CN108190838B - Hydrogen fluoride multiphase gasification separation recovery system - Google Patents
Hydrogen fluoride multiphase gasification separation recovery system Download PDFInfo
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- CN108190838B CN108190838B CN201810087628.8A CN201810087628A CN108190838B CN 108190838 B CN108190838 B CN 108190838B CN 201810087628 A CN201810087628 A CN 201810087628A CN 108190838 B CN108190838 B CN 108190838B
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- 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
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- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/002—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by condensation
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Abstract
The invention provides a hydrogen fluoride multiphase gasification separation recovery system which is used for treating hydrofluoric acid waste liquid and comprises a solid collecting system, a gas treatment system, a liquid collecting system and a sulfuric acid concentration system; the solid collecting system comprises a raw material tank, a gasification cyclone separation tower and a sodium fluoride high-temperature purifier; the raw material tank is communicated with the gasification cyclone separation tower through a feeding pipeline, a feeding pump, a flow meter and a high-temperature gasification reactor are arranged on the feeding pipeline, and the high-temperature gasification reactor is arranged at the top of the gasification cyclone separation tower; and the feeding pump is used for metering hydrofluoric acid waste liquid in the raw material tank by the flowmeter, pumping the hydrofluoric acid waste liquid into the high-temperature gasification reactor, carrying out instant gasification, and feeding the gasified hydrofluoric acid waste liquid into the gasification cyclone separation tower.
Description
Technical Field
The invention relates to the field of industrial post-treatment, in particular to the field of hydrogen fluoride recovery in hydrofluoric acid waste liquid.
Background
The existing production processes of fluorobenzene, p-fluorotoluene and o-fluorotoluene are all anhydrous hydrogen fluoride methods, reaction residual liquid is generated due to excessive addition of anhydrous hydrogen fluoride in the production process, and the residual liquid consists of more than 60% of hydrogen fluoride, about 20% of sodium fluoride and about 10% of water. The original recovery process adopts a concentrated sulfuric acid replacement method to produce a large amount of waste sulfuric acid liquid and waste sodium bisulfate, which is extremely difficult to treat and causes great environmental protection pressure for enterprises.
Meanwhile, the conventional recovery process cannot completely replace all the components, so that complete separation cannot be realized, recycling cannot be realized, and secondary pollution and the like occur.
Aiming at the situation, the invention adopts a brand new technical mode to treat the residual liquid, and well solves the problems of hydrogen fluoride recovery and environmental protection. Firstly, all the components of anhydrous hydrogen fluoride, water, organic matters and the like are gasified into gas phase in a closed cycle mode, salts in the residual liquid are separated out in a solid form, and secondly, the water and the organic matters in the gas phase are all trapped in concentrated sulfuric acid through the concentrated sulfuric acid to realize gas-liquid separation. And finally, the gas phase component is an anhydrous hydrogen fluoride product, the anhydrous hydrogen fluoride product is recovered in a freezing mode, and the diluted sulfuric acid is continuously concentrated to the original concentration through a sulfuric acid concentration device for cyclic application.
Disclosure of Invention
The invention provides a hydrogen fluoride multiphase gasification separation recovery system which is used for treating hydrofluoric acid waste liquid and comprises a solid collecting system, a gas treatment system, a liquid collecting system and a sulfuric acid concentration system;
the solid collecting system comprises a raw material tank, a gasification cyclone separation tower and a sodium fluoride high-temperature purifier;
the raw material tank is communicated with the gasification cyclone separation tower through a feeding pipeline, a feeding pump, a flow meter and a high-temperature gasification reactor are arranged on the feeding pipeline, and the high-temperature gasification reactor is arranged at the top of the gasification cyclone separation tower; the feeding pump is used for metering hydrofluoric acid waste liquid in the raw material tank through a flowmeter, pumping the hydrofluoric acid waste liquid into the high-temperature gasification reactor, carrying out instant gasification, and feeding the gasified hydrofluoric acid waste liquid into the gasification cyclone separation tower;
the bottom of the gasification cyclone separation tower is provided with a sealed discharging device, and the sealed discharging device is connected with the high-temperature sodium fluoride purifier through a solid pipeline; after the gasified hydrofluoric acid waste liquid is separated by a gasification cyclone separation tower, the solid is discharged into a high-temperature sodium fluoride purifier through a sealed discharging device, so that the collection of the solid is realized;
the gas treatment system and the liquid collection system comprise a raw material tank, a gas cyclone separation tower, a dust removal system, a heating diffuser, a condensation system and a purification system;
the dust removal system is communicated with a heating diffuser through a circulating fan and a circulating pipeline, and the heating diffuser is communicated with an inlet at the top of the gasification cyclone separation tower;
the circulating pipeline is divided into a main pipeline and a branch pipeline; the main pipeline is provided with a distributor, and the branch pipeline is provided with a gas phase flow distributor; the main pipeline is connected with the heating diffuser, and the branch pipeline is connected with the condensing system;
