CN113577811A - Energy-saving device and method for separating anhydrous hydrogen fluoride - Google Patents

Energy-saving device and method for separating anhydrous hydrogen fluoride Download PDF

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Publication number
CN113577811A
CN113577811A CN202110641002.9A CN202110641002A CN113577811A CN 113577811 A CN113577811 A CN 113577811A CN 202110641002 A CN202110641002 A CN 202110641002A CN 113577811 A CN113577811 A CN 113577811A
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crude
tower
degassing
rectifying
reboiler
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尚剑
奚志骏
董文胜
洪钟
杨虹
李佳
张蕊
王一焯
骆彩萍
谢文
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Hualu Engineering and Technology Co Ltd
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Hualu Engineering and Technology Co Ltd
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D3/00Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
    • B01D3/14Fractional distillation or use of a fractionation or rectification column
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D3/00Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
    • B01D3/14Fractional distillation or use of a fractionation or rectification column
    • B01D3/32Other features of fractionating columns ; Constructional details of fractionating columns not provided for in groups B01D3/16 - B01D3/30
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D3/00Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
    • B01D3/14Fractional distillation or use of a fractionation or rectification column
    • B01D3/32Other features of fractionating columns ; Constructional details of fractionating columns not provided for in groups B01D3/16 - B01D3/30
    • B01D3/322Reboiler specifications
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D3/00Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
    • B01D3/42Regulation; Control
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B7/00Halogens; Halogen acids
    • C01B7/19Fluorine; Hydrogen fluoride
    • C01B7/191Hydrogen fluoride
    • C01B7/195Separation; Purification
    • C01B7/196Separation; Purification by distillation
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00Technologies relating to chemical industry
    • Y02P20/10Process efficiency
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00Technologies relating to chemical industry
    • Y02P20/50Improvements relating to the production of bulk chemicals

Abstract

The invention discloses an energy-saving device and method for separating anhydrous hydrogen fluoride. The method makes the following improvements on the common single normal pressure or single pressure rectification anhydrous hydrogen fluoride purification flow path in industry: adjusting the operating pressure of two towers of an anhydrous hydrogen fluoride rectification sequence which removes heavy component impurities firstly and then removes light component impurities, enabling a crude HF rectification tower which removes the heavy component impurities to be in a higher pressure state, enabling a crude HF degassing tower which removes the light component impurities to be in a lower pressure state, and controlling the pressure difference of the two towers to keep sufficient temperature difference; and then, supplying heat to the degassing tower by using the steam at the top of the rectifying tower in a direct heat exchange or indirect working medium heat exchange mode. By the method, the energy consumption in the rectification separation process of the anhydrous hydrogen fluoride can be obviously reduced, and the method has high economic benefit. In addition, the invention also discloses a variant method for carrying out the pressure-variable thermal coupling rectification by keeping the crude HF rectification column at a lower pressure state and the crude HF degassing column at a higher pressure state.

Description

Energy-saving device and method for separating anhydrous hydrogen fluoride
Technical Field
The invention belongs to the field of anhydrous hydrogen fluoride production, and particularly relates to an energy-saving anhydrous hydrogen fluoride rectification separation method; in particular to a method for separating anhydrous hydrogen fluoride products by adopting a variable pressure thermal coupling rectification technology.
Background
The anhydrous hydrogen fluoride is used as an important basic chemical raw material, has strong oxidizing property, strong corrosivity and acidity, is commonly used for producing villiaumite, fluorohaloalkane, fluorine refrigerant, etched glass, impregnated wood, electrolytic element fluorine and the like, and is widely applied to the industries of atomic energy, chemical industry, petroleum and the like; the purified product can be used in the photovoltaic industry after being purified to the electronic grade, and has wide application prospect.
The fluorite method is generally used as a technological process for synthesizing anhydrous hydrogen fluoride in industry, and the preparation method generally comprises the steps of mixing fluorite and sulfuric acid, generating hydrogen fluoride under the heating condition, washing and condensing to obtain a crude product of the hydrogen fluoride, and then rectifying and degassing to obtain a qualified anhydrous hydrogen fluoride product.
