CN108190838A - A kind of hydrogen fluoride multiphase gasification separation recovery system - Google Patents

A kind of hydrogen fluoride multiphase gasification separation recovery system Download PDF

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Publication number
CN108190838A
CN108190838A CN201810087628.8A CN201810087628A CN108190838A CN 108190838 A CN108190838 A CN 108190838A CN 201810087628 A CN201810087628 A CN 201810087628A CN 108190838 A CN108190838 A CN 108190838A
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gasification
condenser
sulfuric acid
gas
tower
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CN201810087628.8A
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CN108190838B (en
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张海军
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Changzhou Anhai Chemical Engineering Technology Co Ltd
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Changzhou Anhai Chemical Engineering Technology Co Ltd
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    • 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
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D50/00Combinations of methods or devices for separating particles from gases or vapours
    • B01D50/20Combinations of devices covered by groups B01D45/00 and B01D46/00
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D53/00Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/002Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by condensation
    • 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
    • Y02P70/00Climate change mitigation technologies in the production process for final industrial or consumer products
    • Y02P70/10Greenhouse gas [GHG] capture, material saving, heat recovery or other energy efficient measures, e.g. motor control, characterised by manufacturing processes, e.g. for rolling metal or metal working

Abstract

The present invention provides a kind of hydrogen fluoride multiphase gasification separation recovery system, and for handling hydrofluoric acid waste liquid, the hydrogen fluoride multiphase gasification separation recovery system includes solids collection system, gas handling system, fluid collection systems and sulphuric acid concentration system;The solids collection system includes head tank, gasification swirl knockout tower and sodium fluoride high temperature purification device;The head tank is communicated by feed pipe and gasification cyclonic separation tower, feed pump, flowmeter and high-temperature gasification reactor is provided on the feed pipe, the high-temperature gasification reactor is arranged on the top of the gasification swirl knockout tower;Hydrofluoric acid waste liquid in head tank is pumped into high-temperature gasification reactor by the feed pump after flowmeter measures, and carries out transient evaporation, and gasification swirl knockout tower is entered after gasification.

Description

A kind of hydrogen fluoride multiphase gasification separation recovery system
Technical field
The present invention relates to industrial post processing fields, are more related to hydrogen fluoride recycling field in hydrofluoric acid waste liquid.
Background technology
The current production technology of fluorobenzene, p-fluorotoluene, o-fluorotobuene is anhydrous hydrogen fluoride method, because of anhydrous fluorine in production process Change excess hydrogen to add and generate reaction residue, it is about 20% that residual night composition is more than 60%, is fluorinated sodium content for hydrogen fluoride content, water Content is about 10%.Original recovery process uses concentrated sulfuric acid displacement method, generates a large amount of waste sulfuric acids and Waste Sulfuric Acid hydrogen sodium, it is extremely difficult to Processing, very big environmental protection pressure is caused to enterprise.
Meanwhile conventional recovery process completely can not all cement out ingredient, not only can not achieve complete Separation, can not recycled, there is situations such as secondary pollution.
For the above situation, the present invention handles above-mentioned raffinate using completely new technical approach, solves hydrogen fluoride well The problem of recycling and environmental protection.It is first by way of closed cycle that whole ingredients such as anhydrous hydrogen fluoride, moisture, organic matter are whole Gas phase is gasificated into, and the salt in raffinate is then separated in solid form, second step is will be in gas phase by the concentrated sulfuric acid All retention in concentrated sulfuric acid, realizes gas-liquid separation for water, organic matter.Last gaseous component is anhydrous hydrogen fluoride product, is passed through The mode of freezing recycles, and third step continues the sulfuric acid after dilution by sulphuric acid concentration device to be concentrated into original concentration circulating set With.
