CN107311109A - A kind of circulating fluidized bed system and method that hydrogen fluoride is produced with Fluorspar Powder - Google Patents

A kind of circulating fluidized bed system and method that hydrogen fluoride is produced with Fluorspar Powder Download PDF

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CN107311109A
CN107311109A CN201710334825.0A CN201710334825A CN107311109A CN 107311109 A CN107311109 A CN 107311109A CN 201710334825 A CN201710334825 A CN 201710334825A CN 107311109 A CN107311109 A CN 107311109A
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gas
section
reaction
reactor
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CN107311109B (en
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黄正梁
杨遥
林王旻
孙婧元
刘仲玄
王靖岱
阳永荣
蒋斌波
廖祖维
范小强
王浩同
訾灿
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Zhejiang University ZJU
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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
    • C01B7/192Preparation from fluorspar
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J8/00Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
    • B01J8/18Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles
    • B01J8/1836Heating and cooling the reactor
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J8/00Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
    • B01J8/18Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles
    • B01J8/1872Details of the fluidised bed reactor
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J8/00Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
    • B01J8/18Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles
    • B01J8/24Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles according to "fluidised-bed" technique

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  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Combustion & Propulsion (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Inorganic Chemistry (AREA)
  • Devices And Processes Conducted In The Presence Of Fluids And Solid Particles (AREA)

Abstract

The invention discloses a kind of circulating fluidized bed system and method that hydrogen fluoride is produced with Fluorspar Powder.System includes reactor, cyclic part, solid segregation section, solid segregation section.The place that reactor part occurs for reaction, cyclic part isolates the incomplete solid of reaction, is returned to after being settled in reactor and continues to react;Solid separate section separates gas-particle two-phase product, and collects the complete solid of reaction, is used as solid product;The gas-phase product that separation residue goes out in solid segregation section is liquefied and collected by gas condensation portion.Present invention, avoiding the appearance that agglomerate glues the anomalies such as wall, improve mass transfer, heat transfer efficiency, by controlling the cycling rate of control valve aperture control recirculating fluidized bed on tolerance size and inclined tube, the solid product ratio isolated is controlled to control solid reaction degree.Liquid condensation is controlled by condensate temperature and consumption, and product quality can be controlled by installing multi-stage condensing device additional when containing other impurities in gaseous product.