Because the boiling point difference among the components of the crude anhydrous hydrogen fluoride product is large, the anhydrous hydrogen fluoride is generally purified industrially by adopting a mode of serially connecting a rectifying tower and a degassing tower, and the difference is that a single pressure rectifying process or an atmospheric pressure rectifying process is generally used. The normal pressure rectification process is relatively wide in application due to relatively mild operation conditions, but in the case, the normal pressure boiling point of the anhydrous hydrogen fluoride is only 19.7 ℃, although the bottom of the tower can be heated by a low-grade heat source, the condensation at the top of the tower needs to use freezing water with relatively high cost for condensation, so that the operation cost is relatively high; in the pressure rectification process, the two towers are pressurized to the tower top temperature of more than 50 ℃ and then run (the operation pressure is about more than 220 kPaA), in this case, the condensation at the tower top of the pressure rectification can be cooled by using circulating water, the tower bottom is generally heated by using low-pressure steam, the running cost is relatively low, but the requirement of higher standard is provided for equipment manufacture.
Thermal coupled rectification (also called heat integrated rectification) is a rectification energy-saving method provided based on a pinch point technology, and the principle is that when a plurality of towers with different energy levels (namely temperatures) exist in the whole process, tower top steam of a tower with higher temperature supplies heat to a reboiler of a tower with lower temperature, and simultaneously the steam is condensed. Therefore, the high-temperature tower does not need an extra cold source for cooling, and the low-temperature tower does not need an extra heat source for heating, thereby achieving the obvious energy-saving effect.
The pressure swing rectification technology is a technology for separating products by instructing a rectifying tower in a flow under different pressure levels. The technology is originally used for breaking through the azeotropic composition of an azeotropic mixture so as to obtain a required pure product, but under the condition of combining a thermal coupling rectification energy-saving technology, different energy levels can be artificially generated in a variable pressure mode, so that the original process which cannot use thermal coupling rectification can save energy through the thermal coupling rectification technology.
Disclosure of Invention
The invention provides an energy-saving device and method for separating anhydrous hydrogen fluoride, which realize energy coupling in the rectification process of anhydrous hydrogen fluoride products by a variable-pressure thermal coupling rectification technology, so that the crude HF rectification tower and the crude HF degassing tower can meet the previous requirements only by consuming the energy consumption of a single tower, and the energy-saving effect is obvious.
One of the purposes of the invention is to provide an energy-saving device for separating anhydrous hydrogen fluoride, which is characterized by comprising the following equipment: a crude HF rectifying tower, a reboiler at the bottom of the crude HF rectifying tower, a crude HF degassing tower, a reboiler at the bottom of the crude HF degassing tower and a condenser at the top of the crude HF degassing tower; the tower top steam outlet of the crude HF rectifying tower is connected to the heating side inlet of the tower bottom reboiler of the crude HF degassing tower, and the heating side outlet of the tower bottom reboiler of the crude HF degassing tower is connected to the tower top condensate inlet of the crude HF rectifying tower through a thermal coupling pipeline reflux pump.
The invention also aims to provide an energy-saving method for separating anhydrous hydrogen fluoride, which is characterized in that a crude HF rectifying tower is in a high-pressure operation condition, a crude HF degassing tower is in a low-pressure operation condition, an anhydrous hydrogen fluoride crude product enters the crude HF rectifying tower, heavy component impurities with high boiling point are extracted from the bottom of the tower, a crude HF product without high-boiling substances is extracted from the top of the tower and enters the crude HF degassing tower; light component impurities with low boiling point are extracted from the top of the coarse HF degassing tower, and anhydrous hydrogen fluoride products with qualified indexes are extracted from the bottom of the coarse HF degassing tower; and a thermal coupling rectification method is adopted between the crude HF rectifying tower and the crude HF degassing tower, so that material steam at the tower top of the crude HF rectifying tower directly supplies heat to a reboiler at the tower bottom of the crude HF degassing tower, and condensed liquid returns to the tower top of the crude HF rectifying tower through a reflux pump of a thermal coupling pipeline.