Invention content
The present invention provides a kind of hydrogen fluoride multiphase gasification separation recovery system, for handling hydrofluoric acid waste liquid, the fluorination Hydrogen multiphase gasification separation recovery system includes solids collection system, gas handling system, fluid collection systems and sulphuric acid concentration system System;
The solids collection system includes head tank, gasification swirl knockout tower and sodium fluoride high temperature purification device;
The head tank is communicated by feed pipe and gasification cyclonic separation tower, and charging is provided on the feed pipe Pump, flowmeter and high-temperature gasification reactor, the high-temperature gasification reactor are arranged on the top of the gasification swirl knockout tower;Institute It states feed pump and the hydrofluoric acid waste liquid in head tank is pumped into high-temperature gasification reactor after flowmeter measures, carry out transient evaporation, Enter gasification swirl knockout tower after gasification;
The bottom of the gasification swirl knockout tower is provided with sealed device for discharging, and the sealed device for discharging passes through solid Body pipeline is connected with high-temperature fluorination sodium clarifier;After the separation of gasification swirl knockout tower, solid leads to hydrofluoric acid waste liquid after gasification It crosses sealed device for discharging and is discharged into high-temperature fluorination sodium clarifier, realize the collection of solid;
The gas handling system and fluid collection systems include head tank, gas cyclone knockout tower, dust pelletizing system, heating Diffuser, condenser system and cleaning system;
The dust pelletizing system is communicated by circulating fan, circulating line and heating diffuser, and the heating diffuser is gentle The top entry for changing cyclonic separation tower communicates;
The circulating line is divided into main pipeline and branch pipe(tube);Distributor is provided on the main pipeline, on the branch pipe(tube) It is provided with gas phase flow rate distributor;The main pipeline is connected with heating diffuser, and the branch pipe(tube) is connected with condenser system;
Hydrofluoric acid waste liquid enters gasification swirl knockout tower after the gasification of high-temperature gasification reactor in the head tank, through gas-solid After separation, gas passes through dust pelletizing system by gas pipeline;It is returned by the processed gas of dust pelletizing system is most of through main pipeline Into gas cyclone knockout tower, fraction enters by branch pipe(tube) in condenser system;The circulating fan provides circulation power, and Gas phase is distributed in real time by distributor and gas phase flow rate distributor;
Gas phase into condenser system is condensed by contact condensing-dewatering tower, primary condenser, I grade of condenser, II grade Device, III grade of condenser condensation process after obtain pure gas phase, pure gas phase high altitude discharge after cleaning system purifies;
The primary condenser is arranged on the top of the contact condensing-dewatering tower;
The bottom of the contact condensing-dewatering tower is provided with concentrated sulfuric acid circulating tank, for collecting the thick liquid of the concentrated sulfuric acid;Described I Grade condenser, II grade of condenser, III grade of condenser bottom connected by condensation pipe with anhydrous hydrogenation fluorine collecting tank, for receiving Collect the anhydrous hydrogenation fluorine collecting tank in gas phase;The purifying column by purge pipe with there is water acid tank to connect, for collecting gas phase In hydrofluoric acid;
The sulphuric acid concentration system includes sulfuric acid evaporator, vaporization chamber, tail gas condenser, condensate tank and sulfuric acid cooler;
The concentrated sulfuric acid circulating tank is sent a part of concentrated sulfuric acid to the tower of contact condensing-dewatering tower by sulfuric acid circulating pump Jacking row atomizing spray;The concentrated sulfuric acid of another part is pumped into sulfuric acid evaporator and vaporization chamber, the sulphur by the sulfuric acid circulating pump Sour evaporator and vaporization chamber are come out the moisture evaporation that the concentrated sulfuric acid in drying process absorbs by heating up;The vapor being evaporated Enter condensate tank into tail gas condenser condensation;It is concentrated by evaporation the sulfuric acid completed and enters the concentrated sulfuric acid after sulfuric acid cooler cools down Circulating tank.
As one embodiment of the present invention, the dust pelletizing system includes high efficiency cyclonic dust collector and bag filter.
As one embodiment of the present invention, the cleaning system includes purifying column, water scrubber and caustic wash tower.
As one embodiment of the present invention, the gas handling system further includes coal heating heating furnace, the hot coal Body heating furnace is connected with the heating diffuser, for providing hot-air to the heating diffuser.
As one embodiment of the present invention, the bottom of the high efficiency cyclonic dust collector and bag filter is provided with close Envelope formula device for discharging, the sealed device for discharging and sodium fluoride high temperature purification device communicate.
As one embodiment of the present invention, the contact condensing-dewatering tower is using cold water as low-temperature receiver.
As one embodiment of the present invention, I grade of condenser, II grade of condenser, III grade of condenser use chilled brine As low-temperature receiver.
As one embodiment of the present invention, the sulfuric acid evaporator and vaporization chamber use deep fat as heat source.
As one embodiment of the present invention, the tail gas condenser and sulfuric acid cooler use cold water as low-temperature receiver.
As one embodiment of the present invention, the sulphuric acid concentration device also includes vacuum pump set.
Advantageous effect:
Whole device provided by the invention does not have secondary pollution, and passes through rational energy distribution and reach low operating cost Mode recycles anhydrous hydrogen fluoride and sodium fluoride product, thoroughly solves anhydrous hydrogen fluoride method production fluorobenzene, p-fluorotoluene, adjacent fluorine first The environmental issue of benzene.
Description of the drawings
In order to illustrate more clearly about the embodiment of the present invention or technical scheme of the prior art, to embodiment or will show below There is attached drawing needed in technology description to be briefly described, it should be apparent that, the accompanying drawings in the following description is only this Some embodiments of invention, for those of ordinary skill in the art, without creative efforts, can be with Other attached drawings are obtained according to these attached drawings.
Fig. 1:The equipment connection diagram of solids collection system;
Fig. 2:The equipment connection diagram of gas handling system and fluid collection systems;
Fig. 3:The equipment connection diagram of sulphuric acid concentration system.
