CN114933282A - Low-consumption high-efficiency separation method for tail gas containing hydrogen fluoride, hydrogen chloride and nitrogen - Google Patents
Low-consumption high-efficiency separation method for tail gas containing hydrogen fluoride, hydrogen chloride and nitrogen Download PDFInfo
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- CN114933282A CN114933282A CN202210424082.7A CN202210424082A CN114933282A CN 114933282 A CN114933282 A CN 114933282A CN 202210424082 A CN202210424082 A CN 202210424082A CN 114933282 A CN114933282 A CN 114933282A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
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- C01B7/00—Halogens; Halogen acids
- C01B7/19—Fluorine; Hydrogen fluoride
- C01B7/191—Hydrogen fluoride
- C01B7/195—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
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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
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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
- C01B7/19—Fluorine; Hydrogen fluoride
- C01B7/191—Hydrogen fluoride
- C01B7/195—Separation; Purification
- C01B7/196—Separation; Purification by distillation
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Abstract
The invention relates to a low-consumption high-efficiency separation method of tail gas containing hydrogen fluoride, hydrogen chloride and nitrogen, belonging to the field of chemical separation. The separation method provided by the invention comprises the steps of compressing and condensing the tail gas to partially liquefy the tail gas, then carrying out gas-liquid separation, sending the separated gas phase into an absorption tower to recover hydrogen chloride contained in the gas, sending the liquid phase into a rectifying tower, and continuously rectifying by utilizing the rectifying tower to realize the separation of light components mainly comprising the hydrogen chloride and the hydrogen fluoride. The separation method provided by the invention can effectively separate and recycle hydrogen fluoride and hydrogen chloride, realize tail gas resource utilization, greatly reduce the operation cost, improve the economic benefit of the whole process and simultaneously enable the whole process to operate more stably.
Description
Technical Field
The invention relates to the field of chemical separation, in particular to a low-consumption high-efficiency separation method for tail gas containing hydrogen fluoride, hydrogen chloride and nitrogen.
Background
The tail gas containing hydrogen fluoride, hydrogen chloride and nitrogen is a common tail gas in the field of fluorine chemical industry at present, and particularly in the production process of lithium hexafluorophosphate, a large amount of tail gas can be generated, which has great harm to the environment and human bodies, so that the treatment of the tail gas has higher requirements. Meanwhile, the hydrogen chloride and the hydrogen fluoride contained in the tail gas have higher recovery value, and if the tail gas can be economically and reasonably recovered and treated, certain economic benefit can be increased while the chemical tail gas is reasonably treated. However, no known effective treatment method has been established for the technical problem of recovering and treating this type of tail gas. The common methods mainly comprise an absorption method and a condensation method, but have obvious technical defects, and the products obtained after the technical treatment have the problems of incomplete separation of hydrogen fluoride and hydrogen chloride, low application value of the separated products and the like. Patent 202111579824.5 reports a pressure distillation method, which can effectively separate hydrogen fluoride and hydrogen chloride when the pressure is 0.6-3.0Mpa, obtain high-purity hydrogen fluoride at the bottom of the tower, obtain the mixed gas of hydrogen chloride and hydrogen fluoride at the top of the tower, and obtain hydrochloric acid and nitrogen by absorption separation. However, the method needs to pressurize the tail gas to a higher pressure, and the energy consumption is higher. Patent 202111634638.7 has improved this technology, after carrying out preliminary pressurization to tail gas, through the condensation, with almost all hydrogen fluoride and most hydrogen chloride condensation get off, through high-pressure pump sending to the heat exchange tower, remaining gas passes through the compressor and steps up the back heat exchange tower, and two strands of fluids get into the rectifying column respectively after the heat exchange tower heat transfer and carry out the rectification separation, obtain high-purity hydrogen fluoride at the bottom of the tower, the top of the tower obtains the mist of hydrogen chloride and hydrogen fluoride. Compared with patent 202111579824.5, the method has the advantages of greatly reduced compressed gas amount, and high energy consumption. However, since the added value of hydrochloric acid is low, it is difficult for the obtained hydrochloric acid profit to cover the running cost of the compressor compared to the energy consumed by the compressor. In addition, the existence of the nitrogen with a large proportion not only increases the debugging and operation difficulty of the rectifying tower, but also makes the steam at the top of the tower difficult to condense, and can meet the condensing requirement of the hydrogen chloride only by needing higher pressure and very low temperature, thereby increasing the operation cost. Therefore, it is necessary to develop a low-energy-consumption and high-efficiency treatment process for chemical tail gas mainly containing hydrogen fluoride, hydrogen chloride and nitrogen.