Furthermore, the material steam at the top of the crude HF rectifying tower can indirectly supply heat to the reboiler at the bottom of the crude HF degassing tower by adopting an intermediate working medium, at the moment, a condenser at the top of the crude HF rectifying tower is added, the intermediate working medium firstly obtains heat from the condenser at the top of the crude HF rectifying tower, then releases the obtained heat from the reboiler at the bottom of the crude HF degassing tower, and then returns to the inlet of the condenser at the top of the crude HF degassing tower through an intermediate working medium circulating reflux pump to form an intermediate working medium heat exchange loop.
Further, the top temperature of the crude HF rectification column is always higher than the bottom temperature of the crude HF degassing column and maintains a temperature difference of not less than 2 ℃.
Further, the operation pressure of the crude HF rectification tower is 150 kPaA-1000 kPaA; the operating pressure of the crude HF degassing column is always lower than that of the crude HF rectifying column and a pressure difference of not less than 20kPa is maintained.
Furthermore, an intermediate heat exchanger is additionally arranged on a pipeline for directly or indirectly supplying heat to a reboiler at the bottom of the crude HF degassing tower by material steam at the top of the crude HF rectifying tower, so that the total heat transferred between the two rectifying towers is supplemented or removed, and the stable operation of the two towers is ensured.
The invention also aims to provide another energy-saving device for separating anhydrous hydrogen fluoride, which is characterized by comprising the following equipment: a crude HF rectifying tower, a reboiler at the bottom of the crude HF rectifying tower, a condenser at the top of the crude HF rectifying tower, a crude HF degassing tower and a reboiler at the bottom of the crude HF degassing tower; the steam outlet at the top of the crude HF degassing tower is connected to the heating side inlet of the reboiler at the bottom of the crude HF rectifying tower, and the heating side outlet of the reboiler at the bottom of the crude HF rectifying tower is connected to the condensate inlet at the top of the crude HF degassing tower through a reflux pump of a thermal coupling pipeline.
The fourth purpose of the invention is to provide another energy-saving method for separating anhydrous hydrogen fluoride, which is characterized in that a crude HF rectifying tower is in a low-pressure operation condition, and a crude HF degassing tower is in a high-pressure operation condition; the anhydrous hydrogen fluoride crude product enters a crude HF rectifying tower, heavy component impurities with high boiling point are extracted from the bottom of the tower, the crude HF product without high boiling point substances is extracted from the top of the tower and enters a crude HF degassing tower; light component impurities with low boiling point are extracted from the top of the coarse HF degassing tower, and anhydrous hydrogen fluoride products with qualified indexes are extracted from the bottom of the coarse HF degassing tower; and a thermal coupling rectification method is adopted between the crude HF degassing tower and the crude HF rectifying tower, so that material steam at the tower top of the crude HF degassing tower directly supplies heat to a reboiler at the tower bottom of the HF rectifying tower, and condensed liquid returns to the tower top of the crude HF degassing tower through a reflux pump of a thermal coupling pipeline.
Furthermore, the material steam at the top of the crude HF degassing tower can also adopt an intermediate working medium to indirectly supply heat to a reboiler at the bottom of the crude HF rectifying tower, at the moment, a condenser at the top of the crude HF degassing tower needs to be added, the intermediate working medium obtains heat in the condenser at the top of the crude HF degassing tower firstly, then releases the obtained heat in the reboiler at the bottom of the crude HF rectifying tower, and then returns to the inlet of the condenser at the top of the crude HF degassing tower through an intermediate working medium circulating reflux pump to form an intermediate working medium heat exchange loop.
The tower top temperature of the crude HF degassing tower is always higher than the tower bottom temperature of the crude HF rectifying tower, and the temperature difference of not less than 2 ℃ is maintained.
Further, the operation pressure of the crude HF degassing tower is 150 kPaA-1000 kPaA; the operating pressure of the crude HF rectification column is always lower than that of the crude HF degassing column and a pressure difference of not less than 20kPa is maintained.