Symbol description:
Head tank -1, flowmeter -3, high-temperature gasification reactor -4, gasification swirl knockout tower -5, sealed unloads feed pump -2 Expect that device -6, sodium fluoride high temperature purification device -7, high efficiency cyclonic dust collector -8, bag filter -9, circulating fan -10, heating are expanded Dissipate device -11, coal heating heating furnace -12, contact condensing-dewatering tower -13, primary condenser -14, I grade of condenser -15, II grade it is cold Condenser -16, anhydrous hydrogen fluoride collecting tank -18, purifying column -19, has water acid tank -20, circulating pump -21, water at III grade of condenser -17 Wash tower -22, wind turbine -23, caustic wash tower -24, concentrated sulfuric acid circulating tank -25, sulfuric acid evaporator -26, vaporization chamber -27, tail gas condenser - 28th, sulfuric acid cooler -29, condensate tank -30, condensate pump -31, vacuum pump set -32,
Feed pipe -33, solid pipeline -34, gas pipeline -35, circulating line -36, distributor -37, gas phase flow rate point Orchestration -38, hot-air duct -39, condensation pipe -40, sulfuric acid pipeline -41,
Chilled brine reflux line -42, cold-water reflux pipeline -43, deep fat reflux line -44, sulfuric acid circulating pump -45
Specific embodiment
The detailed description for preferred implementation method of the invention below of participating in the election of and including embodiment this hair can be more easily understood Bright content.Unless otherwise defined, all technologies used herein and scientific terminology have common with fields of the present invention The normally understood identical meaning of technical staff.When there is a conflict, the definition in this specification shall prevail.
Below in conjunction with the attached drawing in the embodiment of the present invention, the technical solution in the embodiment of the present invention is carried out clear, complete Site preparation describes, it is clear that described embodiment is only part of the embodiment of the present invention, instead of all the embodiments.It is based on Embodiment in the present invention, those of ordinary skill in the art are obtained every other without making creative work Embodiment shall fall within the protection scope of the present invention.
Those skilled in the art of the present technique are appreciated that unless otherwise defined all terms used herein are (including technology art Language and scientific terminology) there is the meaning identical with the general understanding of the those of ordinary skill in fields of the present invention.Should also Understand, those terms such as defined in the general dictionary, which should be understood that, to be had and the meaning in the context of the prior art The consistent meaning of justice, and unless defined as here, will not be with idealizing or the meaning of too formal be explained.
The meaning of heretofore described "and/or" refers to that the simultaneous situation of respective individualism or both is wrapped Including including.
The meaning of heretofore described " inside and outside " referred to relative to equipment itself, the side inside sensing equipment To be interior, on the contrary is specific restriction outer rather than to the device of the invention mechanism.
When the meaning of heretofore described " left and right " refers to reader's face attached drawing, the left side of reader is a left side, The right of reader is the right rather than specific restriction to the device of the invention mechanism.
The meaning of heretofore described " connection " can be between component to be directly connected to can also pass through between component Other components are indirectly connected with.
The present invention provides a kind of hydrogen fluoride multiphase gasification separation recovery system, for handling hydrofluoric acid waste liquid, the fluorination Hydrogen multiphase gasification separation recovery system includes solids collection system, gas handling system, fluid collection systems and sulphuric acid concentration system System;
The solids collection system includes head tank, gasification swirl knockout tower and sodium fluoride high temperature purification device;
The head tank is communicated by feed pipe and gasification cyclonic separation tower, and charging is provided on the feed pipe Pump, flowmeter and high-temperature gasification reactor, the high-temperature gasification reactor are arranged on the top of the gasification swirl knockout tower;Institute It states feed pump and the hydrofluoric acid waste liquid in head tank is pumped into high-temperature gasification reactor after flowmeter measures, carry out transient evaporation, Enter gasification swirl knockout tower after gasification;
The bottom of the gasification swirl knockout tower is provided with sealed device for discharging, and the sealed device for discharging passes through solid Body pipeline is connected with high-temperature fluorination sodium clarifier;After the separation of gasification swirl knockout tower, solid leads to hydrofluoric acid waste liquid after gasification It crosses sealed device for discharging and is discharged into high-temperature fluorination sodium clarifier, realize the collection of solid;
The gas handling system includes head tank, gas cyclone knockout tower, dust pelletizing system, heating diffuser, condensed system System and cleaning system;
The dust pelletizing system is communicated by circulating fan, circulating line and heating diffuser, and the heating diffuser is gentle The top entry for changing cyclonic separation tower communicates;
The circulating line is divided into main pipeline and branch pipe(tube);Distributor is provided on the main pipeline, on the branch pipe(tube) It is provided with gas phase flow rate distributor;The main pipeline is connected with heating diffuser, and the branch pipe(tube) is connected with condenser system;
Hydrofluoric acid waste liquid enters gasification swirl knockout tower after the gasification of high-temperature gasification reactor in the head tank, through gas-solid After separation, gas passes through dust pelletizing system by gas pipeline;It is returned by the processed gas of dust pelletizing system is most of through main pipeline Into gas cyclone knockout tower, fraction enters by branch pipe(tube) in condenser system;The circulating fan provides circulation power, and Gas phase is distributed in real time by distributor and gas phase flow rate distributor;