Disclosure of Invention
In order to solve the problem of higher energy consumption in the prior art, the invention provides a low-consumption high-efficiency separation method of tail gas containing hydrogen fluoride, hydrogen chloride and nitrogen.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a low-consumption high-efficiency separation method of tail gas containing hydrogen fluoride, hydrogen chloride and nitrogen, which comprises the following steps:
(1) firstly, compressing and boosting tail gas by a compressor;
(2) cooling the boosted tail gas obtained in the step (1) by a heat exchanger, and partially condensing to obtain a gas-liquid two-phase;
(3) and (3) rectifying the liquid phase obtained in the step (2) by using a rectifying tower, extracting high-purity hydrogen fluoride liquid at the bottom of the tower, and extracting a mixture of high-purity hydrogen chloride and a small amount of nitrogen at the top of the tower.
Preferably, the pressure of the tail gas in the step (1) is increased from the normal pressure to 2.0-8.0bar after the tail gas is compressed by a compressor.
Preferably, the condensation temperature of the heat exchanger in the step (2) is-25 to-80 ℃.
Preferably, the theoretical plate number of the rectifying tower in the step (3) is 6-30, and the reflux ratio of the rectifying tower is 0.5-5.
Preferably, the feeding position of the liquid phase in the step (3) is 3-20 theoretical plates from top to bottom in the rectifying tower.
Preferably, the top temperature of the rectifying tower in the step (3) is-55 to 5 ℃, and the top pressure of the rectifying tower is 5 to 30 bar.
Preferably, the tail gas mainly contains hydrogen fluoride, hydrogen chloride and nitrogen, and also contains a small amount of phosphorus pentafluoride, and the contents of the components are as follows by mass fraction: 20-70% of hydrogen fluoride, 10-60% of nitrogen, 5-50% of hydrogen chloride and 0.01-1.5% of phosphorus pentafluoride. The separation method provided by the invention comprises the following steps of firstly compressing and condensing the chemical tail gas to obtain a gas phase and a liquid phase, wherein the gas phase mainly comprises nitrogen and hydrogen chloride, the hydrogen chloride can be recovered through an absorption tower, and a small amount of hydrogen fluoride can be removed in advance through absorption; the liquid phase is a mixed liquid mainly containing hydrogen chloride, hydrogen fluoride and a small amount of nitrogen and phosphorus pentafluoride, and is pumped into a rectifying tower, and the separation of the hydrogen fluoride and the hydrogen chloride is completed in the rectifying tower. High-purity hydrogen fluoride is extracted from the tower bottom, and gas mainly containing hydrogen chloride is extracted from the tower top and can be used as a hydrogen chloride product or used for preparing hydrochloric acid through absorption. The invention has the following remarkable advantages:
(1) the gas phase is directly absorbed to prepare the hydrochloric acid without going to the rectifying tower, so that the subsequent compression energy consumption of the part of gas can be saved, the operation cost is greatly reduced, and meanwhile, the operation pressure of the rectifying tower is reduced, the operation temperature is increased, the operation condition is more moderate, and the operation cost is reduced;
(2) the content of nitrogen in the liquid phase entering the rectification is very low, which is beneficial to the continuous and stable operation of the rectification tower;
(3) the rectification method has better separation effect and larger processing capacity, and can obtain high-quality hydrogen fluoride and hydrogen chloride.