Furthermore, a heat exchanger is additionally arranged on a pipeline for directly or indirectly supplying heat to a reboiler at the bottom of the crude HF degassing tower by material steam at the top of the crude HF rectifying tower, so that the supplement or removal of total heat transferred between the two rectifying towers is carried out, and the stable operation of the two towers is ensured.
Furthermore, in the energy-saving method for indirectly supplying heat by using the intermediate working medium, the inflow or outflow of the intermediate working medium can be carried out by additionally arranging an intermediate working medium feeding and discharging branch in a formed intermediate working medium heat exchange loop, so that the proper working medium flow and heat exchange quantity are ensured, and the condition that the heat exchange quantity of the intermediate working medium is too much or too little is avoided.
The invention has the beneficial effects that:
1. the energy coupling of the refining process of the anhydrous hydrogen fluoride product is realized by the variable-pressure thermal coupling rectification technology, so that the crude HF rectifying tower and the crude HF degassing tower can meet the previous separation requirement only by consuming the energy consumption of a single tower, and the energy-saving effect is obvious.
2. Compared with the common single normal pressure or pressurization rectification process in the industry, the method has the advantages of obvious energy-saving effect, no obvious increase of new equipment requirements, strong operation controllability, high safety and strong industrial practical feasibility. But also can be flexibly applied to the reconstruction of the existing anhydrous hydrogen fluoride device.
Drawings
FIG. 1 is a schematic illustration of the separation of an anhydrous hydrogen fluoride product using pressure swing thermal coupling rectification techniques;
FIG. 2 is a schematic diagram of a variation of a process for separating an anhydrous hydrogen fluoride product using pressure swing thermal coupling rectification techniques;
FIG. 3 is a schematic illustration of the separation of an anhydrous hydrogen fluoride product by indirect heat exchange using pressure swing thermal coupling rectification techniques;
FIG. 4 is a schematic diagram of a process for separating an anhydrous hydrogen fluoride product by indirect heat exchange using a variation of the pressure swing thermal coupling rectification technique;
FIG. 5 is a schematic diagram of a process for improved pressure swing thermal coupling rectification separation of an anhydrous hydrogen fluoride product using an intermediate heat exchanger;
FIG. 6 is a schematic diagram of a process for improved indirect heat exchange pressure swing thermal coupling rectification separation of an anhydrous hydrogen fluoride product using an intermediate heat exchanger;
FIG. 7 is a schematic diagram of a process for improved pressure swing thermal coupling rectification separation of an anhydrous hydrogen fluoride product using an intermediate medium inlet and outlet line;
in the attached drawing, the sequence A is a schematic diagram of an energy-saving method and an improved method for the high pressure of a crude HF rectifying tower and the low pressure of a crude HF degassing tower, wherein T1A is a crude HF rectifying tower, H1A is a reboiler at the bottom of the crude HF rectifying tower, and C1A is a condenser at the top of the crude HF rectifying tower; T2A-crude HF degasser, H2A-reboiler at bottom of crude HF degasser, C2A-condenser at top of crude HF degasser, P1A-thermal coupling pipeline reflux pump, P1C-intermediate working medium circulating reflux pump, E1A-intermediate heat exchanger;
the sequence B is a schematic diagram of an energy-saving variant method and an improved method thereof for the high pressure of a crude HF degassing tower and the low pressure of a crude HF rectifying tower, wherein T1B is a crude HF rectifying tower, H1B is a reboiler at the bottom of the crude HF rectifying tower, and C1B is a condenser at the top of the crude HF rectifying tower; T2B-crude HF degasser, H2B-reboiler at bottom of crude HF degasser, C2B-condenser at top of crude HF degasser, P1B-thermal coupling pipeline reflux pump, P1D-intermediate working medium circulating reflux pump, E1B-intermediate heat exchanger.
Detailed Description
The invention is described in further detail below with reference to the following figures and specific examples:
as shown in fig. 1, an energy-saving device for separating anhydrous hydrogen fluoride comprises a crude HF rectifying tower T1A, a tower bottom reboiler H1A of the crude HF rectifying tower; crude HF degasser T2A, crude HF degasser bottoms reboiler H2A, crude HF degasser overhead condenser C2A. Wherein, the reboiler H2A at the bottom of the crude HF degassing tower supplies heat by using the condensation heat of the vapor at the top of the crude HF rectifying tower T1A. A reboiler H2A at the bottom of the crude HF rectifying tower supplies heat by using heat sources such as steam and the like, and a condenser C2A at the top of the crude HF degassing tower supplies cold by using cold sources such as chilled water, circulating water and the like.
