CN113955723A - Rectification separation purification method and system for gas containing hydrogen chloride sulfur dioxide - Google Patents
Rectification separation purification method and system for gas containing hydrogen chloride sulfur dioxide Download PDFInfo
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- CN113955723A CN113955723A CN202111290949.6A CN202111290949A CN113955723A CN 113955723 A CN113955723 A CN 113955723A CN 202111290949 A CN202111290949 A CN 202111290949A CN 113955723 A CN113955723 A CN 113955723A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B17/00—Sulfur; Compounds thereof
- C01B17/48—Sulfur dioxide; Sulfurous acid
- C01B17/50—Preparation of sulfur dioxide
- C01B17/56—Separation; Purification
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B7/00—Halogens; Halogen acids
- C01B7/01—Chlorine; Hydrogen chloride
- C01B7/07—Purification ; Separation
- C01B7/0706—Purification ; Separation of hydrogen chloride
- C01B7/0712—Purification ; Separation of hydrogen chloride by distillation
Abstract
The application discloses a rectification separation and purification method and a rectification separation and purification system for a gas containing hydrogen chloride sulfur dioxide, wherein the method comprises the steps of compressing and cooling the gas containing the hydrogen chloride sulfur dioxide; cooling the compressed and cooled sulfur dioxide gas containing hydrogen chloride by a second cooler to form gas and condensate; and (3) carrying out light weight removal and heavy weight removal rectification separation on the cooled gas and condensate to obtain pure hydrogen chloride and sulfur dioxide. Can avoid producing a large amount of washing waste water and waste salt, separate and recycle hydrogen chloride and sulfur dioxide in the production tail gas, obtain high-purity high-value by-products.
Description
Technical Field
The application relates to chemical equipment, in particular to a rectification separation and purification method and a rectification separation and purification system for a gas containing hydrogen chloride and sulfur dioxide.
Background
In the field of pharmaceutical chemistry, chlorination and sulfonation are common reaction sections. The reaction tail gas is a mixed gas containing a large amount of hydrogen chloride, sulfur dioxide, various organic solvents and trace moisture, the existing process is usually carried out washing treatment by adopting a water washing and alkali washing process, although the treatment effect can meet the emission requirement, a large amount of waste water and waste salt are generated, the utilization rate of raw materials of organic reaction is greatly reduced by failing to recycle effective components in the waste gas, and therefore a safe, environment-friendly and economic continuous hydrogen chloride, sulfur dioxide and trace high-boiling gas separation and recovery process is needed.
Disclosure of Invention
The present application is directed to solving at least one of the problems in the prior art. Therefore, the invention provides a rectification separation purification method of sulfur dioxide gas containing hydrogen chloride, which has high recovery rate of hydrogen fluoride and can obtain high-purity products for recycling or serving as byproducts.
In order to solve the technical problem, the following technical scheme is adopted in the application: a method for rectifying, separating and purifying a gas containing hydrogen chloride sulfur dioxide comprises the steps of compressing and cooling the gas containing hydrogen chloride sulfur dioxide; cooling the compressed and cooled sulfur dioxide gas containing hydrogen chloride by a second cooler to form gas and condensate; and (3) carrying out light weight removal and heavy weight removal rectification separation on the cooled gas and condensate to obtain pure hydrogen chloride and sulfur dioxide.
The improvement comprises compressing and cooling the sulfur dioxide gas containing hydrogen chloride by a compressor, wherein the compressed pressure of the sulfur dioxide gas containing hydrogen chloride is 0.5-2.0 Mpa, and the compressed temperature is 60-150 ℃; cooling the compressed and cooled sulfur dioxide gas containing hydrogen chloride to-15-50 ℃ through a second cooler to form cooled gas and condensate; dehydrochlorination is carried out on the cooled gas and condensate through a light component removal device, the light component removal device comprises a light component removal tower, a condenser and a first reboiler, the operating pressure of the light component removal tower is controlled to be 0.5-2.0 MPa, the tower top temperature of the light component removal tower is controlled to be-50-10 ℃, the tower kettle temperature of the light component removal tower is controlled to be 35-85 ℃, and the tower top reflux ratio of the light component removal tower is controlled to be 0.2-5.