the hydrofluoric acid waste liquid in the raw material tank is gasified by a high-temperature gasification reactor and then enters a gasification cyclone separation tower, and after gas-solid separation, the gas passes through a dust removal system through a gas pipeline; most of the gas treated by the dust removal system returns to the gas cyclone separation tower through the main pipeline, and the small part of the gas enters the condensation system through the branch pipeline; the circulating fan provides circulating power and distributes gas phase in real time through the distributor and the gas phase flow distributor;
the gas phase entering the condensing system is condensed by a contact type condensation dehydration tower, a primary condenser, a first-stage condenser, a second-stage condenser and a third-stage condenser to obtain pure gas phase, and the pure gas phase is purified by a purifying system and then is discharged at high altitude;
the primary condenser is arranged at the top of the contact type condensation dehydration tower;
the bottom of the contact type condensation dehydration tower is provided with a concentrated sulfuric acid circulating tank for collecting a concentrated sulfuric acid crude liquid; the bottoms of the I-stage condenser, the II-stage condenser and the III-stage condenser are connected with an anhydrous hydrogenated fluorine collecting tank through condensing pipelines and are used for collecting the anhydrous hydrogenated fluorine collecting tank in a gas phase; the purification tower is connected with the aqueous acid tank through a purification pipeline and is used for collecting hydrofluoric acid in a gas phase;
the sulfuric acid concentration system comprises a sulfuric acid evaporator, an evaporation chamber, a tail gas condenser, a condensate tank and a sulfuric acid cooler;
the concentrated sulfuric acid circulating tank sends a part of concentrated sulfuric acid to the top of the contact type condensation dehydration tower through a sulfuric acid circulating pump for atomization spraying; pumping the other part of concentrated sulfuric acid into a sulfuric acid evaporator and an evaporation chamber by the sulfuric acid circulating pump, and evaporating water absorbed by the concentrated sulfuric acid in the drying process by the sulfuric acid evaporator and the evaporation chamber through temperature rise; the evaporated water vapor enters a tail gas condenser to be condensed and enters a condensation tank; the sulfuric acid after the evaporation concentration enters a concentrated sulfuric acid circulating tank after being cooled by a sulfuric acid cooler.
As an embodiment of the invention, the dust removal system comprises a high-efficiency cyclone dust collector and a bag-type dust collector.
As an embodiment of the present invention, the purification system includes a purification tower, a water wash tower, and a caustic wash tower.
As an embodiment of the present invention, the gas treatment system further comprises a hot coal body heating furnace, and the hot coal body heating furnace is connected with the heating diffuser and is used for providing hot air for the heating diffuser.
As an implementation mode of the invention, the bottom parts of the high-efficiency cyclone dust collector and the bag-type dust collector are provided with sealed discharging devices, and the sealed discharging devices are communicated with the sodium fluoride high-temperature purifier.
As an embodiment of the present invention, the contact condensation dehydration tower uses cold water as a cold source.
As an embodiment of the invention, the I-stage condenser, the II-stage condenser and the III-stage condenser adopt frozen brine as cold sources.
As an embodiment of the present invention, the sulfuric acid evaporator and the evaporation chamber use hot oil as a heat source.
As an embodiment of the present invention, the tail gas condenser and the sulfuric acid cooler use cold water as a cooling source.
As an embodiment of the present invention, the sulfuric acid concentration device further comprises a vacuum unit.
Has the advantages that:
the whole device provided by the invention has no secondary pollution, and can recover anhydrous hydrogen fluoride and sodium fluoride products in a mode of achieving low operation cost through reasonable energy distribution, thereby thoroughly solving the environmental protection problem of producing fluorobenzene, p-fluorotoluene and o-fluorotoluene by an anhydrous hydrogen fluoride method.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
FIG. 1: a schematic of the equipment connections of the solids collection system;
FIG. 2: a schematic diagram of the equipment connections of the gas treatment system and the liquid collection system;
FIG. 3: the equipment connection of the sulfuric acid concentration system is schematic.
Description of the symbols:
a raw material tank-1, a feed pump-2, a flow meter-3, a high-temperature gasification reactor-4, a gasification cyclone separation tower-5, a sealed unloading device-6, a sodium fluoride high-temperature purifier-7, a high-efficiency cyclone dust collector-8, a bag-type dust collector-9, a circulating fan-10, a heating diffuser-11, a hot coal body heating furnace-12, a contact type condensation dehydration tower-13, a primary condenser-14, a I-stage condenser-15, a II-stage condenser-16, a III-stage condenser-17, an anhydrous hydrogen fluoride collecting tank-18, a purifying tower-19, an aqueous acid tank-20, a circulating pump-21, a water washing tower-22, a fan-23, an alkaline washing tower-24, a concentrated sulfuric acid circulating tank-25, a sulfuric acid evaporator-26, a water-vapor separator-26, a water, An evaporation chamber-27, a tail gas condenser-28, a sulfuric acid cooler-29, a condensate tank-30, a condensate pump-31, a vacuum unit-32,
A feeding pipeline-33, a solid pipeline-34, a gas pipeline-35, a circulating pipeline-36, a distributor-37, a gas phase flow distributor-38, a hot air pipeline-39, a condensing pipeline-40, a sulfuric acid pipeline-41, a circulating pipeline-36, a circulating pipeline-37, a gas phase flow distributor-38, a hot air pipeline-39, a condensing pipeline-40, a sulfuric acid pipeline-41,
a frozen brine return pipeline-42, a cold water return pipeline-43, a hot oil return pipeline-44 and a sulfuric acid circulating pump-45
Detailed Description
The disclosure may be understood more readily by reference to the following detailed description of preferred embodiments of the invention and the examples included therein. 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 invention belongs. In case of conflict, the present specification, including definitions, will control.