An energy-saving method for separating anhydrous hydrogen fluoride, firstly, utilizing a pressure swing rectification technology to adjust the operating pressure of a crude HF rectifying tower T1A and a crude HF degassing tower T2A, so that the operating pressure of the crude HF rectifying tower T1A is always higher than the operating pressure of the crude HF degassing tower T2A, and simultaneously, enough operating pressure difference is kept, thereby a certain temperature difference exists between the two towers; and then, the tower top steam of the crude HF rectifying tower T1A is used for supplying heat to a tower bottom reboiler H2A of the crude HF degassing tower, so that thermal coupling rectification is formed, and a remarkable energy-saving effect is achieved.
An energy-saving method for separating anhydrous hydrogen fluoride products by adopting a variable pressure thermal coupling rectification technology comprises the following steps:
the anhydrous hydrogen fluoride crude product enters a crude HF rectifying tower T1A, heavy component impurities with high boiling point are extracted from the bottom of the tower, the crude HF product without high boiling point substances is extracted from the top of the tower and enters a crude HF degassing tower T2A; light component impurities with low boiling point are extracted from the top of the crude HF degassing tower T2A, and anhydrous hydrogen fluoride products with qualified indexes are extracted from the bottom of the tower. The overhead vapor of crude HF rectifier T1A is used directly to supply heat to the crude HF degasser reboiler H2A.
The operating pressure of the crude HF rectification column T1A should be not less than 150kPaA, preferably 200kPaA to 1000 kPaA;
the operating pressure of the crude HF degassing tower T2A is always lower than the operating pressure of the crude HF rectifying tower T1A, and the pressure difference is at least not less than 20kPa, so that the sufficient heat exchange temperature difference between the two towers is ensured; the reboiler H2A at the bottom of the tower adopts the vapor at the top of the crude HF rectifying tower T1A to supply heat.
A variant of the process according to the invention provides for the crude HF degasser T2B to be at a higher pressure and thus for the supply of heat to the relatively low-pressure crude HF rectifier T1B, the flow diagram being as shown in FIG. 2. The device comprises a crude HF rectifying tower T1B, a crude HF rectifying tower top condenser C1B and a crude HF rectifying tower bottom reboiler H1B; crude HF degasser T2B, crude HF degasser bottoms reboiler H2B.
At this point, the operating pressure of the crude HF degasser T2B should be not less than 150kPaA, preferably between 200kPaA and 1000 kPaA; the operating pressure of the crude HF rectification column T1B is at least not less than 20kPa lower than the operating pressure of the crude HF degassing column T2B, so that the sufficient heat exchange temperature difference between the two columns is ensured; the reboiler H1B at the bottom of the tower adopts the overhead vapor of a crude HF degasser T2B to supply heat.
In addition, the invention also provides an improved method for indirect heat exchange by using the intermediate working medium, and at least a crude HF rectification overhead condenser C1A (shown in figure 3) or a crude HF degassing overhead condenser C2B (shown in figure 4) is added.
When the crude HF rectifying tower T1A is used as a high-temperature heat source, an indirect heat exchange improvement method is shown in figure 3, an intermediate working medium forms a heat exchange cycle, firstly, in a crude HF rectifying tower top condenser C1A, the steam at the top of the crude HF rectifying tower T1A supplies heat to the intermediate working medium and then is condensed, and the intermediate working medium obtains heat; then, in a reboiler H2A at the bottom of the crude HF degassing tower, the intermediate working medium transfers heat to the liquid at the bottom of the crude HF degassing tower, so that indirect heat exchange circulation is realized. If crude HF degasser T2B is used as the high temperature heat source, an indirect heat exchange modification is shown in FIG. 4.