In the improvement, the method comprises washing the gas containing hydrogen chloride sulfur dioxide to remove the rest high boilers and trace water in the gas before the gas containing hydrogen chloride sulfur dioxide is compressed and cooled.
If the mixed gas contains the rest high boiling substances or trace water before compression, the hydrogen chloride-containing sulfur dioxide gas can be selectively washed by washing equipment to remove the rest high boiling substances and trace water in the gas before the hydrogen chloride-containing sulfur dioxide gas is compressed and cooled, wherein the washing equipment comprises a washing tower, a circulating pump and a first cooler, and washing liquid is cooled to-15 ℃ by the first cooler and then enters the washing tower to wash the hydrogen chloride-containing sulfur dioxide gas.
In the improvement, the hydrogen chloride-containing sulfur dioxide gas also comprises high-boiling gas, and the method comprises the steps of removing light components from the gas and condensate to obtain pure hydrogen chloride and a heavy component containing sulfur dioxide, and removing heavy components containing sulfur dioxide to obtain pure sulfur dioxide and a high-boiling solvent.
In the method, the gas and the condensate are subjected to lightness removal to obtain pure hydrogen chloride and a heavy component containing sulfur dioxide, the heavy component containing sulfur dioxide is subjected to weight removal through a weight removal device to obtain pure sulfur dioxide and a high-boiling solvent, the weight removal device comprises a weight removal tower, a third cooler and a second reboiler, the operating pressure of the weight removal tower is controlled to be 0.5-2.0 MPa, the tower top temperature of the weight removal tower is controlled to be 30-85 ℃, and the tower kettle temperature of the weight removal tower is determined according to the physical properties of the high-boiling gas.
The application still provides a rectification separation purification system that contains hydrogen chloride sulfur dioxide gas, including compressor, second cooler, liquid phase buffer tank and lightness-removing equipment, lightness-removing equipment is including taking off light tower, condenser and first reboiler again, the export of compressor is linked together with the import of second cooler, the export of second cooler is linked together with the import of liquid phase buffer tank, the export of liquid phase buffer tank is linked together with the import of taking off the light tower, it includes gaseous phase export and liquid phase export to take off the light tower, the gaseous phase export of taking off the light tower is linked together with the condenser, the liquid phase export of taking off the light tower is linked together with first reboiler again.
The improved washing system further comprises washing equipment, the washing equipment comprises a washing tower, a circulating pump and a first cooler, the washing tower comprises a gas phase inlet, a gas phase outlet, a washing liquid inlet and a washing liquid outlet, the gas phase outlet of the washing tower is communicated with the inlet of the compressor, the washing liquid inlet of the washing tower is communicated with the outlet of the first cooler, the washing liquid outlet of the washing tower is communicated with the inlet of the circulating pump, the outlet of the circulating pump is communicated with the inlet of the first cooler, a washing liquid circulating loop is formed among the washing tower, the circulating pump and the first cooler, and the washing liquid circulating loop is provided with a washing liquid inlet and a washing liquid outlet.
The system further comprises a heavy component removing device, the heavy component removing device comprises a heavy component removing tower, a third cooler and a second reboiler, the heavy component removing tower comprises an inlet, a gas outlet, a liquid phase outlet, a third reflux port A and a fourth reflux port A, the outlet of the first reboiler is communicated with the inlet of the heavy component removing tower, the gas phase outlet of the heavy component removing tower is communicated with the inlet of the third cooler, the third cooler is provided with an outlet and a third reflux port B, the third reflux port B is communicated with the third reflux port A, the liquid phase outlet of the heavy component removing tower is communicated with the inlet of the second reboiler, the second reboiler is provided with an outlet and a fourth reflux port B, and the fourth reflux port B is communicated with the fourth reflux port A.
In an improvement, the condenser comprises a first flow channel, a gas phase outlet of the lightness-removing tower is communicated with an inlet of the first flow channel, the first flow channel is provided with a first reflux opening B, the lightness-removing tower is provided with a first reflux opening A, and the first reflux opening B is communicated with the first reflux opening A; and/or the first reboiler comprises a third flow channel, a liquid phase outlet of the light component removal tower is communicated with an inlet of the third flow channel, the third flow channel is provided with a second reflux port B, the light component removal tower is provided with a second reflux port A, and the second reflux port B is communicated with the second reflux port A.