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, 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 invention.
It will be understood by those skilled in the art that, unless otherwise defined, all terms (including technical and scientific terms) used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. It will be further understood that terms, such as those defined in commonly used dictionaries, should be interpreted as having a meaning that is consistent with their meaning in the context of the prior art and will not be interpreted in an idealized or overly formal sense unless expressly so defined herein.
The meaning of "and/or" in the present invention means that the respective single or both of them exist individually or in combination.
The meaning of "inside and outside" in the present invention means that the direction pointing to the inside of the device is inside and vice versa with respect to the device itself, and is not a specific limitation of the mechanism of the apparatus of the present invention.
The meaning of "left and right" in the present invention means that when the reader is facing the drawings, the left side of the reader is left, and the right side of the reader is right, and is not a specific limitation on the mechanism of the apparatus of the present invention.
The term "connected" as used herein may mean either a direct connection between the components or an indirect connection between the components via other components.
The invention provides a hydrogen fluoride multiphase gasification separation recovery system which is used for treating hydrofluoric acid waste liquid and comprises a solid collecting system, a gas treatment system, a liquid collecting system and a sulfuric acid concentration system;
the solid collecting system comprises a raw material tank, a gasification cyclone separation tower and a sodium fluoride high-temperature purifier;
the raw material tank is communicated with the gasification cyclone separation tower through a feeding pipeline, a feeding pump, a flow meter and a high-temperature gasification reactor are arranged on the feeding pipeline, and the high-temperature gasification reactor is arranged at the top of the gasification cyclone separation tower; the feeding pump is used for metering hydrofluoric acid waste liquid in the raw material tank through a flowmeter, pumping the hydrofluoric acid waste liquid into the high-temperature gasification reactor, carrying out instant gasification, and feeding the gasified hydrofluoric acid waste liquid into the gasification cyclone separation tower;
the bottom of the gasification cyclone separation tower is provided with a sealed discharging device, and the sealed discharging device is connected with the high-temperature sodium fluoride purifier through a solid pipeline; after the gasified hydrofluoric acid waste liquid is separated by a gasification cyclone separation tower, the solid is discharged into a high-temperature sodium fluoride purifier through a sealed discharging device, so that the collection of the solid is realized;
the gas treatment system comprises a raw material tank, a gas cyclone separation tower, a dust removal system, a heating diffuser, a condensation system and a purification system;
the dust removal system is communicated with a heating diffuser through a circulating fan and a circulating pipeline, and the heating diffuser is communicated with an inlet at the top of the gasification cyclone separation tower;
the circulating pipeline is divided into a main pipeline and a branch pipeline; the main pipeline is provided with a distributor, and the branch pipeline is provided with a gas phase flow distributor; the main pipeline is connected with the heating diffuser, and the branch pipeline is connected with the condensing system;
the hydrofluoric acid waste liquid in the raw material tank is gasified by a high-temperature gasification reactor and then enters a gasification cyclone separation tower, and after gas-solid separation, the gas passes through a dust removal system through a gas pipeline; most of the gas treated by the dust removal system returns to the gas cyclone separation tower through the main pipeline, and the small part of the gas enters the condensation system through the branch pipeline; the circulating fan provides circulating power and distributes gas phase in real time through the distributor and the gas phase flow distributor;
the condensation system comprises a contact type condensation dehydration tower, a primary condenser, a first-stage condenser, a second-stage condenser and a third-stage condenser;
the gas phase entering the condensing system is condensed by a contact type condensation dehydration tower, a primary condenser, a first-stage condenser, a second-stage condenser and a third-stage condenser to obtain pure gas phase, and the pure gas phase is purified by a purifying system and then is discharged at high altitude;
the primary condenser is arranged at the top of the contact type condensation dehydration tower;
the bottom of the contact type condensation dehydration tower is provided with a concentrated sulfuric acid circulating tank for collecting a concentrated sulfuric acid crude liquid; the bottoms of the I-stage condenser, the II-stage condenser and the III-stage condenser are connected with an anhydrous hydrogenated fluorine collecting tank through condensing pipelines and are used for collecting the anhydrous hydrogenated fluorine collecting tank in a gas phase; the purification tower is connected with the aqueous acid tank through a purification pipeline and is used for collecting hydrofluoric acid in a gas phase;
the sulfuric acid concentration system comprises a sulfuric acid evaporator, an evaporation chamber, a tail gas condenser, a condensate tank and a sulfuric acid cooler;
the concentrated sulfuric acid circulating tank sends a part of concentrated sulfuric acid to the top of the contact type condensation dehydration tower through a sulfuric acid circulating pump for atomization spraying; pumping the other part of concentrated sulfuric acid into a sulfuric acid evaporator and an evaporation chamber by the sulfuric acid circulating pump, and evaporating water absorbed by the concentrated sulfuric acid in the drying process by the sulfuric acid evaporator and the evaporation chamber through temperature rise; the evaporated water vapor enters a tail gas condenser to be condensed and enters a condensation tank; the sulfuric acid after the evaporation concentration enters a concentrated sulfuric acid circulating tank after being cooled by a sulfuric acid cooler.