The condenser system include contact condensing-dewatering tower, primary condenser, I grade of condenser, II grade of condenser, III grade Condenser;
Gas phase into condenser system is condensed by contact condensing-dewatering tower, primary condenser, I grade of condenser, II grade Device, III grade of condenser condensation process after obtain pure gas phase, pure gas phase high altitude discharge after cleaning system purifies;
The primary condenser is arranged on the top of the contact condensing-dewatering tower;
The bottom of the contact condensing-dewatering tower is provided with concentrated sulfuric acid circulating tank, for collecting the thick liquid of the concentrated sulfuric acid;Described I Grade condenser, II grade of condenser, III grade of condenser bottom connected by condensation pipe with anhydrous hydrogenation fluorine collecting tank, for receiving Collect the anhydrous hydrogenation fluorine collecting tank in gas phase;The purifying column by purge pipe with there is water acid tank to connect, for collecting gas phase In hydrofluoric acid;
The sulphuric acid concentration system includes sulfuric acid evaporator, vaporization chamber, tail gas condenser, condensate tank and sulfuric acid cooler;
The concentrated sulfuric acid circulating tank is sent a part of concentrated sulfuric acid to the tower of contact condensing-dewatering tower by sulfuric acid circulating pump Jacking row atomizing spray;The concentrated sulfuric acid of another part is pumped into sulfuric acid evaporator and vaporization chamber, the sulphur by the sulfuric acid circulating pump Sour evaporator and vaporization chamber are come out the moisture evaporation that the concentrated sulfuric acid in drying process absorbs by heating up;The vapor being evaporated Enter condensate tank into tail gas condenser condensation;It is concentrated by evaporation the sulfuric acid completed and enters the concentrated sulfuric acid after sulfuric acid cooler cools down Circulating tank.
As one embodiment of the present invention, the dust pelletizing system includes high efficiency cyclonic dust collector and bag filter.
As one embodiment of the present invention, the cleaning system includes purifying column, water scrubber and caustic wash tower.
As one embodiment of the present invention, the gas handling system further includes coal heating heating furnace, the hot coal Body heating furnace is connected with the heating diffuser, for providing hot-air to the heating diffuser.
As one embodiment of the present invention, the bottom of the high efficiency cyclonic dust collector and bag filter is provided with close Envelope formula device for discharging, the sealed device for discharging and sodium fluoride high temperature purification device communicate.
As one embodiment of the present invention, the contact condensing-dewatering tower is using cold water as low-temperature receiver.
As one embodiment of the present invention, I grade of condenser, II grade of condenser, III grade of condenser use chilled brine As low-temperature receiver.
As one embodiment of the present invention, the sulfuric acid evaporator and vaporization chamber use deep fat as heat source.
As one embodiment of the present invention, the tail gas condenser and sulfuric acid cooler use cold water as low-temperature receiver.
As one embodiment of the present invention, the sulphuric acid concentration device also includes vacuum pump set.
The second aspect of the present invention provides the equipment for the hydrogen fluoride multiphase gasification separation recovery system, the equipment Comprising:Head tank, feed pump, flowmeter, high-temperature gasification reactor, gasification swirl knockout tower, sealed device for discharging, sodium fluoride High temperature purification device, high efficiency cyclonic dust collector, bag filter, circulating fan, heating diffuser, coal heating heating furnace, contact Condensing-dewatering tower, primary condenser, I grade of condenser, II grade of condenser, III grade of condenser, anhydrous hydrogen fluoride collecting tank, purification Tower has water acid tank, circulating pump, water scrubber, wind turbine, caustic wash tower, concentrated sulfuric acid circulating tank, sulfuric acid evaporator, vaporization chamber, tail gas condensing Device, sulfuric acid cooler, condensate tank, condensate pump, vacuum pump set.
As one embodiment of the present invention, the head tank is connected by feed pipe with high-temperature gasification reactor, The high-temperature gasification reactor is arranged on the top of gasification swirl knockout tower, and feed pump and flow are provided on the feed pipe Meter;
The bottom of the gasification swirl knockout tower, high efficiency cyclonic dust collector and bag filter is provided with sealed discharging dress It puts, the sealed device for discharging is connected by solid pipeline with sodium fluoride high temperature purification device;
The gasification swirl knockout tower is connected by gas pipeline with the top of high efficiency cyclonic dust collector, the efficient cyclone Deduster is connected by gas pipeline with bag filter;
The top of the bag filter is connected by gas pipeline with circulating fan, and the circulating fan passes through circulation pipe Road connects respectively with heating diffuser with contact condensing-dewatering tower, sets distributor and gas phase stream on the circulating line respectively Measure distributor;
The heating diffuser is connected by the top of gas pipeline with the gasification swirl knockout tower, and the coal heating adds Hot stove is connected by hot-air duct with heating diffuser;
The bottom of the contact condensing-dewatering tower is provided with concentrated sulfuric acid circulating tank, the top of the contact condensing-dewatering tower Portion is provided with primary condenser, the primary condenser by condensation pipe successively with I grade of condenser, II grade of condenser, III grade Condenser connects,
The bottom of I grade of condenser, II grade of condenser and III grade of condenser is connected with anhydrous hydrogen fluoride collecting tank, described The top of I grade of condenser, II grade of condenser and III grade of condenser is connected by gas pipeline with purifying column;The bottom of the purifying column Portion with have water acid tank and connect;The tower top of the purifying column is connected with water scrubber, and the tower top of the water scrubber is connected with caustic wash tower.