Description

A kind of circulating fluidized bed system and method that hydrogen fluoride is produced with Fluorspar Powder
Technical field
The present invention relates to a kind of Circulating Fluidized Bed Process that hydrogen fluoride is produced for Fluorspar Powder.
Technical background
Hydrofluoric acid (HF) is the basic product of whole fluorine chemical industry, is mainly used in fluorohydrocarbon industry, accounts for hydrogen fluoride and always disappear 50% or so of consumption;Next to that the inorganic fluorine salt dissolving such as production electrolytic aluminium and the aluminum fluoride and ice crystal of aluminum profile extrusion industry, Account for more than 30%;Be again be used as in pickling of metal, oil plant iso-butane and the catalyst of butane alkylated reaction and other The production industry of fluorinated organic compound.China is continuously increased to the demand of anhydrous hydrogen fluoride in recent years.
Hydrogen fluoride production is mainly obtained by fluorite with sulfuric acid reaction.Calcirm-fluoride and sulfuric acid reaction are an endothermic reactions, Industrially need to react at high temperature, external heat is needed in production process.Current existing production technology mainly has rotary kiln Technique, gas-solid multicompartment fluidized bed technique, gas-liquid-solid fluidized-bed process, intermittent reaction technique etc..United States Patent (USP) US3102787 is announced The methods that two kinds of Fluorspar Powders produce hydrogen fluoride with sulfuric acid reaction.One of which is rotary kiln technology, and one kind is multilayer gas-solid flow Change bed process.Rotary kiln technology is the most frequently used production technology in current industry.In the technique, Fluorspar Powder passes through premix with sulfuric acid The modes such as conjunction, stirring, housing revolution react in the rotary kiln with heating rotary shell in mixing.According to internal mix Agitating member is different, is broadly divided into simple rotary kiln, the rotary kiln with premixer, the rotary kiln with pre-reactor, interior returns Return slag rotary kiln and several simultaneous with the rotary kiln of pre-reactor, interior return slag, destroyer in slag rotary kiln, pre-reactor. Rotary kiln technology has obtained sufficient development at present, from production maintenance, operating cost, equipment manufacturing cost, consumption of raw materials be difficult into One step is reduced.Gas-solid multicompartment fluidized bed technique uses vapor and SO3Gas is simultaneously released as air inlet, gas phase reaction generation sulfuric acid Big calorimetric, reaction raw materials sulfuric acid is provided for device, while providing fluorite and the heat needed for sulfuric acid reaction.Gas-solid multicompartment fluidized bed work Artistic skill enough improves the reaction efficiency of reactor and eliminates the problem of reaction of fluid sulphuric acid and fluorite is easily tacky, with being swift in response, Fluorite utilization rate is high, the characteristics of facility compact is simple.Chinese patent CN201210276366.2 is further perfect gas-solid fluidized Bed process, expands available Fluorspar Powder purity range.But due in industry fluorite grain diameter used smaller (average grain diameter exists Between 20~40 μm), particle agglomeration causes fluidisation and interlayer transmission to become extremely difficult caused by strong Van der Waals force between particle, many Laminarization bed reaction technique is not yet truly applied in practice in industry.
In addition to such a technique, Chinese patent CN201210489798.1 also disclosed a kind of gas-liquid-solid fluidized-bed process, make With phenyl-hexafluoride as inertia dispersant, Fluorspar Powder is disperseed, sulfuric acid is dissolved in phenyl-hexafluoride, reacted with Fluorspar Powder, released Hydrogen fluoride gas.The technique can solve the problem that the problem of Fluorspar Powder is bonded, and improve the efficiency that powder is contacted with acid.But after reaction The problem of separation of the calcium sulfate and dispersant of discharge has very big, dispersant entrainment is excessive and is difficult to separation so that the technique is difficult Further to develop.
In view of the above-mentioned problems, the present invention proposes a kind of Circulating Fluidized Bed Process that hydrogen fluoride is produced for Fluorspar Powder.
In recirculating fluidized bed, on the one hand high fluidizing gas velocity can suppress particle agglomeration and viscous wall, effectively eliminate and reunite And influence of the viscous wall to mass-and heat-transfer;It is quick anti-that another aspect Fluorspar Powder carries out short-time contact progress in fluid bed with sulfuric acid Settler should be entered afterwards to settle, be recirculated back in fluid bed and continue to react.Fast reaction can keep higher sulfuric acid concentration, keep away The problem of not enough caused reaction rate of reaction later stage sulfuric acid significantly slows down is exempted from, production efficiency can be effectively improved.
The content of the invention
The present invention provides a kind of Circulating Fluidized Bed Process that hydrogen fluoride is produced for Fluorspar Powder, passes through Fluorspar Powder Rapid Circulation By fluidized-bed reaction, particle agglomeration and viscous wall are effectively inhibited, mass-and heat-transfer efficiency is enhanced, improves production efficiency.