As an embodiment of the invention, the dust removal system comprises a high-efficiency cyclone dust collector and a bag-type dust collector.
As an embodiment of the present invention, the purification system includes a purification tower, a water wash tower, and a caustic wash tower.
As an embodiment of the present invention, the gas treatment system further comprises a hot coal body heating furnace, and the hot coal body heating furnace is connected with the heating diffuser and is used for providing hot air for the heating diffuser.
As an implementation mode of the invention, the bottom parts of the high-efficiency cyclone dust collector and the bag-type dust collector are provided with sealed discharging devices, and the sealed discharging devices are communicated with the sodium fluoride high-temperature purifier.
As an embodiment of the present invention, the contact condensation dehydration tower uses cold water as a cold source.
As an embodiment of the invention, the I-stage condenser, the II-stage condenser and the III-stage condenser adopt frozen brine as cold sources.
As an embodiment of the present invention, the sulfuric acid evaporator and the evaporation chamber use hot oil as a heat source.
As an embodiment of the present invention, the tail gas condenser and the sulfuric acid cooler use cold water as a cooling source.
As an embodiment of the present invention, the sulfuric acid concentration device further comprises a vacuum unit.
A second aspect of the present invention provides an apparatus for the hydrogen fluoride heterogeneous gasification separation recovery system, the apparatus comprising: raw material tank, charge pump, flowmeter, high-temperature gasification reactor, gasification cyclone separation tower, sealed discharge device, sodium fluoride high-temperature purifier, high-efficiency cyclone dust collector, bag-type dust collector, circulating fan, heating diffuser, hot coal body heating furnace, contact condensation dehydration tower, primary condenser, I-grade condenser, II-grade condenser, III-grade condenser, anhydrous hydrogen fluoride collecting tank, purifying tower, aqueous acid tank, circulating pump, water scrubber, fan, alkaline tower, concentrated sulfuric acid circulating tank, sulfuric acid evaporator, evaporation chamber, tail gas condenser, sulfuric acid cooler, water condensing tank, water condensing pump and vacuum unit.
As an embodiment of the invention, the raw material tank is connected with a high-temperature gasification reactor through a feeding pipeline, the high-temperature gasification reactor is arranged at the top of the gasification cyclone separation tower, and a feeding pump and a flow meter are arranged on the feeding pipeline;
the bottom parts of the gasification cyclone separation tower, the high-efficiency cyclone dust collector and the bag-type dust collector are provided with sealed discharging devices, and the sealed discharging devices are connected with the sodium fluoride high-temperature purifier through solid pipelines;
the gasification cyclone separation tower is connected with the top of a high-efficiency cyclone dust collector through a gas pipeline, and the high-efficiency cyclone dust collector is connected with a bag-type dust collector through a gas pipeline;
the top of the bag-type dust collector is connected with a circulating fan through a gas pipeline, the circulating fan is respectively connected with a heating diffuser and a contact type condensation dehydration tower through circulating pipelines, and a distributor and a gas phase flow distributor are respectively arranged on the circulating pipelines;
the heating diffuser is connected with the top of the gasification cyclone separation tower through a gas pipeline, and the hot coal body heating furnace is connected with the heating diffuser through a hot air pipeline;
the bottom of the contact type condensation dehydration tower is provided with a concentrated sulfuric acid circulating tank, the top of the contact type condensation dehydration tower is provided with a primary condenser, the primary condenser is sequentially connected with a first-level condenser, a second-level condenser and a third-level condenser through condensing pipelines,
the bottom parts of the first-stage condenser, the second-stage condenser and the third-stage condenser are connected with an anhydrous hydrogen fluoride collecting tank, and the top parts of the first-stage condenser, the second-stage condenser and the third-stage condenser are connected with a purification tower through gas pipelines; the bottom of the purification tower is connected with an aqueous acid tank; the tower top of the purification tower is connected with the water washing tower, and the tower top of the water washing tower is connected with the alkaline washing tower.
The concentrated sulfuric acid circulating tank is respectively connected with a sulfuric acid evaporator and an evaporation chamber through a sulfuric acid pipeline, the top of the evaporation chamber is connected with a tail gas condenser through a gas pipeline, and the tail gas condenser transports condensed water into a condensate tank through a vacuum unit; the condensate pump transports the condensate water in the condensate tank for use.
