chloride according to claim 4, characterized in that: the method is characterized in that in the step (2), part of the compressed hydrogen chloride gas containing impurities is introduced into a third heat exchanger, the refrigerant used for carrying out heat exchange on the second condenser in the step (3) is introduced into the third heat exchanger before being recovered, and exchanges heat with the hydrogen chloride gas containing the impurity gas of the third heat exchanger to liquefy part of the hydrogen chloride in the third heat exchanger, the hydrogen chloride liquid, the uncondensed hydrogen chloride gas and the impurity gas enter a rectifying tower, the liquefied hydrogen chloride gas is output from a liquid outlet of the rectifying tower and enters a shell pass of the first condenser through a control valve for decompression so as to be vaporized, and low-temperature hydrogen chloride gas is formed; outputting the uncondensed hydrogen chloride gas and the impurity gas from a gas outlet of a rectifying tower of the rectifying tower, entering the first condenser from a fourth gas inlet of the first condenser, and continuously liquefying in the manner of the steps (3) and (4).
7. The dry purification process of hydrogen chloride according to claim 5, characterized in that: in the step (3) and the step (4), before the hydrogen chloride liquid enters the control valve from the rectifying tower for pressure reduction, the temperature of the hydrogen chloride liquid is also raised through a reboiler, and impurities dissolved in the hydrogen chloride liquid are separated and returned to the rectifying tower.
8. The dry purification process of hydrogen chloride according to claim 1, characterized in that: the specific steps of drying the hydrogen chloride gas containing the impurity gas in the step 1) are as follows:
(1.1) introducing the hydrogen chloride gas containing the impurity gas into a drying cooler, and cooling the hydrogen chloride gas containing the impurity gas to ensure that part of water vapor is liquefied due to cooling and separated from the hydrogen chloride gas containing the impurity gas;
(1.2) introducing the hydrogen chloride gas containing the impurity gas obtained in the step (1.1) into a sulfuric acid drying tower, and absorbing water vapor by using concentrated sulfuric acid in the sulfuric acid drying tower;
and (1.3) introducing the hydrogen chloride gas containing the impurity gas obtained in the step (1.2) into a gas demister to remove sulfuric acid mist generated when a sulfuric acid drying tower absorbs water vapor.
9. A hydrogen chloride dry purification system is characterized in that: the system comprises a drying device, a compressor, a first heat exchanger, a first condenser, a second heat exchanger and a second condenser; the compressor is provided with a first air inlet and a first air outlet which are communicated with each other, and the first air inlet is connected with the drying device;
the first heat exchanger is provided with a second air inlet and a second air outlet which are communicated with each other, and a third air inlet and a third air outlet which are communicated with each other, wherein the second air inlet is communicated with the first air outlet of the compressor;
the first condenser is provided with a fourth air inlet, a fourth air outlet and a first liquid outlet which are communicated with each other, and a fifth liquid inlet and a fifth air outlet which are communicated with each other, the fourth air inlet is communicated with the second air outlet of the first heat exchanger, the first liquid outlet is communicated with the fifth liquid inlet through a pipeline and a control valve arranged on the pipeline, and the fifth air outlet is communicated with the third air inlet of the first heat exchanger;
the second heat exchanger is provided with a sixth air inlet and a sixth air outlet which are communicated with each other, and a seventh air inlet and a seventh air outlet which are communicated with each other, the sixth air inlet is communicated with the first air outlet of the compressor, and the sixth air outlet is communicated with the fourth air inlet of the first condenser;
the second condenser is provided with an eighth air inlet, an eighth air outlet and a second liquid outlet which are communicated with each other, and a refrigerant feeding hole and a refrigerant discharging hole which are used for inputting and outputting external refrigerants;
the third gas outlet is used for outputting the purified hydrogen chloride gas, and the seventh gas outlet is used for outputting the processed impurity gas.
10. The hydrogen chloride dry purification system according to claim 9, characterized in that: the drying device comprises a drying cooler, a sulfuric acid drying tower and a gas demister which are connected in sequence.
11. The hydrogen chloride dry purification system according to claim 10, characterized in that: the bottom of the drying cooler is connected with a condensed acid tank, and the sulfuric acid drying tower is provided with a cooler for cooling.
12. The hydrogen chloride dry purification system according to claim 10, characterized in that: and a plurality of cooling condensers are also arranged between the gas demister and the sulfuric acid drying tower.
13. The hydrogen chloride dry purification system according to claim 9, characterized in that: it still includes the rectifying column, the rectifying column includes the rectifying column air inlet, the rectifying column gas outlet, rectifying column inlet and rectifying column liquid outlet, first heat exchanger's second gas outlet and second heat exchanger's sixth gas outlet all communicate with the rectifying column air inlet, the rectifying column gas outlet communicates with the fourth air inlet of first condenser, the first liquid outlet of first condenser and the second liquid outlet of second condenser all communicate with the rectifying column inlet, the rectifying column liquid outlet passes through the pipeline and sets up the fifth inlet intercommunication of control valve on the pipeline and first condenser on the pipeline.
14. The hydrogen chloride dry purification system according to claim 13, characterized in that: the heat exchanger further comprises a third heat exchanger, the third heat exchanger comprises a first channel and a second channel, two ends of the first channel are respectively communicated with the compressor and the rectifying tower, one end of the second channel is connected with a refrigerant discharge hole of the second condenser, and the other end of the second channel is used for recovering refrigerants.
15. The hydrogen chloride dry purification system according to claim 13, characterized in that: the rectifying tower is also provided with a reboiler, the bottom of the reboiler is connected with a liquid outlet of the rectifying tower, and the top of the reboiler is communicated with the inside of the rectifying tower through a gas pipeline.
CN202110485956.5A 2021-05-01 2021-05-01 Hydrogen chloride dry purification method and system Pending CN113144812A (en)

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