The concentrated sulfuric acid circulating tank is connected by sulfuric acid pipeline with sulfuric acid evaporator with vaporization chamber respectively, the vaporization chamber Top is connected by gas pipeline with tail gas condenser, and the tail gas condenser will condense water transport to condensate by vacuum pump set In tank;Condensed water in condensate tank is transported out use by the condensate pump.
The third aspect of the present invention provides a kind of hydrogen fluoride multiphase gasification separation technique, the technique include heating, Gas solid separation, gas-liquid separation stage and sulphuric acid concentration stage;
The hydrofluoric acid waste liquid is heated by high-temperature gasification reactor, is carried out just through gasification swirl knockout tower after transient evaporation Secondary gas solid separation, gas carries out gas solid separation again by high efficiency cyclonic dust collector and bag filter, described to isolate The solid come is collected by sealed device for discharging in sodium fluoride high temperature purification device;By the gas after gas solid separation again It is most of to be recycled into heating diffuser in heat cycles to gasification swirl knockout tower again by gas phase;Fraction gas again Gu the gas after separation enters the gas-liquid separation stage by gas phase flow rate distributor;
Gas into the gas-liquid separation stage carries out primary dewatering by contact condensing-dewatering tower, then by primary cold Condenser, I grade of condenser, II grade of condenser, III grade of condenser carry out multiple condensation;
To through the gas of multiple condensation isolate anhydrous liquid hydrogen fluoride carry out after, gas by purifying column, water scrubber and Caustic wash tower completes last evolutionary process, and subsequent gas is through high altitude discharge;
The bottom of the purifying column is connected with water acid tank, for collecting the liquid HF acid isolated by purifying column.
The bottom of the contact condensing-dewatering tower is equipped with concentrated sulfuric acid circulating tank, the dense sulphur in the concentrated sulfuric acid circulating tank The tower top that sulfuric acid is promoted to contact condensing-dewatering tower by sulfuric acid circulating pump by acid carries out atomizing spray.
The concentrated sulfuric acid in the concentrated sulfuric acid circulating tank after dehydration is concentrated through sulphuric acid concentration technique.
The step of sulphuric acid concentration technique, is as follows:
(1) sulfuric acid in concentrated sulfuric acid circulating tank heated, evaporated, generate vapor;
(2) vapor in step (1) is condensed, collects condensed water;
(3) concentrated sulfuric acid of the water removal after heating in step (1) is handled by cooling, conveying is back to concentrated sulfuric acid circulating tank It is interior.
The flow of the hydrogen fluoride multiphase gasification separation technique is 500kg/h.
The heating diffuser heats stove heat air by coal heating, provides hot gas source.
It is of the invention that above-mentioned raffinate is handled using completely new technical approach, it solves fluorination hydrogen retrieval and environmentally friendly well and asks Topic.Hydrogen fluoride multiphase gasification separation retracting device, including high-temperature gasification reactor, eddy flow gas-solid separator, heating system, solid Discharger, gas phase purifying device, heat-source Cycles system, gas phase drying device, gas phase refrigerating plant.
High-temperature gasification reactor is connected to ensure that the gas phase in raffinate and solid phase are efficiently separated with eddy flow gas-solid separator, supplies Hot systems provide the required thermal energy of gasification reaction, and the gas phase after gas solid separation sequentially enters gas phase purifying device, heat-source Cycles system Anhydrous liquid hydrogen fluoride is formed after system, gas phase drying device, gas phase refrigerating plant.It is connected between each device by pipeline.Solid High-temperature purification device is discharged by the way that the solids exit device of gas phase is fully sealed in eddy flow gas-solid separator bottom, is further purified Into byproduct.
With reference to specific attached drawing, hydrogen fluoride multiphase gasification separation recovery system of the present invention is described in detail.
Attached drawing 1:
The present invention provides a kind of hydrogen fluoride multiphase gasification separation recovery system, for handling hydrofluoric acid waste liquid, the fluorination Hydrogen multiphase gasification separation recovery system includes solids collection system, gas handling system, fluid collection systems and sulphuric acid concentration system System, is as shown in Figure 1 solids collection system.
As shown in Figure 1, the solids collection system includes:Head tank 1, feed pump 2, flowmeter 3, high-temperature gasification reactor 4th, gasification swirl knockout tower 5, sealed device for discharging 6, sodium fluoride high temperature purification device 7, high efficiency cyclonic dust collector 8, bag-type dust Device 9, circulating fan 10, heating diffuser 11, coal heating heating furnace 12.