The third aspect of the invention provides the hydrogen fluoride multiphase gasification separation process, which comprises a heating stage, a gas-solid separation stage, a gas-liquid separation stage and a sulfuric acid concentration stage;
heating the hydrofluoric acid waste liquid by a high-temperature gasification reactor, carrying out primary gas-solid separation by a gasification cyclone separation tower after instantaneous gasification, carrying out secondary gas-solid separation on gas by a high-efficiency cyclone dust collector and a bag-type dust collector, and collecting the separated solid into a sodium fluoride high-temperature purifier by a sealed discharging device; most of the gas after the gas-solid separation again enters the heating diffuser through gas phase circulation and is heated and circulated again to the gasification cyclone separation tower; a small part of gas after the gas-solid separation again enters a gas-liquid separation stage through a gas-phase flow distributor;
the gas entering the gas-liquid separation stage is subjected to primary dehydration through a contact type condensation dehydration tower and then is subjected to multiple condensation through a primary condenser, a first-stage condenser, a second-stage condenser and a third-stage condenser;
after the anhydrous hydrogen fluoride liquid is separated from the gas subjected to multiple condensation, the gas passes through a purification tower, a water washing tower and an alkali washing tower to complete the final evolution process, and then the gas is discharged at high altitude;
the bottom of the purification tower is connected with an aqueous acid tank for collecting hydrofluoric acid liquid separated by the purification tower.
And a concentrated sulfuric acid circulating tank is installed at the bottom of the contact type condensation dehydration tower, and concentrated sulfuric acid in the concentrated sulfuric acid circulating tank is lifted to the top of the contact type condensation dehydration tower through a sulfuric acid circulating pump for atomization spraying.
And concentrating the concentrated sulfuric acid subjected to dehydration treatment in the concentrated sulfuric acid circulating tank by using a sulfuric acid concentration process.
The sulfuric acid concentration process comprises the following steps:
(1) heating and evaporating sulfuric acid in a concentrated sulfuric acid circulating tank to generate steam;
(2) condensing the water vapor in the step (1), and collecting condensed water;
(3) and (3) cooling the dehydrated concentrated sulfuric acid heated in the step (1), and conveying the concentrated sulfuric acid back to a concentrated sulfuric acid circulating tank.
The flow rate of the hydrogen fluoride multiphase gasification separation process is 500 kg/h.
The heating diffuser heats air through the hot coal body heating furnace to provide a hot air source.
The invention adopts a brand new technical mode to treat the residual liquid, and well solves the problems of hydrogen fluoride recovery and environmental protection. The hydrogen fluoride multiphase gasification separation and recovery device comprises a high-temperature gasification reactor, a rotational flow gas-solid separator, a heat supply system, a solid discharger, a gas phase purifier, a heat source circulating system, a gas phase drying device and a gas phase refrigerating device.
The high-temperature gasification reactor is connected with the rotational flow gas-solid separator to ensure that gas phase and solid phase in the residual liquid are effectively separated, the heat supply system provides heat energy required by the gasification reaction, and the gas phase after the gas-solid separation sequentially enters the gas phase purifier, the heat source circulating system, the gas phase drying device and the gas phase refrigerating device to form liquid anhydrous hydrogen fluoride. All the devices are connected by pipelines. The solid is discharged into a high-temperature purification device at the bottom of the cyclone gas-solid separator through a solid discharger which completely seals the gas phase, and is further purified into a byproduct.
The hydrogen fluoride multiphase gasification separation and recovery system of the present invention will be described in detail with reference to the accompanying drawings.
FIG. 1:
the invention provides a hydrogen fluoride multiphase gasification separation and recovery system which is used for treating hydrofluoric acid waste liquid and comprises a solid collecting system, a gas treatment system, a liquid collecting system and a sulfuric acid concentrating system, wherein the solid collecting system is shown in figure 1.
As shown in fig. 1, the solids collection system comprises: the device comprises a raw material tank 1, a feed pump 2, a flowmeter 3, a high-temperature gasification reactor 4, a gasification cyclone separation tower 5, a sealed discharging device 6, a sodium fluoride high-temperature purifier 7, a high-efficiency cyclone dust collector 8, a bag-type dust collector 9, a circulating fan 10, a heating diffuser 11 and a hot coal body heating furnace 12.
The raw material tank 1 is connected with a high-temperature gasification reactor 4 through a feeding pipeline 33, the high-temperature gasification reactor 4 is arranged at the top of a gasification cyclone separation tower 5, and a feeding pump 2 and a flow meter 3 are arranged on the feeding pipeline 33;
the bottom parts of the gasification cyclone separation tower 5, the high-efficiency cyclone dust collector 8 and the bag-type dust collector 9 are provided with a sealed discharging device 6, and the sealed discharging device 6 is connected with the sodium fluoride high-temperature purifier 7 through a solid pipeline 34;
the gasification cyclone separation tower 5 is connected with the top of a high-efficiency cyclone dust collector 8 through a gas pipeline 35, and the high-efficiency cyclone dust collector 8 is connected with a bag-type dust collector 9 through the gas pipeline 35;
the top of the bag-type dust collector 9 is connected with a circulating fan 10 through a gas pipeline 35, the circulating fan 10 is respectively connected with a heating diffuser 11 and a contact type condensation dehydration tower 13 through a circulating pipeline 36, and a distributor 37 and a gas phase flow distributor 38 are respectively arranged on the circulating pipeline 36;
the heating diffuser 11 is connected with the top of the gasification cyclone separation tower 5 through a gas pipeline 35, and the hot coal body heating furnace 12 is connected with the heating diffuser 11 through a hot air pipeline 39.