After adopting above-mentioned technical scheme, this application has following advantage: can avoid producing a large amount of washing waste water and waste salt, separate and recycle hydrogen chloride and sulfur dioxide in the production tail gas, obtain high-purity high-value by-products.
Drawings
The following further describes embodiments of the present application in conjunction with the attached drawings:
fig. 1 is a schematic structural diagram of a gas rectification separation and purification system according to the present application.
Detailed Description
The technical solutions in the embodiments of the present application will be clearly and completely described below with reference to the drawings in the embodiments of the present application, and it is obvious that the described embodiments are only a part of the embodiments of the present application, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present application.
It will be understood that when an element is referred to as being "secured to" or "disposed on" another element, it can be directly on the other element or intervening elements may also be present. When an element is referred to as being "connected" to another element, it can be directly connected to the other element or intervening elements may be present, and in particular, when an element is referred to as being "fixedly connected" to another element, the "fixedly connected" can be non-removably connected, such as by welding, riveting, or the like, or removably connected, such as by threading, snapping, or the like. The terms "vertical," "horizontal," "left," "right," and the like as used herein are for illustrative purposes only and do not represent the only embodiments.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs. The terminology used herein in the description of the present application is for the purpose of describing particular embodiments only and is not intended to be limiting of the application.
The terms "first" and "second" in this application do not denote any particular order or quantity, but rather are used to distinguish one element from another.
The first embodiment is as follows:
the application provides a rectification separation and purification method of a gas containing hydrogen chloride sulfur dioxide, which comprises the steps of washing the gas containing hydrogen chloride sulfur dioxide to remove the rest high wastes and trace water in the gas containing hydrogen chloride sulfur dioxide; compressing and cooling the washed sulfur dioxide gas containing hydrogen chloride; cooling the compressed and cooled sulfur dioxide gas containing hydrogen chloride by a second cooler 5 to form gas and condensate; and removing light components from the gas and the condensate formed by cooling to obtain separated pure hydrogen chloride and sulfur dioxide.
Specifically, the gas containing the sulfur dioxide and the hydrogen chloride is washed by washing equipment to remove other high wastes and trace water in the gas containing the sulfur dioxide and the hydrogen chloride, the washing equipment comprises a washing tower 1, a circulating pump 2 and a first cooler 3, and washing liquid is cooled to-15 ℃ by the first cooler 3 and then enters the washing tower 1 to wash the gas containing the sulfur dioxide and the hydrogen chloride; compressing and cooling the washed sulfur dioxide gas containing hydrogen chloride by a compressor 4, wherein the pressure of the sulfur dioxide gas containing hydrogen chloride after compression and cooling is 0.5-2.0 Mpa, and the temperature is 60-150 ℃; cooling the compressed and cooled sulfur dioxide gas containing hydrogen chloride to-15-50 ℃ through a second cooler 5 to form gas and condensate; buffering the gas and the condensate formed by cooling through a liquid phase buffer tank 6; and (3) removing the light components from the buffered gas and condensate through light component removing equipment, wherein the light component removing equipment comprises a light component removing tower 7, a condenser 8 and a first reboiler 9, the operating pressure of the light component removing tower 7 is controlled to be 0.5-2.0 MPa, the tower top temperature of the light component removing tower 7 is controlled to be-50-10 ℃, the tower kettle temperature of the light component removing tower 7 is controlled to be 35-85 ℃, and the tower top reflux ratio of the light component removing tower 7 is controlled to be 0.2-5.
Of course, if the hydrogen chloride-containing sulfur dioxide gas does not contain high waste and trace amounts of water, it may not be washed.
If the sulfur dioxide gas containing hydrogen chloride also comprises high-boiling gas, the separated gas and condensate are subjected to light weight removal to obtain pure hydrogen chloride and heavy components containing sulfur dioxide, and the heavy components containing sulfur dioxide can be further subjected to heavy weight removal to obtain pure sulfur dioxide and a high-boiling solvent.