The head tank 1 is connected by feed pipe 33 and high-temperature gasification reactor 4, and the high-temperature gasification reactor 4 is set It puts and is provided with feed pump 2 and flowmeter 3 on the top of gasification swirl knockout tower 5, the feed pipe 33;
The bottom of the gasification swirl knockout tower 5, high efficiency cyclonic dust collector 8 and bag filter 9 is provided with sealed unload Expect device 6, the sealed device for discharging 6 is connected by solid pipeline 34 and sodium fluoride high temperature purification device 7;
The gasification swirl knockout tower 5 is connected by the top of gas pipeline 35 with high efficiency cyclonic dust collector 8, described efficient Cyclone dust collectors 8 are connected by gas pipeline 35 and bag filter 9;
The top of the bag filter 9 is connected by gas pipeline 35 and circulating fan 10, and the circulating fan 10 is logical It crosses circulating line 36 to connect with heating diffuser 11 and contact condensing-dewatering tower 13 respectively, be set respectively on the circulating line 36 Put distributor 37 and gas phase flow rate distributor 38;
The heating diffuser 11 is connected by the top of gas pipeline 35 with the gasification swirl knockout tower 5, the heat Coal body heating furnace 12 is connected by hot-air duct 39 and heating diffuser 11.
The head tank 1 is communicated by feed pipe 33 and gasification cyclonic separation tower 5, and the feed pump 2 will be in head tank Hydrofluoric acid waste liquid be pumped into high-temperature gasification reactor 4 after the metering of flowmeter 3, carry out transient evaporation, gasification rotation entered after gasification Flow separation tower 5;For hydrofluoric acid waste liquid after gasification after the separation of gasification swirl knockout tower 5, solid passes through sealed 6 row of device for discharging Enter high-temperature fluorination sodium clarifier 7, realize the collection of solid.
Attached drawing 2:
The present invention provides a kind of hydrogen fluoride multiphase gasification separation recovery system, for handling hydrofluoric acid waste liquid, the fluorination Hydrogen multiphase gasification separation recovery system includes solids collection system, gas handling system, fluid collection systems and sulphuric acid concentration system System is gas gathering system and fluid collection systems as shown in Figure 1.
As depicted in figs. 1 and 2,
The gas handling system and fluid collection systems include head tank 1, gas cyclone knockout tower 5, dust pelletizing system, add Heat diffuser 11, condenser system and cleaning system;
The dust pelletizing system includes high efficiency cyclonic dust collector 8 and bag filter 9;
The cleaning system includes purifying column 19, water scrubber 22 and caustic wash tower 24;
The condenser system includes contact condensing-dewatering tower 13,14, I grades of primary condenser, 15, II grades of condenser condenses 16, III grades of condensers 17 of device;
The bottom of the contact condensing-dewatering tower 13 is provided with concentrated sulfuric acid circulating tank 25, the contact condensing-dewatering tower 13 top is provided with primary condenser 14, the primary condenser by condensation pipe 40 successively with I grade of 15, II grades of condenser 16, III grades of condensers 17 of condenser connect,
The bottom of I grade of condenser, 15, II grades of condensers 16 and III grade of condenser 17 is connected with anhydrous hydrogen fluoride collection The top of tank 18, I grade of condenser, 15, II grades of condensers 16 and III grade of condenser 17 passes through gas pipeline 35 and purifying column 19 Connection;The bottom of the purifying column 19 and there is water acid tank 20 to connect;The tower top and water scrubber 22 of the purifying column 19 connect, described The tower top and caustic wash tower 24 of water scrubber 22 connect.
The dust pelletizing system is communicated by circulating fan 10, circulating line 36 and heating diffuser 11, the heating diffusion The top entry of device 11 and gasification cyclonic separation tower 5 communicates;
The circulating line 36 divides for main pipeline and branch pipe(tube);Distributor 37, the branch pipe are provided on the main pipeline Gas phase flow rate distributor 38 is provided on road;The main pipeline and heating diffuser 11 connect, the branch pipe(tube) and condenser system Connection;
Hydrofluoric acid waste liquid enters gasification swirl knockout tower after the gasification of high-temperature gasification reactor in the head tank, through gas-solid After separation, gas passes through dust pelletizing system by gas pipeline;It is returned by the processed gas of dust pelletizing system is most of through main pipeline Into gas cyclone knockout tower, fraction enters by branch pipe(tube) in condenser system;The circulating fan provides circulation power, and Gas phase is distributed in real time by distributor and gas phase flow rate distributor;
Gas phase into condenser system is condensed by contact condensing-dewatering tower, primary condenser, I grade of condenser, II grade Device, III grade of condenser condensation process after obtain pure gas phase, pure gas phase high altitude discharge after cleaning system purifies;
The bottom of the contact condensing-dewatering tower is provided with concentrated sulfuric acid circulating tank, for collecting the thick liquid of the concentrated sulfuric acid;Described I Grade condenser, II grade of condenser, III grade of condenser bottom connected by condensation pipe with anhydrous hydrogenation fluorine collecting tank, for receiving Collect the anhydrous hydrogenation fluorine collecting tank in gas phase;The purifying column by purge pipe with there is water acid tank to connect, for collecting gas phase In hydrofluoric acid.