The improved method can decouple the original method, reduce the operation difficulty during driving, simultaneously avoid the out-of-control rectification process caused by the chain effect under the accident working condition and improve the safety of the thermal coupling rectification.
Generally, the intermediate working medium used in the improved method is water, but other suitable intermediate working media besides water can be used according to actual conditions.
In the case that the pressure difference between the two towers is too large or too small, the thermal load difference between the two towers may be too large to be sufficiently matched, and at this time, an intermediate heat exchanger E1A may be added to the heat supply pipeline in the thermally coupled rectification structure, as shown in fig. 5 or fig. 6. At the moment, a heat source or a cold source can be introduced according to the actual condition, so that the heat loads of the two towers are matched, and the stable operation of the device is ensured.
For the improved method of indirect heat supply using intermediate working medium, the flow of intermediate working medium can also be allocated by adding an intermediate working medium inlet and outlet pipeline, as shown in fig. 7. At the moment, the proper heat exchange amount is ensured by adjusting the flow of the intermediate working medium, and the condition that the heat exchange amount of the intermediate working medium is too much or too little is avoided.
[ example 1 ]
As shown in figure 1, a method for separating anhydrous hydrogen fluoride products by adopting a pressure swing thermal coupling rectification technology comprises a crude HF rectification tower T1A, a reboiler H1A at the bottom of the crude HF rectification tower; crude HF degasser T2A, crude HF degasser bottoms reboiler H2A, crude HF degasser overhead condenser C2A. Wherein, the reboiler H2A at the bottom of the crude HF degassing tower supplies heat by using the condensation heat of the vapor at the top of the crude HF rectifying tower T1A. The reboiler H1A at the bottom of the crude HF rectifying tower uses low-pressure steam to supply heat, and the condenser C2A at the top of the crude HF degassing tower uses low-temperature chilled water to supply cold.
The rectification separation process flow of the anhydrous hydrogen fluoride comprises the following steps: the anhydrous hydrogen fluoride crude product flows into a crude HF rectifying tower T1A, heavy component impurities with high boiling point are extracted from the bottom of the tower, the crude HF product without high boiling point substances is extracted from the top of the tower and flows into a crude HF degassing tower T2A; light component impurities with low boiling point are extracted from the top of the crude HF degassing tower T2A, and anhydrous hydrogen fluoride products with qualified indexes are extracted from the bottom of the tower.
The invention adopts a pressure swing rectification technology, and by adjusting the operating pressure and temperature of each tower, the steam at the top of the crude HF rectifying tower T1A can be used for supplying heat to a reboiler H2A at the bottom of a crude HF degassing tower T2A.
The operation pressure of the crude HF rectifying tower T1A is 170kPaA, and the temperature of a tower kettle is controlled at 60 ℃; the crude HF degasser T2A was operated at 110kPaA and the column bottom temperature was controlled at 25 ℃.
Compared with the existing industrial process, the utility energy consumption of unit products of the process scheme is reduced by about 50 percent, and the energy consumption of the single atmospheric distillation process operated in the factory is greatly reduced.
[ example 2 ]
As shown in fig. 2, a variation of the pressure swing thermal coupling rectification technique for separating anhydrous hydrogen fluoride products. The device comprises a crude HF rectifying tower T1B, a reboiler H1B at the bottom of the crude HF rectifying tower, and a condenser C1B at the top of the crude HF rectifying tower; crude HF degasser T2B, crude HF degasser bottoms reboiler H2B. Wherein, the reboiler H1B at the bottom of the crude HF rectifying tower supplies heat by using the condensation heat of the vapor at the top of the crude HF degassing tower T2B. The reboiler H2B at the bottom of the crude HF degassing tower uses low-pressure steam to supply heat, and the condenser C1B at the top of the crude HF rectifying tower uses low-temperature chilled water to supply cold.
The operation pressure of the crude HF rectifying tower T1B is 120kPaA, and the temperature of a tower kettle is controlled at 30 ℃; the crude HF degasser T2B was operated at a pressure of 200kPaA and the column bottom temperature was controlled at 52 ℃.