The raw material tank 1 is communicated with the gasification cyclone separation tower 5 through a feeding pipeline 33, hydrofluoric acid waste liquid in the raw material tank is metered by a feeding pump 2 through a flowmeter 3 and then pumped into a high-temperature gasification reactor 4 for instantaneous gasification, and the gasified hydrofluoric acid waste liquid enters the gasification cyclone separation tower 5; after the gasified hydrofluoric acid waste liquid is separated by the gasification cyclone separation tower 5, the solid is discharged into the high-temperature sodium fluoride purifier 7 through the sealed discharging device 6, and the collection of the solid is realized.
FIG. 2 is a drawing:
the invention provides a hydrogen fluoride multiphase gasification separation and recovery system which is used for treating hydrofluoric acid waste liquid and comprises a solid collecting system, a gas treating system, a liquid collecting system and a sulfuric acid concentrating system, wherein the gas collecting system and the liquid collecting system are shown in figure 1.
As shown in figures 1 and 2 of the drawings,
the gas treatment system and the liquid collection system comprise a raw material tank 1, a gas cyclone separation tower 5, a dust removal system, a heating diffuser 11, a condensation system and a purification system;
the dust removal system comprises a high-efficiency cyclone dust collector 8 and a bag-type dust collector 9;
the purification system comprises a purification tower 19, a water washing tower 22 and an alkaline washing tower 24;
the condensation system comprises a contact condensation dehydration tower 13, a primary condenser 14, a first-stage condenser 15, a second-stage condenser 16 and a third-stage condenser 17;
a concentrated sulfuric acid circulating tank 25 is arranged at the bottom of the contact type condensation dehydration tower 13, a primary condenser 14 is arranged at the top of the contact type condensation dehydration tower 13, the primary condenser is sequentially connected with a first-stage condenser 15, a second-stage condenser 16 and a third-stage condenser 17 through a condensing pipeline 40,
the bottom parts of the I-stage condenser 15, the II-stage condenser 16 and the III-stage condenser 17 are connected with an anhydrous hydrogen fluoride collecting tank 18, and the top parts of the I-stage condenser 15, the II-stage condenser 16 and the III-stage condenser 17 are connected with a purifying tower 19 through a gas pipeline 35; the bottom of the purification tower 19 is connected with an aqueous acid tank 20; the top of the purification tower 19 is connected with a water scrubber 22, and the top of the water scrubber 22 is connected with a caustic wash tower 24.
The dedusting system is communicated with a heating diffuser 11 through a circulating fan 10 and a circulating pipeline 36, and the heating diffuser 11 is communicated with the top inlet of the gasification cyclone separation tower 5;
the circulating pipeline 36 is divided into a main pipeline and a branch pipeline; the main pipeline is provided with a distributor 37, and the branch pipeline is provided with a gas phase flow distributor 38; the main pipeline is connected with the heating diffuser 11, and the branch pipeline is connected with the condensing system;
the hydrofluoric acid waste liquid in the raw material tank is gasified by a high-temperature gasification reactor and then enters a gasification cyclone separation tower, and after gas-solid separation, the gas passes through a dust removal system through a gas pipeline; most of the gas treated by the dust removal system returns to the gas cyclone separation tower through the main pipeline, and the small part of the gas enters the condensation system through the branch pipeline; the circulating fan provides circulating power and distributes gas phase in real time through the distributor and the gas phase flow distributor;
the gas phase entering the condensing system is condensed by a contact type condensation dehydration tower, a primary condenser, a first-stage condenser, a second-stage condenser and a third-stage condenser to obtain pure gas phase, and the pure gas phase is purified by a purifying system and then is discharged at high altitude;
the bottom of the contact type condensation dehydration tower is provided with a concentrated sulfuric acid circulating tank for collecting a concentrated sulfuric acid crude liquid; the bottoms of the I-stage condenser, the II-stage condenser and the III-stage condenser are connected with an anhydrous hydrogenated fluorine collecting tank through condensing pipelines and are used for collecting the anhydrous hydrogenated fluorine collecting tank in a gas phase; the purification tower is connected with the aqueous acid tank through a purification pipeline and is used for collecting hydrofluoric acid in gas phase.