The hydrofluoric acid waste liquid is heated by high-temperature gasification reactor, is carried out just through gasification swirl knockout tower after transient evaporation Secondary gas solid separation, gas carries out gas solid separation again by high efficiency cyclonic dust collector and bag filter, described to isolate The solid come is collected by sealed device for discharging in sodium fluoride high temperature purification device;By the gas after gas solid separation again It is most of to be recycled into heating diffuser in heat cycles to gasification swirl knockout tower again by gas phase;Fraction gas again Gu the gas after separation enters the gas-liquid separation stage by gas phase flow rate distributor;
Gas into the gas-liquid separation stage carries out primary dewatering by contact condensing-dewatering tower, then by primary cold Condenser, I grade of condenser, II grade of condenser, III grade of condenser carry out multiple condensation;
To through the gas of multiple condensation isolate anhydrous liquid hydrogen fluoride carry out after, gas by purifying column, water scrubber and Caustic wash tower completes last evolutionary process, and subsequent gas is through high altitude discharge;
The bottom of the purifying column is connected with water acid tank, for collecting the liquid HF acid isolated by purifying column.
The bottom of the contact condensing-dewatering tower is equipped with concentrated sulfuric acid circulating tank, the dense sulphur in the concentrated sulfuric acid circulating tank The tower top that sulfuric acid is promoted to contact condensing-dewatering tower by sulfuric acid circulating pump by acid carries out atomizing spray.
Attached drawing 3:
The present invention provides a kind of hydrogen fluoride multiphase gasification separation recovery system, for handling hydrofluoric acid waste liquid, the fluorination Hydrogen multiphase gasification separation recovery system includes solids collection system, gas handling system, fluid collection systems and sulphuric acid concentration system System, is illustrated in figure 3 sulphuric acid concentration system.
The sulphuric acid concentration system includes concentrated sulfuric acid circulating tank 25, sulfuric acid evaporator 26, vaporization chamber 27, tail gas condenser 28th, sulfuric acid cooler 29, condensate tank 30, condensate pump 31, vacuum pump set 32.
The concentrated sulfuric acid circulating tank 25 is connected by sulfuric acid pipeline 41 with sulfuric acid evaporator 26 and vaporization chamber 27 respectively, described The top of vaporization chamber 27 is connected by gas pipeline 35 and tail gas condenser 28, and the tail gas condenser 28 passes through vacuum pump set 32 It will condense in water transport to condensate tank 30;Condensed water in condensate tank 30 is transported out use by the condensate pump 31.
The concentrated sulfuric acid circulating tank 25 is sent a part of concentrated sulfuric acid to contact condensing-dewatering tower by sulfuric acid circulating pump 45 13 tower top carries out atomizing spray;The concentrated sulfuric acid of another part is pumped into sulfuric acid evaporator 26 and evaporation by the sulfuric acid circulating pump 45 Room 27, the sulfuric acid evaporator 26 and vaporization chamber 27 are come out the moisture evaporation that the concentrated sulfuric acid in drying process absorbs by heating up; The vapor being evaporated enters the condensation of tail gas condenser 28 and enters condensate tank 30;It is cold through persulfuric acid to be concentrated by evaporation the sulfuric acid completed But enter concentrated sulfuric acid circulating tank 25 after device 29 cools down.
The concentrated sulfuric acid in the concentrated sulfuric acid circulating tank after dehydration is concentrated through sulphuric acid concentration technique.
The step of sulphuric acid concentration technique, is as follows:
(1) sulfuric acid in concentrated sulfuric acid circulating tank heated, evaporated, generate vapor;
(2) vapor in step (1) is condensed, collects condensed water;
(3) concentrated sulfuric acid of the water removal after heating in step (1) is handled by cooling, conveying is back to concentrated sulfuric acid circulating tank It is interior.
Within the mentality of designing and protection domain of the present invention, to other changes or modifications of above-mentioned specific embodiment to this It is obvious for field technology personnel.Although present invention control specific embodiment is described, these implementations The purpose of example is only to illustrate rather than in order to be defined, and correspondingly, this patent is not limited in the several spies described herein Determine the range and effect of embodiment, be also not necessarily limited to and inconsistent to a certain extent by inventing acquired progress in the art Other any modes.