Compared with the existing industrial process, the utility energy consumption of unit product of the process scheme is reduced by about 45 percent, and the energy consumption of the single atmospheric distillation process operated in the factory is also greatly reduced.
[ example 3 ]
As shown in fig. 3, a method for separating anhydrous hydrogen fluoride products by using a pressure swing thermal coupling rectification technology in an indirect heat exchange mode. The device comprises a crude HF rectifying tower T1A, a reboiler H1A at the bottom of the crude HF rectifying tower, and a condenser C1A at the top of the crude HF rectifying tower; crude HF degasser T2A, crude HF degasser bottoms reboiler H2A, crude HF degasser overhead condenser C2A. Wherein, a circulation loop is formed between the condenser C1A at the top of the crude HF rectifying tower and the reboiler H2A at the bottom of the crude HF degassing tower, and water is used as an intermediate working medium for transferring heat. The reboiler H1A at the bottom of the crude HF rectifying tower uses low-pressure steam to supply heat, and the condenser C2A at the top of the crude HF degassing tower uses low-temperature chilled water to supply cold.
The process flow and the operation pressure are similar to those of the embodiment 1, and only the direct heat exchange mode is changed into the indirect heat exchange mode, so that the details are not repeated.
Compared with the existing industrial process, the utility energy consumption of unit products in the process scheme is also reduced by about 50 percent, and the energy consumption of the single atmospheric distillation process operated in the factory is greatly reduced.

Claims (13)

1. An energy-saving device for separating anhydrous hydrogen fluoride is characterized by comprising the following equipment: a crude HF rectifying tower, a reboiler at the bottom of the crude HF rectifying tower, a crude HF degassing tower, a reboiler at the bottom of the crude HF degassing tower and a condenser at the top of the crude HF degassing tower; the tower top steam outlet of the crude HF rectifying tower is connected to the heating side inlet of the tower bottom reboiler of the crude HF degassing tower, and the heating side outlet of the tower bottom reboiler of the crude HF degassing tower is connected to the tower top condensate inlet of the crude HF rectifying tower through a thermal coupling pipeline reflux pump.
2. An energy-saving method for separating anhydrous hydrogen fluoride is characterized in that a crude HF rectifying tower is in a high-pressure operation condition, a crude HF degassing tower is in a low-pressure operation condition, an anhydrous hydrogen fluoride crude product enters the crude HF rectifying tower, heavy component impurities with high boiling point are extracted from the bottom of the tower, the crude HF product without high boiling point substances is extracted from the top of the tower and enters the crude HF degassing tower; light component impurities with low boiling point are extracted from the top of the coarse HF degassing tower, and anhydrous hydrogen fluoride products with qualified indexes are extracted from the bottom of the coarse HF degassing tower; and a thermal coupling rectification method is adopted between the crude HF rectifying tower and the crude HF degassing tower, so that material steam at the tower top of the crude HF rectifying tower directly supplies heat to a reboiler at the tower bottom of the crude HF degassing tower, and condensed liquid returns to the tower top of the crude HF rectifying tower through a reflux pump of a thermal coupling pipeline.
3. The energy-saving method as claimed in claim 2, wherein the tower top material steam of the crude HF rectifying tower indirectly supplies heat to the reboiler at the bottom of the crude HF degassing tower by using the intermediate working medium, and at this time, a tower top condenser of the crude HF rectifying tower is added, the intermediate working medium firstly obtains heat from the tower top condenser of the crude HF rectifying tower, then releases the obtained heat from the reboiler at the bottom of the crude HF degassing tower, and then returns to the tower top condenser of the crude HF degassing tower through the intermediate working medium circulating reflux pump to form the intermediate working medium heat exchange loop.
4. Energy-saving process according to claim 2 or 3, characterized in that the temperature at the top of the crude HF rectification column is always higher than the temperature at the bottom of the crude HF degassing column and a temperature difference of not less than 2 ℃ is maintained.
5. Energy-saving process according to claim 2 or 3, characterized in that the operating pressure of the crude HF rectification column is from 150kPaA to 1000 kPaA; the operating pressure of the crude HF degassing column is always lower than that of the crude HF rectifying column and a pressure difference of not less than 20kPa is maintained.