Heating the hydrofluoric acid waste liquid by a high-temperature gasification reactor, carrying out primary gas-solid separation by a gasification cyclone separation tower after instantaneous gasification, carrying out secondary gas-solid separation on gas by a high-efficiency cyclone dust collector and a bag-type dust collector, and collecting the separated solid into a sodium fluoride high-temperature purifier by a sealed discharging device; most of the gas after the gas-solid separation again enters the heating diffuser through gas phase circulation and is heated and circulated again to the gasification cyclone separation tower; a small part of gas after the gas-solid separation again enters a gas-liquid separation stage through a gas-phase flow distributor;
the gas entering the gas-liquid separation stage is subjected to primary dehydration through a contact type condensation dehydration tower and then is subjected to multiple condensation through a primary condenser, a first-stage condenser, a second-stage condenser and a third-stage condenser;
after the anhydrous hydrogen fluoride liquid is separated from the gas subjected to multiple condensation, the gas passes through a purification tower, a water washing tower and an alkali washing tower to complete the final evolution process, and then the gas is discharged at high altitude;
the bottom of the purification tower is connected with an aqueous acid tank for collecting hydrofluoric acid liquid separated by the purification tower.
And a concentrated sulfuric acid circulating tank is installed at the bottom of the contact type condensation dehydration tower, and concentrated sulfuric acid in the concentrated sulfuric acid circulating tank is lifted to the top of the contact type condensation dehydration tower through a sulfuric acid circulating pump for atomization spraying.
FIG. 3:
the invention provides a hydrogen fluoride multiphase gasification separation and recovery system which is used for treating hydrofluoric acid waste liquid and comprises a solid collecting system, a gas treating system, a liquid collecting system and a sulfuric acid concentrating system, wherein the sulfuric acid concentrating system is shown in figure 3.
The sulfuric acid concentration system comprises a concentrated sulfuric acid circulating tank 25, a sulfuric acid evaporator 26, an evaporation chamber 27, a tail gas condenser 28, a sulfuric acid cooler 29, a water condensation tank 30, a water condensation pump 31 and a vacuum unit 32.
The concentrated sulfuric acid circulating tank 25 is respectively connected with a sulfuric acid evaporator 26 and an evaporation chamber 27 through a sulfuric acid pipeline 41, the top of the evaporation chamber 27 is connected with a tail gas condenser 28 through a gas pipeline 35, and the tail gas condenser 28 transports condensed water into a water condensing tank 30 through a vacuum unit 32; the condensate pump 31 transports the condensate water in the condensate tank 30 for use.
The concentrated sulfuric acid circulating tank 25 sends a part of concentrated sulfuric acid to the top of the contact condensation dehydration tower 13 through a sulfuric acid circulating pump 45 for atomization spraying; the sulfuric acid circulating pump 45 pumps the other part of the concentrated sulfuric acid into the sulfuric acid evaporator 26 and the evaporation chamber 27, and the sulfuric acid evaporator 26 and the evaporation chamber 27 evaporate water absorbed by the concentrated sulfuric acid in the drying process through temperature rise; the evaporated water vapor enters a tail gas condenser 28 to be condensed and enters a condensation tank 30; the sulfuric acid after the evaporation concentration is cooled by a sulfuric acid cooler 29 and then enters a concentrated sulfuric acid circulating tank 25.
And concentrating the concentrated sulfuric acid subjected to dehydration treatment in the concentrated sulfuric acid circulating tank by using a sulfuric acid concentration process.
The sulfuric acid concentration process comprises the following steps:
(1) heating and evaporating sulfuric acid in a concentrated sulfuric acid circulating tank to generate steam;
(2) condensing the water vapor in the step (1), and collecting condensed water;
(3) and (3) cooling the dehydrated concentrated sulfuric acid heated in the step (1), and conveying the concentrated sulfuric acid back to a concentrated sulfuric acid circulating tank.
Other variations and modifications to the specific embodiments described above will be apparent to those skilled in the art, which will be within the spirit and scope of the invention. Although the present invention has been described in relation to particular embodiments thereof, which are intended to be illustrative and not restrictive, the scope of the invention is not to be limited to the specific embodiments shown and described herein, nor is it limited to any specific form or manner which is inconsistent with the progress in the art and that which is believed to be achieved by the invention.