Claims (10)

1. a kind of hydrogen fluoride multiphase gasification separation recovery system, for handling hydrofluoric acid waste liquid, which is characterized in that the hydrogen fluoride Multiphase gasification separation recovery system includes solids collection system, gas handling system, fluid collection systems and sulphuric acid concentration system;
The solids collection system includes head tank, gasification swirl knockout tower and sodium fluoride high temperature purification device;
The head tank is communicated by feed pipe and gasification cyclonic separation tower, and feed pump, stream are provided on the feed pipe Gauge and high-temperature gasification reactor, the high-temperature gasification reactor are arranged on the top of the gasification swirl knockout tower;It is described into Hydrofluoric acid waste liquid in head tank is pumped into high-temperature gasification reactor by material pump after flowmeter measures, and carries out transient evaporation, gasification Enter gasification swirl knockout tower afterwards;
The bottom of the gasification swirl knockout tower is provided with sealed device for discharging, and the sealed device for discharging passes through solid tube Road is connected with high-temperature fluorination sodium clarifier;After the separation of gasification swirl knockout tower, solid passes through close hydrofluoric acid waste liquid after gasification Envelope formula device for discharging is discharged into high-temperature fluorination sodium clarifier, realizes the collection of solid;
The gas handling system and fluid collection systems include head tank, gas cyclone knockout tower, dust pelletizing system, heating diffusion Device, condenser system and cleaning system;
The dust pelletizing system is communicated by circulating fan, circulating line and heating diffuser, and the heating diffuser and gasification are revolved The top entry of flow separation tower communicates;
The circulating line is divided into main pipeline and branch pipe(tube);Distributor is provided on the main pipeline, is set on the branch pipe(tube) There is gas phase flow rate distributor;The main pipeline is connected with heating diffuser, and the branch pipe(tube) is connected with condenser system;
Hydrofluoric acid waste liquid enters gasification swirl knockout tower after the gasification of high-temperature gasification reactor in the head tank, through gas solid separation Afterwards, gas passes through dust pelletizing system by gas pipeline;By the processed gas of dust pelletizing system is most of gas is returned to through main pipeline In body cyclonic separation tower, fraction enters by branch pipe(tube) in condenser system;The circulating fan provides circulation power, and passes through Distributor and gas phase flow rate distributor distribute gas phase in real time;
Gas phase into condenser system passes through contact condensing-dewatering tower, primary condenser, I grade of condenser, II grade of condenser, III Pure gas phase, pure gas phase high altitude discharge after cleaning system purifies are obtained after the condensation process of grade condenser;
The primary condenser is arranged on the top of the contact condensing-dewatering tower;
The bottom of the contact condensing-dewatering tower is provided with concentrated sulfuric acid circulating tank, for collecting the thick liquid of the concentrated sulfuric acid;Described I grade cold Condenser, II grade of condenser, III grade of condenser bottom connected by condensation pipe with anhydrous hydrogenation fluorine collecting tank, for collecting gas Anhydrous hydrogenation fluorine collecting tank in phase;The purifying column by purge pipe with there is water acid tank to connect, for collecting in gas phase Hydrofluoric acid;
The sulphuric acid concentration system includes sulfuric acid evaporator, vaporization chamber, tail gas condenser, condensate tank and sulfuric acid cooler;
The concentrated sulfuric acid circulating tank by sulfuric acid circulating pump by a part of concentrated sulfuric acid send to the tower top of contact condensing-dewatering tower into Row atomizing spray;The concentrated sulfuric acid of another part is pumped into sulfuric acid evaporator and vaporization chamber by the sulfuric acid circulating pump, and the sulfuric acid steams Hair device and vaporization chamber are come out the moisture evaporation that the concentrated sulfuric acid in drying process absorbs by heating up;The vapor being evaporated enters Tail gas condenser condensation enters condensate tank;It is concentrated by evaporation the sulfuric acid completed and enters concentrated sulfuric acid cycle after sulfuric acid cooler cools down Tank.
A kind of 2. hydrogen fluoride multiphase gasification separation recovery system described in claim 1, which is characterized in that the dust pelletizing system packet Include high efficiency cyclonic dust collector and bag filter.
A kind of 3. hydrogen fluoride multiphase gasification separation recovery system described in claim 1, which is characterized in that the cleaning system packet Include purifying column, water scrubber and caustic wash tower.
A kind of 4. hydrogen fluoride multiphase gasification separation recovery system described in claim 1, which is characterized in that the gas treatment system System further includes coal heating heating furnace, and the coal heating heating furnace is connected with the heating diffuser, for being spread to the heating Device provides hot-air.
5. a kind of hydrogen fluoride multiphase gasification separation recovery system described in claim 2, which is characterized in that the efficient cyclone removes The bottom of dirt device and bag filter is provided with sealed device for discharging, the sealed device for discharging and sodium fluoride high temperature purification Device communicates.
A kind of 6. hydrogen fluoride multiphase gasification separation recovery system described in claim 1, which is characterized in that the contact condensation Dehydrating tower is using cold water as low-temperature receiver.
A kind of 7. hydrogen fluoride multiphase gasification separation recovery system described in claim 1, which is characterized in that I grade of condenser, II grade Condenser, III grade of condenser are using chilled brine as low-temperature receiver.
A kind of 8. hydrogen fluoride multiphase gasification separation recovery system described in claim 1, which is characterized in that the sulfuric acid evaporator With vaporization chamber using deep fat as heat source.
A kind of 9. hydrogen fluoride multiphase gasification separation recovery system described in claim 1, which is characterized in that the tail gas condenser With sulfuric acid cooler using cold water as low-temperature receiver.
A kind of 10. hydrogen fluoride multiphase gasification separation recovery system described in claim 1, which is characterized in that the sulphuric acid concentration Device also includes vacuum pump set.
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