Specifically, the heavy component containing sulfur dioxide is subjected to heavy component removal through a heavy component removal device to obtain pure sulfur dioxide and a high-boiling solvent, the heavy component removal device comprises a heavy component removal tower 10, a third cooler 11 and a second reboiler 12, the operating pressure of the heavy component removal tower 10 is controlled to be 0.5-2.0 MPa, the tower top temperature of the heavy component removal tower 10 is controlled to be 30-85 ℃, the tower kettle temperature of the heavy component removal tower 10 is determined according to the physical properties of high-boiling gas, and the tower top reflux ratio of the heavy component removal tower 10 is controlled to be 0.2-5.
Example two:
as shown in fig. 1, the present application provides a rectification separation and purification system for a sulfur dioxide gas containing hydrogen chloride, which comprises a washing device, a compressor 4, a second cooler 5, a liquid phase buffer tank 6, a light component removal device and a heavy component removal device.
Washing equipment includes scrubbing tower 1, circulating pump 2 and first cooler 3, scrubbing tower 1 includes the gaseous phase import, the gaseous phase export, washing liquid import and washing liquid export, the washing liquid import of scrubbing tower 1 is linked together with the export of first cooler 3, the washing liquid export of scrubbing tower 1 is linked together with circulating pump 2's import, circulating pump 2's export is linked together with first cooler 3's import, scrubbing tower 1, form washing liquid circulation circuit between circulating pump 2 and the first cooler 3, washing liquid circulation circuit is equipped with washing liquid import and washing liquid export, the gaseous phase export of scrubbing tower 1 is linked together with compressor 4's import. After the hydrogen chloride, the sulfur dioxide and the trace high-boiling gas are washed by the high-boiling washing tower 1, trace water and various organic solvents in the gas can be removed, the efficiency of subsequent rectification and separation is effectively improved, the problem of corrosion of the whole set of system by the hydrous hydrogen chloride and the sulfur dioxide is avoided, and the corrosion resistance of the whole set of device is improved.
The outlet of the compressor 4 is communicated with the inlet of a second cooler 5, and the outlet of the second cooler 5 is communicated with the inlet of a liquid phase buffer tank 6.
The light component removing equipment comprises a light component removing tower 7, a condenser 8 and a first reboiler 9, an outlet of the liquid phase buffer tank 6 is communicated with an inlet of the light component removing tower, the light component removing tower 7 comprises a gas phase outlet and a liquid phase outlet, the gas phase outlet of the light component removing tower 7 is communicated with the condenser 8, and the liquid phase outlet of the rectifying tower is communicated with the first reboiler 9.
The condenser 8 comprises a first flow channel and a second flow channel, the first flow channel comprises an inlet and an outlet, a gas phase outlet of the lightness-removing tower 7 is communicated with the inlet of the first flow channel, a baffle is arranged at the outlet of the first flow channel, the first flow channel is provided with a first return port B, the lightness-removing tower 7 is provided with a first return port A, the first return port B is communicated with the first return port A, and the first return port B is provided with a liquid collecting bag.
The condenser 8 comprises a shell pass and a tube pass, the tube pass comprises a first flow channel, the shell pass comprises a second flow channel, the system further comprises an adjusting valve for adjusting the liquid level of a medium in the shell pass, the liquid level of the medium in the shell pass is adjusted through the adjusting valve to control the backflow flow of the fluid at the first backflow port B, during work, the backflow ratio of the fluid at the first backflow port B is controlled to be 0.2-5, namely the backflow ratio at the top of the light component removal tower 7 is controlled to be 0.2-5, and the medium in the shell pass is preferably a liquid-phase refrigerant or liquid nitrogen.
As an alternative embodiment, the condenser 8 is a lightness-removing column condenser 8 of the kettle reboiled U tube (BKU) type.
The condenser 8 condenses and reflows hydrogen chloride gas by adopting liquid-phase refrigerant or liquid nitrogen evaporation, the reflow flow is controlled by adjusting the liquid level of the refrigerant, and the refrigerant pipeline adjusting valve participates in cascade linkage.
The first reboiler 9 comprises a third flow channel and a fourth flow channel, the third flow channel comprises an inlet and an outlet, the liquid phase outlet of the lightness-removing tower 7 is communicated with the inlet of the third flow channel, the third flow channel is provided with a second reflux port B, the lightness-removing tower 7 is provided with a second reflux port A, and the second reflux port B is communicated with the second reflux port A.
The medium of the fourth flow channel is steam or heat conducting oil.