Claims (9)
1. A hydrogen fluoride multiphase gasification separation recovery system is used for treating hydrofluoric acid waste liquid and is characterized by comprising a solid collecting system, a gas treatment system, a liquid collecting system and a sulfuric acid concentrating system;
the solid collecting system comprises a raw material tank, a gasification cyclone separation tower and a sodium fluoride high-temperature purifier;
the raw material tank is communicated with the gasification cyclone separation tower through a feeding pipeline, a feeding pump, a flow meter and a high-temperature gasification reactor are arranged on the feeding pipeline, and the high-temperature gasification reactor is arranged at the top of the gasification cyclone separation tower; the feeding pump is used for metering hydrofluoric acid waste liquid in the raw material tank through a flowmeter, pumping the hydrofluoric acid waste liquid into the high-temperature gasification reactor, carrying out instant gasification, and feeding the gasified hydrofluoric acid waste liquid into the gasification cyclone separation tower;
the bottom of the gasification cyclone separation tower is provided with a sealed discharging device, and the sealed discharging device is connected with the sodium fluoride high-temperature purifier through a solid pipeline; after the gasified hydrofluoric acid waste liquid is separated by a gasification cyclone separation tower, the solid is discharged into a sodium fluoride high-temperature purifier through a sealed discharging device, so that the collection of the solid is realized;
the gas treatment system and the liquid collection system comprise a raw material tank, a gasification cyclone separation tower, a dust removal system, a heating diffuser, a condensation system and a purification system;
the dust removal system is communicated with a heating diffuser through a circulating fan and a circulating pipeline, and the heating diffuser is communicated with an inlet at the top of the gasification cyclone separation tower;
the circulating pipeline is divided into a main pipeline and a branch pipeline; the main pipeline is provided with a distributor, and the branch pipeline is provided with a gas phase flow distributor; the main pipeline is connected with the heating diffuser, and the branch pipeline is connected with the condensing system;
the hydrofluoric acid waste liquid in the raw material tank is gasified by a high-temperature gasification reactor and then enters a gasification cyclone separation tower, and after gas-solid separation, the gas passes through a dust removal system through a gas pipeline; most of the gas treated by the dust removal system returns to the gasification cyclone separation tower through the main pipeline, and the small part of the gas enters the condensation system through the branch pipeline; the circulating fan provides circulating power and distributes gas phase in real time through the distributor and the gas phase flow distributor;
the gas phase entering the condensing system is condensed by a contact type condensation dehydration tower, a primary condenser, a first-stage condenser, a second-stage condenser and a third-stage condenser to obtain pure gas phase, and the pure gas phase is purified by a purifying system and then is discharged at high altitude;
the primary condenser is arranged at the top of the contact type condensation dehydration tower;
the bottom of the contact type condensation dehydration tower is provided with a concentrated sulfuric acid circulating tank for collecting a concentrated sulfuric acid crude liquid; the bottoms of the I-stage condenser, the II-stage condenser and the III-stage condenser are connected with an anhydrous hydrogen fluoride collecting tank through condensing pipelines and are used for collecting the anhydrous hydrogen fluoride collecting tank in a gas phase; the purification tower is connected with the aqueous acid tank through a purification pipeline and is used for collecting hydrofluoric acid in a gas phase;
the sulfuric acid concentration system comprises a concentrated sulfuric acid circulating tank, a sulfuric acid evaporator, an evaporation chamber, a tail gas condenser, a sulfuric acid cooler, a water condensation tank, a water condensation pump and a vacuum unit;
the concentrated sulfuric acid circulating tank is respectively connected with a sulfuric acid evaporator and an evaporation chamber through a sulfuric acid pipeline, the top of the evaporation chamber is connected with a tail gas condenser through a gas pipeline, and the tail gas condenser transports condensed water into a condensate tank through a vacuum unit; the condensate pump transports the condensate water in the condensate tank out for use;
the concentrated sulfuric acid circulating tank sends a part of concentrated sulfuric acid to the top of the contact type condensation dehydration tower through a sulfuric acid circulating pump for atomization spraying; pumping the other part of concentrated sulfuric acid into a sulfuric acid evaporator and an evaporation chamber by the sulfuric acid circulating pump, and evaporating water absorbed by the concentrated sulfuric acid in the drying process by the sulfuric acid evaporator and the evaporation chamber through temperature rise; the evaporated water vapor enters a tail gas condenser to be condensed and enters a condensation tank; the sulfuric acid which is finished by evaporation concentration passes through.
2. The multiphase gasification separation recovery system of hydrogen fluoride according to claim 1, wherein the dust removal system comprises a high-efficiency cyclone dust collector and a bag-type dust collector.
3. The heterogeneous gasification separation recovery system of hydrogen fluoride of claim 1, wherein the purification system comprises a purification tower, a water scrubber and a caustic scrubber.
4. The multiphase gasification separation recovery system for hydrogen fluoride of claim 1, wherein the gas treatment system further comprises a heating medium heating furnace, the heating medium heating furnace is connected with the heating diffuser and is used for providing hot air for the heating diffuser.
5. The multi-phase gasification separation recovery system of hydrogen fluoride as claimed in claim 2, wherein the bottom of the high efficiency cyclone dust collector and the bag-type dust collector is provided with a sealed discharge device, and the sealed discharge device is communicated with the high temperature sodium fluoride purifier.
6. The multiphase gasification separation recovery system of hydrogen fluoride as recited in claim 1, wherein the contact type condensation dehydration tower uses cold water as a cooling source.
7. The multi-phase gasification separation recovery system of claim 1, wherein the first, second and third stage condensers use chilled brine as a cooling source.
8. The multiphase gasification separation recovery system of hydrogen fluoride as recited in claim 1, wherein the sulfuric acid evaporator and the evaporation chamber use hot oil as a heat source.
9. The multiphase gasification separation recovery system for hydrogen fluoride as recited in claim 1, wherein the tail gas condenser and the sulfuric acid cooler use cold water as a cooling source.
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| JP2006111487A (en) * | 2004-10-14 | 2006-04-27 | Mitsubishi Chemical Engineering Corp | Method for recovering hydrofluoric acid |
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| JP2006111487A (en) * | 2004-10-14 | 2006-04-27 | Mitsubishi Chemical Engineering Corp | Method for recovering hydrofluoric acid |
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