Drawings
FIG. 1 is a low-consumption and high-efficiency separation method of tail gas containing hydrogen fluoride, hydrogen chloride and nitrogen in the embodiment of the invention; in the figure, 1 is a compressor, 2 is a condensing heat exchanger, 3 is a gas-liquid separation tank, 4 is an HCl absorption tower, 5 is a rectifying tower feed pump, 6 is a rectifying tower, 7 is a rectifying tower condenser, 8 is a rectifying tower reflux tank, 9 is a reflux pump, and 10 is a rectifying tower reboiler
Detailed Description
The invention provides a low-consumption high-efficiency separation method of tail gas containing hydrogen fluoride, hydrogen chloride and nitrogen, which comprises the following steps:
(1) firstly, compressing and boosting tail gas by a compressor;
(2) cooling the boosted tail gas obtained in the step (1) by a heat exchanger, and partially condensing to obtain a gas phase and a liquid phase;
(3) and (3) rectifying the liquid phase obtained in the step (2) by using a rectifying tower, extracting high-purity hydrogen fluoride liquid at the bottom of the tower, and extracting a mixture of high-purity hydrogen chloride and a small amount of nitrogen at the top of the tower.
Preferably, the pressure of the tail gas in the step (1) is increased from the normal pressure to 2.0-8.0bar after being compressed by a compressor.
Preferably, the condensation temperature of the heat exchanger in the step (2) is-25 to-80 ℃.
Preferably, the theoretical plate number of the rectifying tower in the step (3) is 6-30, and the reflux ratio of the rectifying tower is 0.5-5.
Preferably, the feeding position of the liquid phase in the step (3) is 3-20 theoretical plates from top to bottom in the rectifying tower.
Preferably, the top temperature of the rectifying tower in the step (3) is-55 to 5 ℃, and the top pressure of the rectifying tower is 5 to 30 bar.
Preferably, the tail gas mainly contains hydrogen fluoride, hydrogen chloride and nitrogen, and also contains a small amount of phosphorus pentafluoride, and the contents of the components are as follows by mass fraction: 20-70% of hydrogen fluoride, 10-60% of nitrogen, 5-50% of hydrogen chloride and 0.01-1.5% of phosphorus pentafluoride.
In the present invention, it is preferable that the chemical off-gas mainly containing hydrogen fluoride, hydrogen chloride and nitrogen is condensed after being compressed.
The compression is not particularly limited by the present invention and may be performed in a manner well known in the art.
The condensation can be directly cooled by an external cold source, and can also be subjected to heat exchange with mixed gas which is obtained from the top of the rectifying tower and mainly comprises hydrogen chloride/nitrogen to condense the chemical tail gas.
In the invention, preferably, the gas-liquid two phases obtained in the step (2) are separated by a gas-liquid separation tank, and then the liquid phase is sent to a rectifying tower for continuous rectification and separation; the gas phase is sent to the bottom of the absorption tower and contacts with the absorbent in the absorption tower in a countercurrent way to absorb the hydrogen chloride contained in the gas.
After the rectification is finished, preferably, the distillate at the top of the tower is extracted, then is subjected to partial condensation and gas-liquid separation in sequence to obtain a gas-liquid two phase, the liquid phase flows back to the rectification tower, and the gas phase is extracted.
The present invention is not particularly limited to such condensation and may be carried out in a manner well known in the art.
The technical solution of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. 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 invention.
Example 1
FIG. 1 is a process flow diagram of a low-consumption and high-efficiency separation method of tail gas containing hydrogen fluoride, hydrogen chloride and nitrogen in the embodiment, the chemical tail gas is condensed and pressurized to 2.0-8.0bar by a compressor 1 at normal temperature and normal pressure and then sent into a condensing heat exchanger 2, partial gas phase obtained after the partial condensation in the condensation heat exchanger reaches-25 to 80 ℃ is sent into a gas-liquid separation tank 3, gas phase extracted from the top of the gas-liquid separation tank enters the bottom of a hydrogen chloride absorption tower 4, the hydrogen chloride contained in the gas phase is absorbed by the countercurrent contact of the absorption agent in the absorption tower, the liquid phase extracted from the bottom of the gas-liquid separation tank enters a rectifying tower 6 through a rectifying tower feed pump 5, distilling out light components mainly containing hydrogen chloride from the top of the rectifying tower 6, partially condensing by a rectifying tower condenser 7, performing gas-liquid separation by a rectifying tower reflux tank 8, completely refluxing a liquid phase into the rectifying tower 6, and extracting a gas phase to obtain a gas mainly containing hydrogen chloride with extremely low hydrogen fluoride content; the rectifying tower reboiler 10 provides rising steam for the tower, and the rectifying tower 6 produces high-purity hydrogen fluoride, and the hydrogen fluoride is cooled and then enters a hydrogen fluoride product tank for storage.