The system also comprises an adjusting valve for adjusting the liquid level of the liquid phase fluid in the third flow channel, the liquid level is controlled to be stable by adjusting the opening degree of the adjusting valve, and the liquid is discharged to the hydrogen fluoride storage tank through pressure during high liquid level.
The condenser 8, the first reboiler 9 and the light component removal tower 7 are made of carbon steel, S30408, S30403, S22053, S31603, Monel alloy, Inconel alloy or Hastelloy alloy. As one of the embodiments, the condenser 8, the first reboiler 9, and the light component removal column 7 are made of a column steel-lined carbon steel, S30408, S30403, S22053, S31603, monel, Inconel, and hastelloy.
The heavy component removal equipment comprises a heavy component removal tower 10, a third cooler 11 and a second reboiler 12, the heavy component removal tower 10 comprises an inlet, a gas phase outlet, a liquid phase outlet, a third reflux port A and a fourth reflux port A, the outlet of the first reboiler 9 is communicated with the inlet of the heavy component removal tower 10, the gas phase outlet of the heavy component removal tower 10 is communicated with the inlet of the third cooler 11, the third cooler 11 is provided with an outlet and a third reflux port B, the third reflux port B is communicated with the third reflux port A, the liquid phase outlet of the heavy component removal tower 10 is communicated with the inlet of the second reboiler 12, the second reboiler 12 is provided with an outlet and a fourth reflux port B, and the fourth reflux port B is communicated with the fourth reflux port A.
When the gas scrubbing device works, the gas containing the sulfur dioxide containing the hydrogen chloride is scrubbed by scrubbing equipment to remove other high wastes and trace water in the gas containing the sulfur dioxide containing the hydrogen chloride, the scrubbing solution is sent into a scrubbing solution circulation loop through a scrubbing solution inlet, the scrubbing solution circularly flows in the loop through a circulating pump 2 in the scrubbing solution circulation loop, flows through a first cooler 3, is cooled to-15 ℃ through the first cooler 3, and then enters a scrubbing tower 1 to scrub the gas containing the sulfur dioxide containing the hydrogen chloride; conveying the washed sulfur dioxide gas containing hydrogen chloride to a compressor 4 for compression cooling, wherein the pressure of the sulfur dioxide gas containing hydrogen chloride after compression cooling is 0.5-2.0 Mpa, and the temperature is 60-150 ℃; the gas containing the hydrogen chloride sulfur dioxide is compressed and cooled by a compressor 4, then is input into a second cooler 5 to be further cooled to-15-50 ℃, and is cooled to form gas and condensate; the gas and the condensate formed by cooling are input into a liquid phase buffer tank 6 for buffering and then input into a lightness-removing column 7, the gas flows upwards in the lightness-removing column 7 and is input into a first flow passage of a condenser 8 from a gas phase outlet of the lightness-removing column 7, the gas in the first flow passage exchanges heat with a medium in a second flow passage to be further separated into gas and condensate, the separated gas flows out from an outlet of the first flow passage, the separated condensate flows back to the lightness-removing column 7 from a first return port B, the condensate flows downwards in the lightness-removing column 7 and is input into a third flow passage of a first reboiler 9 from a liquid phase outlet of the lightness-removing column 7, the condensate in the third flow passage exchanges heat with a medium in a fourth flow passage to be further separated into gas and condensate, the separated condensate flows out from an outlet of the third flow passage, the separated gas flows back to the lightness-removing column 7 from a second return port B of the third flow passage, the operating pressure of the lightness-removing column 7 is controlled to be 0.5-2.0 MPa, the temperature of the top of the light component removal tower 7 is controlled to be-50 to-10 ℃ by a condenser 8, the temperature of the bottom of the light component removal tower 7 is controlled to be 35 to 85 ℃ by a first reboiler 9, and the reflux ratio of the top of the light component removal tower 7 is controlled to be 0.2 to 5; inputting the condensate flowing out of the outlet of the third flow passage into a heavy component removal tower 10, controlling the operating pressure of the heavy component removal tower 10 to be 0.5-2.0 MPa, controlling the operating temperature at the top of the tower to be 30-85 ℃ through a third cooler 11, determining the operating temperature of a tower kettle according to the physical property of a high-boiling solvent and controlling the reflux ratio at the top of the heavy component removal tower 10 to be 0.2-5 through a second reboiler 12, separating sulfur dioxide and the high-boiling solvent in the condensate in the heavy component removal tower, gasifying the sulfur dioxide, flowing out of a gas phase outlet at the top of the heavy component removal tower 10 to the third cooler 11, cooling through the third cooler 11 to form liquid-phase sulfur dioxide, extracting the liquid-phase sulfur dioxide from the outlet of the third cooler 11, refluxing the cooled residual gas to the heavy component removal tower 10 through a third reflux port B of the third cooler 11, flowing out of the high-boiling solvent from a liquid phase outlet at the bottom of the heavy component removal tower 10 to the second reboiler 12, heating through the reboiler, the partially vaporized high-boiling solvent is refluxed to the heavy component removal column 10 from the fourth reflux port B of the second reboiler 12, and the unvaporized high-boiling solvent is withdrawn from the outlet of the second reboiler 12. The sulfur dioxide content in the hydrogen chloride extracted by the light component removal equipment can reach below 200ppm, the content of the high-boiling organic solvent can reach below 100ppm, and the recovery rate of the hydrogen chloride is more than or equal to 99%. The content of hydrogen chloride in the sulfur dioxide extracted by the light component removal equipment can reach below 200ppm, the content of high-boiling organic solvent can reach below 100ppm, and the recovery rate of the sulfur dioxide is more than or equal to 99%.
Compared with the prior art, the invention has the following beneficial effects: can avoid producing a large amount of washing waste water and waste salt, separate and recycle hydrogen chloride and sulfur dioxide in the production tail gas, obtain high-purity high-value by-products. Meanwhile, the invention utilizes liquid nitrogen or liquid-phase refrigerant for refrigeration, can adopt a complete set of refrigerating unit to supply the refrigerant for recycling, can also utilize the liquid nitrogen in the factory public engineering station for cold energy recycling, and also has excellent energy-saving effect.
Example three:
the flow rate was 1400Nm3H contains hydrogen chloride, sulfur dioxide and trace amount of high-boiling gas, wherein the high content of the high-boiling gas contains a large amount of thionyl chloride and trace amount of high-boiling dichloroethane. The mixed gas contains 48% of sulfur dioxide (mass fraction, the remainder), 40% of hydrogen chloride, 10% of thionyl chloride, 0.05% of dichloroethane and the balance of non-condensable gases such as nitrogen.
The mixed gas is subjected to a washing tower 1, fresh thionyl chloride is used as a washing agent for cyclic washing, dichloroethane and trace water in the mixed gas are removed, the mixed gas enters a compressor 4 to be compressed to 1.9MPa, and then a second cooler 5 is used for cooling to 0 ℃ and then enters a material feeding section of the lightness-removing tower. And (4) the washed thionyl chloride is sent to a production workshop for recycling.
The pressure of the light component removal tower is controlled to be 1.9MPa, a reboiler (namely a first reboiler 9) of the light component removal tower is heated by 0.6MPa steam, and the material temperature of a tower kettle is controlled to be 85 ℃. The condenser 8 at the top of the tower carries out evaporative refrigeration through R22, the temperature at the top of the tower is controlled at-14 ℃, total reflux is slowly established at the top of the tower, and partial non-condensable gas is discharged to stabilize the pressure of the tower. After the total reflux, the temperature of the tower bottom and the temperature of the tower kettle are stable, sampling from the tower top and detecting that the content of the hydrogen chloride is qualified, and stabilizing the tower pressure by adjusting gas phase discharging. The tower kettle controls the liquid level stability by adjusting the opening degree of the regulating valve, and discharges the liquid to the de-weighting tower 10 by pressure when the liquid level is high. The hydrogen chloride gas containing noncondensable gas and with the sulfur dioxide content lower than 0.1 percent can be obtained at the top of the light component removal tower 7 and is sent to the next working section for further separation or is sent to a film-falling absorption to produce hydrochloric acid as a byproduct.