6. An energy-saving device for separating anhydrous hydrogen fluoride is characterized by comprising the following equipment: a crude HF rectifying tower, a reboiler at the bottom of the crude HF rectifying tower, a condenser at the top of the crude HF rectifying tower, a crude HF degassing tower and a reboiler at the bottom of the crude HF degassing tower; the steam outlet at the top of the crude HF degassing tower is connected to the heating side inlet of the reboiler at the bottom of the crude HF rectifying tower, and the heating side outlet of the reboiler at the bottom of the crude HF rectifying tower is connected to the condensate inlet at the top of the crude HF degassing tower through a reflux pump of a thermal coupling pipeline.
7. An energy-saving method for separating anhydrous hydrogen fluoride is characterized in that a crude HF rectifying tower is in a low-pressure operation condition, and a crude HF degassing tower is in a high-pressure operation condition; the anhydrous hydrogen fluoride crude product enters a crude HF rectifying tower, heavy component impurities with high boiling point are extracted from the bottom of the tower, the crude HF product without high boiling point substances is extracted from the top of the tower and enters a crude HF degassing tower; light component impurities with low boiling point are extracted from the top of the coarse HF degassing tower, and anhydrous hydrogen fluoride products with qualified indexes are extracted from the bottom of the coarse HF degassing tower; and a thermal coupling rectification method is adopted between the crude HF degassing tower and the crude HF rectifying tower, so that material steam at the tower top of the crude HF degassing tower directly supplies heat to a reboiler at the tower bottom of the HF rectifying tower, and condensed liquid returns to the tower top of the crude HF degassing tower through a reflux pump of a thermal coupling pipeline.
8. The energy-saving method as claimed in claim 7, wherein the tower top material steam of the crude HF degassing tower indirectly supplies heat to the reboiler at the bottom of the crude HF rectifying tower by using the intermediate working medium, and at the moment, a condenser at the top of the crude HF degassing tower is added, the intermediate working medium firstly obtains heat from the condenser at the top of the crude HF degassing tower, then releases the obtained heat from the reboiler at the bottom of the crude HF rectifying tower, and then returns to the condenser at the top of the crude HF degassing tower through an intermediate working medium circulating reflux pump to form an intermediate working medium heat exchange loop.
9. Energy-saving process according to claim 7 or 8, characterized in that the top temperature of the crude HF degassing column is always higher than the bottom temperature of the crude HF rectification column and a temperature difference of not less than 2 ℃ is maintained.
10. Energy-saving process according to claim 7 or 8, characterized in that the operating pressure of the crude HF degassing column is from 150kPaA to 1000 kPaA; the operating pressure of the crude HF rectification column is always lower than that of the crude HF degassing column and a pressure difference of not less than 20kPa is maintained.
11. An energy-saving method as claimed in claim 2 or 3, characterized in that an intermediate heat exchanger is additionally arranged on a pipeline for directly or indirectly supplying heat to a reboiler at the bottom of the crude HF degassing tower by material steam at the top of the crude HF rectifying tower, so as to supplement or remove the total heat transferred between the two rectifying towers and ensure the stable operation of the two towers.
12. The energy-saving method as claimed in claim 7 or 8, characterized in that an intermediate heat exchanger is additionally arranged on a pipeline for directly or indirectly supplying heat to a reboiler at the bottom of the crude HF rectifying tower by material steam at the top of the crude HF degassing tower, so as to supplement or remove total heat transferred between the two rectifying towers and ensure the stable operation of the two towers.
13. The energy-saving method as claimed in claim 3 or 8, wherein the intermediate working medium heat exchange loop is additionally provided with an intermediate working medium inlet and outlet branch for inflow or outflow of the intermediate working medium, thereby ensuring proper working medium flow and heat exchange amount and avoiding the occurrence of excessive or insufficient heat exchange amount of the intermediate working medium.
CN202110641002.9A 2021-06-09 2021-06-09 Energy-saving device and method for separating anhydrous hydrogen fluoride Pending CN113577811A (en)

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