(1) Firstly, compressing and boosting tail gas by a compressor;
(2) cooling the boosted tail gas obtained in the step (1) by a heat exchanger, and partially condensing to obtain a gas-liquid two-phase;
(3) and (3) rectifying the liquid phase obtained in the step (2) by using a rectifying tower, extracting high-purity hydrogen fluoride liquid at the bottom of the tower, and extracting a mixture of high-purity hydrogen chloride and a small amount of nitrogen at the top of the tower.
According to mass fraction, the chemical tail gas comprises 42.7% of hydrogen fluoride, 28.1% of hydrogen chloride, 28.9% of nitrogen and 0.3% of phosphorus pentafluoride;
the pressure of the chemical tail gas in the step (1) is increased to 2.1 bar;
partially condensing the gas phase of the step (2) to-25 ℃ through a condensing heat exchanger;
the theoretical plate number of the rectifying tower is 30, and the reflux ratio is 2.0;
the feeding position of the liquid phase is the 11 th theoretical plate counted from top to bottom in the rectifying tower;
the top temperature of the rectifying tower is-51 ℃, and the top pressure is 5.0 bar;
the mixed gas which is obtained from the tower top and mainly comprises nitrogen and hydrogen chloride contains 98.51% of hydrogen chloride, 1.01% of nitrogen, 0.47% of phosphorus pentafluoride and less than 100ppm of hydrogen fluoride in terms of mass fraction;
the tower bottom extracts high-purity hydrogen fluoride, and the purity of the hydrogen fluoride is more than 99.99 percent and the purity of the hydrogen chloride is less than 50ppm in terms of mass fraction.
Example 2
A low-consumption high-efficiency separation method of tail gas containing hydrogen fluoride, hydrogen chloride and nitrogen comprises the following steps:
(1) firstly, compressing and boosting tail gas by a compressor;
(2) cooling the boosted tail gas obtained in the step (1) by a heat exchanger, and partially condensing to obtain a gas-liquid two-phase;
(3) and (3) rectifying the liquid phase obtained in the step (2) by using a rectifying tower, extracting high-purity hydrogen fluoride liquid at the bottom of the tower, and extracting a mixture of high-purity hydrogen chloride and a small amount of nitrogen at the top of the tower.
According to mass fraction, the chemical tail gas comprises 48.7% of hydrogen fluoride, 28.6% of hydrogen chloride, 22.5% of nitrogen and 0.2% of phosphorus pentafluoride;
the pressure of the chemical tail gas in the step (1) is increased to 5.0 bar;
the gas phase of step (2) is partially condensed to-50 ℃ by a condensing heat exchanger;
the number of theoretical plates of the rectifying tower is 21, and the reflux ratio is 3.2;
the feeding position of the liquid phase is 15 th theoretical plate counted from top to bottom in the rectifying tower;
the top temperature of the rectifying tower is-27 ℃, and the top pressure is 12 bar;
the mixed gas which is mainly composed of nitrogen and hydrogen chloride and is extracted from the tower top contains 99.29% of hydrogen chloride, 0.49% of nitrogen, 0.21% of phosphorus pentafluoride and less than 100ppm of hydrogen fluoride in terms of mass fraction;
the tower bottom is used for extracting high-purity hydrogen fluoride, and the purity of the hydrogen fluoride is more than 99.99 percent and the hydrogen chloride is less than 50ppm in terms of mass fraction.
Example 3
A low-consumption high-efficiency separation method of tail gas containing hydrogen fluoride, hydrogen chloride and nitrogen comprises the following steps:
(1) firstly, compressing and boosting tail gas by a compressor;
(2) cooling the boosted tail gas obtained in the step (1) by a heat exchanger, and partially condensing to obtain a gas-liquid two-phase;
(3) and (3) rectifying the liquid phase obtained in the step (2) by using a rectifying tower, extracting high-purity hydrogen fluoride liquid at the bottom of the tower, and extracting a mixture of high-purity hydrogen chloride and a small amount of nitrogen at the top of the tower.