The operating pressure of the heavy component removal tower 10 is 0.8Mpa, a reboiler (namely a second reboiler 12) of the heavy component removal tower 10 is heated by 0.6Mpa steam, the operating temperature of a tower kettle is 140 ℃, circulating water is adopted for cooling the tower top, and the operating temperature of the tower top is 47 ℃. The content of hydrogen chloride in the sulfur dioxide obtained from the tower top can reach below 100ppm, the content of high-boiling organic solvent can reach below 100ppm, the recovery rate of the sulfur dioxide is more than or equal to 99 percent, and the sulfur dioxide can be recycled on a production line or sold as a byproduct. The thionyl chloride containing a trace amount of sulfur dioxide in the tower bottom is removed to a washing tower 1.
In addition to the preferred embodiments described above, other embodiments of the present application can be devised by those skilled in the art, and various changes and modifications can be made without departing from the spirit of the present application, which is defined by the scope of the appended claims.
Claims (10)
1. A rectification separation and purification method of sulfur dioxide gas containing hydrogen chloride is characterized by comprising the steps of compressing and cooling the sulfur dioxide gas containing hydrogen chloride; cooling the compressed and cooled sulfur dioxide gas containing hydrogen chloride by a second cooler to form gas and condensate; and (3) carrying out light weight removal and heavy weight removal rectification separation on the cooled gas and condensate to obtain pure hydrogen chloride and sulfur dioxide.
2. The method according to claim 1, comprising compressing and cooling the gas containing hydrogen chloride and sulfur dioxide by a compressor, wherein the compressed gas containing hydrogen chloride and sulfur dioxide has a pressure of 0.5-2.0 MPa and a temperature of 60-150 ℃; cooling the compressed and cooled sulfur dioxide gas containing hydrogen chloride to-15-50 ℃ through a second cooler to form cooled gas and condensate; dehydrochlorination is carried out on the cooled gas and condensate through a light component removal device, the light component removal device comprises a light component removal tower, a condenser and a first reboiler, the operating pressure of the light component removal tower is controlled to be 0.5-2.0 MPa, the tower top temperature of the light component removal tower is controlled to be-50-10 ℃, the tower kettle temperature of the light component removal tower is controlled to be 35-85 ℃, and the tower top reflux ratio of the light component removal tower is controlled to be 0.2-5.
3. The method as claimed in claim 1 or 2, characterized in that the method comprises washing the hydrogen chloride-containing sulphur dioxide gas to remove remaining high boilers and traces of water in the gas before the gas is cooled down in compression.
4. The method as set forth in claim 1 or 2, characterized in that if the mixed gas contains the rest of high boiling or trace water before compression, the hydrogen chloride-containing sulfur dioxide gas is optionally washed by a washing device to remove the rest of high boiling substances and trace water in the gas before the hydrogen chloride-containing sulfur dioxide gas is compressed and cooled, wherein the washing device comprises a washing tower, a circulating pump and a first cooler, and the washing liquid is cooled to-15 ℃ by the first cooler and then enters the washing tower to wash the hydrogen chloride-containing sulfur dioxide gas.
5. The process according to claim 1 or 2, wherein the hydrogen chloride-containing sulfur dioxide gas further comprises a high-boiling gas, and the process comprises lightness removing the gas and condensate to obtain pure hydrogen chloride and a sulfur dioxide-containing heavy component, and weight removing the sulfur dioxide-containing heavy component to obtain pure sulfur dioxide and a high-boiling solvent.
6. The method according to claim 1 or 2, wherein the hydrogen chloride-containing sulfur dioxide gas further comprises high-boiling gas, the method comprises the steps of removing light from the gas and condensate to obtain pure hydrogen chloride and heavy components containing sulfur dioxide, removing heavy components containing sulfur dioxide through a heavy removal device to obtain pure sulfur dioxide and high-boiling solvent, the heavy removal device comprises a heavy removal tower, a third cooler and a second reboiler, the operating pressure of the heavy removal tower is controlled to be 0.5-2.0 MPa, the overhead temperature of the heavy removal tower is controlled to be 30-85 ℃, and the kettle temperature of the heavy removal tower is determined according to the physical properties of the high-boiling gas.
7. The utility model provides a rectification separation purification system of chlorine hydride sulfur dioxide gas which characterized in that: the device comprises a compressor, a second cooler, a liquid phase buffer tank and a light component removal device, wherein the light component removal device comprises a light component removal tower, a condenser and a first reboiler, an outlet of the compressor is communicated with an inlet of the second cooler, an outlet of the second cooler is communicated with an inlet of the liquid phase buffer tank, an outlet of the liquid phase buffer tank is communicated with an inlet of the light component removal tower, the light component removal tower comprises a gas phase outlet and a liquid phase outlet, the gas phase outlet of the light component removal tower is communicated with the condenser, and the liquid phase outlet of the light component removal tower is communicated with the first reboiler.
8. The system of claim 7, further comprising a washing device, wherein the washing device comprises a washing tower, a circulating pump and a first cooler, the washing tower comprises a gas phase inlet, a gas phase outlet, a washing liquid inlet and a washing liquid outlet, the gas phase outlet of the washing tower is communicated with the inlet of the compressor, the washing liquid inlet of the washing tower is communicated with the outlet of the first cooler, the washing liquid outlet of the washing tower is communicated with the inlet of the circulating pump, the outlet of the circulating pump is communicated with the inlet of the first cooler, a washing liquid circulating loop is formed among the washing tower, the circulating pump and the first cooler, and the washing liquid circulating loop is provided with the washing liquid inlet and the washing liquid outlet.
9. The system of claim 7, further comprising a de-heaving apparatus comprising a de-heaving column comprising an inlet, a vapor outlet, a liquid phase outlet, a third reflux port A, and a fourth reflux port A, a third cooler, and a second reboiler, the outlet of the first reboiler being in communication with the inlet of the de-heaving column, the vapor outlet of the de-heaving column being in communication with the inlet of the third cooler, the third cooler having an outlet and a third reflux port B, the third reflux port B being in communication with the third reflux port A, the liquid outlet of the de-heaving column being in communication with the inlet of the second reboiler, the second reboiler having an outlet and a fourth reflux port B, the fourth reflux port B being in communication with the fourth reflux port A.
10. The system of claim 7, 8 or 9, wherein the condenser comprises a first flow passage, the gas phase outlet of the lightness-removing column is communicated with the inlet of the first flow passage, the first flow passage is provided with a first reflux port B, the lightness-removing column is provided with a first reflux port A, and the first reflux port B is communicated with the first reflux port A; and/or the first reboiler comprises a third flow channel, a liquid phase outlet of the light component removal tower is communicated with an inlet of the third flow channel, the third flow channel is provided with a second reflux port B, the light component removal tower is provided with a second reflux port A, and the second reflux port B is communicated with the second reflux port A.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN107082427A (en) * | 2017-04-19 | 2017-08-22 | 苏州市兴鲁空分设备科技发展有限公司 | Carbon disulfide retracting device |
| CN115231524A (en) * | 2022-07-12 | 2022-10-25 | 浙江省天正设计工程有限公司 | Separation and purification method and device for tail gas containing hydrogen fluoride in fluorine chemical production |
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| CN107746040A (en) * | 2017-10-17 | 2018-03-02 | 山东新龙科技股份有限公司 | A kind of Processes and apparatus that hydrogen chloride is refined using the by-product gas for producing trichloro ethylene |
| CN210278686U (en) * | 2019-07-25 | 2020-04-10 | 山东瀚华工程设计有限公司 | Sulfur dioxide and hydrogen chloride containing tail gas recovery processing device |
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| CN107746040A (en) * | 2017-10-17 | 2018-03-02 | 山东新龙科技股份有限公司 | A kind of Processes and apparatus that hydrogen chloride is refined using the by-product gas for producing trichloro ethylene |
| CN210278686U (en) * | 2019-07-25 | 2020-04-10 | 山东瀚华工程设计有限公司 | Sulfur dioxide and hydrogen chloride containing tail gas recovery processing device |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107082427A (en) * | 2017-04-19 | 2017-08-22 | 苏州市兴鲁空分设备科技发展有限公司 | Carbon disulfide retracting device |
| CN115231524A (en) * | 2022-07-12 | 2022-10-25 | 浙江省天正设计工程有限公司 | Separation and purification method and device for tail gas containing hydrogen fluoride in fluorine chemical production |
| CN115231524B (en) * | 2022-07-12 | 2024-03-12 | 浙江省天正设计工程有限公司 | Separation and purification method and device for tail gas containing hydrogen fluoride in fluorine chemical production |
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