According to the mass fraction, the chemical tail gas comprises 55.9% of hydrogen fluoride, 30.4% of hydrogen chloride, 13.6% of nitrogen and 0.1% of phosphorus pentafluoride;
the pressure of the chemical tail gas in the step (1) is increased to 6.0 bar;
the gas phase of step (2) is partially condensed to-65 ℃ by a condensing heat exchanger;
the number of theoretical plates of the rectifying tower is 10, and the reflux ratio is 4.8;
the feeding position of the liquid phase is a 7 th theoretical plate counted from top to bottom in the rectifying tower;
the temperature at the top of the rectifying tower is-2 ℃, and the pressure at the top of the rectifying tower is 25 bar;
the mixed gas which is obtained from the tower top and mainly comprises nitrogen and hydrogen chloride contains 98.28 percent of hydrogen chloride, 1.43 percent of nitrogen, 0.28 percent of phosphorus pentafluoride and less than 100ppm of hydrogen fluoride in terms of mass fraction;
the tower bottom extracts high-purity hydrogen fluoride, and the purity of the hydrogen fluoride is more than 99.99 percent and the purity of the hydrogen chloride is less than 50ppm in terms of mass fraction.
According to the results of the embodiment, the separation method provided by the invention can obtain the hydrogen fluoride liquid with the mass fraction higher than 99.99%, and meanwhile, the mixed gas obtained from the tower top can be processed by subsequent working sections to obtain high-purity hydrogen chloride. The two substances can be used or sold as byproducts, so that the emission of waste gas is reduced, and meanwhile, the economic value is created for enterprises.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (7)
1. A low-consumption high-efficiency separation method of tail gas containing hydrogen fluoride, hydrogen chloride and nitrogen comprises the following steps:
(1) firstly, compressing and boosting tail gas by a compressor;
(2) cooling the boosted tail gas obtained in the step (1) by a heat exchanger, and partially condensing to obtain a gas-liquid two-phase;
(3) and (3) rectifying the liquid phase obtained in the step (2) by using a rectifying tower, extracting high-purity hydrogen fluoride liquid at the bottom of the tower, and extracting a mixture of high-purity hydrogen chloride and a small amount of nitrogen at the top of the tower.
2. The separation method according to claim 1, wherein the pressure of the tail gas in the step (1) is increased from the normal pressure to 2.0-8.0bar after being compressed by a compressor.
3. The separation process according to claim 1, wherein the condensation temperature of the heat exchanger in step (2) is from-25 to-80 ℃.
4. The separation process according to claim 1, wherein the number of theoretical plates of the rectifying column in the step (3) is 6 to 30, and the reflux ratio of the rectifying column is 0.5 to 5.
5. The separation process according to claim 1, wherein the liquid phase in the step (3) is fed from the top to the bottom of 3 to 20 theoretical plates in the rectification column.
6. The separation method according to claim 1, wherein the temperature of the top of the rectifying column in the step (3) is-55 to 5 ℃ and the pressure of the top of the rectifying column is 5 to 30 bar.
7. The separation method according to claim 1, wherein the tail gas mainly comprises hydrogen fluoride, hydrogen chloride and nitrogen, and also comprises a small amount of phosphorus pentafluoride, and the content of each component is as follows by mass fraction: 20-70% of hydrogen fluoride, 10-60% of nitrogen, 5-50% of hydrogen chloride and 0.01-1.5% of phosphorus pentafluoride.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN205550002U (en) * | 2016-03-11 | 2016-09-07 | 河南晋开化工投资控股集团有限责任公司 | Transforming gas desulfurization device |
| CN110248918A (en) * | 2017-01-31 | 2019-09-17 | 大金工业株式会社 | The manufacturing method of fluorine-containing halogenated hydrocarbon |
| CN114180527A (en) * | 2021-12-22 | 2022-03-15 | 中国矿业大学(北京) | Method for separating hydrogen fluoride and hydrogen chloride from chemical tail gas |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN205550002U (en) * | 2016-03-11 | 2016-09-07 | 河南晋开化工投资控股集团有限责任公司 | Transforming gas desulfurization device |
| CN110248918A (en) * | 2017-01-31 | 2019-09-17 | 大金工业株式会社 | The manufacturing method of fluorine-containing halogenated hydrocarbon |
| CN114180527A (en) * | 2021-12-22 | 2022-03-15 | 中国矿业大学(北京) | Method for separating hydrogen fluoride and hydrogen chloride from chemical tail gas |
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