It is an object of the present invention to provide a kind of circulating fluidized bed system that hydrogen fluoride is produced for Fluorspar Powder, it is wrapped Include:Reactor, the expanding reach more than direct tube section, direct tube section, the section of the undergauge below direct tube section and closing heating shell are constituted; Cyclic part, by gas reactor export after primary cyclone, solid settling section, be connected to reactor air inlet pipe Inclined tube section, the control valve on inclined tube and lagging casing are constituted;Solid segregation section, is received by secondary cyclone and solid Tank is constituted;Gas condensation portion, by condenser, Liquid acquisition tank is constituted.Reaction mass enters below reactor into reactor Row reaction, isolates solid reactant into cyclic part afterwards.The solid retention time of high conversion rate is long, weares and teares tighter Weight, its particle diameter is smaller, and cyclic part is left above primary cyclone into solid segregation section with gas phase reaction material, and After being separated through secondary cyclone gas-particle two-phase product is respectively obtained in its upper and lower ends.After the condensed device condensation of gas-phase product Received by Liquid acquisition tank, solid product enters solid receiving tank.The isolated reaction mass of cyclic part passes through from bottom Control valve enters the air inlet pipe of reactor lower end and make-up gas is mixed into reactor cycles reaction.Solid is supplemented from circulation Part adds supplement.Above-mentioned reaction mass includes inert filler and reaction raw materials etc.;Make-up gas and supplement solid, including need Inert filler and reaction raw materials of supplement etc..Wherein reaction raw materials refer to Fluorspar Powder, sulfuric acid vapor or sulfur trioxide and vapor is mixed Close gas.
In the solid segregation section of the present invention, counterbalance valve can be installed additional above solid receiving tank, made in secondary cyclone Deposition solid passes through by phased manner, reduces solid and receives pressure inside the tank.
According to system of the present invention, second object of the present invention is to provide the side that a kind of Fluorspar Powder produces hydrogen fluoride Method, it comprises the following steps:
1) reacting gas with solid circle is made to be reacted into reactor part, output is with reaction is not solid completely The reaction product of body.
2) reaction product with unreacted solid of output enters cyclic part above above-mentioned reactor, isolates particle diameter Larger not reaction solid particle completely enters solid settling section, and gas and the smaller solid particle of high conversion rate enter solid Segregation section.Solid control valve by lower diagonal and thereon into solid settling section enters air inlet pipe and mixed with reacting gas Conjunction is recycled back to reactor.
3) gas and the smaller solid particle of high conversion rate that above-mentioned cyclic part is isolated enter the two of solid segregation section Level cyclone separator, upper and lower ends distinguish isolated gas-solid phase reaction product, and gas-phase product enters condensation portion.
4) above-mentioned isolated gas phase reaction product enters Liquid acquisition tank after entering condenser condensation.
Fluorspar Powder of the present invention produces the method for hydrogen fluoride, the reaction condition of reactor, used reaction raw materials Species and its consumption, it is specific as follows:
The present invention uses reaction raw materials, and reactor air inlet is from sulfuric acid vapor or sulfur trioxide and vapor mixed gas At least one of two kinds.Preferred molar ratio 4:1-1:4 sulfur trioxide and vapor gaseous mixture or mass fraction more than 95% Sulfuric acid vapor.Inert gas can be added into air inlet with reduce sulfuric acid vapor or sulfur trioxide and vapor gaseous mixture partial pressure with Reaction temperature needed for reducing.Nitrogen, hydrogen fluoride gas etc., preferred fluorinated hydrogen, and mole fraction may be selected in inert gas Less than 30%.Inert gas content is too high to reduce reaction rate.
30-200 μm, preferably 50-100 μm of Fluorspar Powder average grain diameter used of the invention.Calcium Fluoride Content is more than in Fluorspar Powder 80%, preferably more than 90% high-purity calcirm-fluoride.
Above-mentioned steps 1) in, 170-400 degrees Celsius of reactor operation temperature, 250-350 degrees Celsius of preferable temperature;Operation pressure Power is 0.5-2bar, preferably 0.8-1.2bar;The preferred 0.9-0.12m/s of operating gas velocity 0.07-0.15m/s.
Above-mentioned steps 2) in, cyclic part primary cyclone operating pressure 0.5-2bar, preferably 0.7-1.1bar;Gu Body settling section operating pressure 0.5-2bar, preferably 0.7-1.1bar.30-70 ° of angle between inclined tube and horizontal plane, preferably 50-60 °, Upper and lower ends difference in height is more than 10cm.Control valve aperture 0.1-0.7, preferably 0.3-0.5 on inclined tube, predetermined amount of flow is pressed with solid By and gas will not enter solid deposit section be advisable.
Above-mentioned predetermined amount of flow enters solid deposition section flow plus benefit for complete reaction solid from primary cyclone Fill Fluorspar Powder amount of solid.Above-mentioned supplement Fluorspar Powder amount of solid is equal to step 3) in isolate 0.9-1.2 times of amount of solid, preferably 1- 1.1 again.
Above-mentioned steps 3) in, cyclic part primary cyclone operating pressure;Solid receiving tank operating pressure 0.5- 2bar, preferably 0.7-1.05bar.
Above-mentioned steps 4) in, condenser is divided into two sections, is cooled down respectively using cooling water and chilled brine.Or using only cooling Water, wherein second segment cooling water temperature are less than 15 degrees Celsius.
Above-mentioned shell of reactor has two schemes according to using unstrpped gas species difference.One preferred scheme is to select sulphur Acid vapor is as unstripped gas, it is necessary to needed for the offer reaction of additional amount of heat, install closing heating shell outside reactor additional, use electricity Heating.Another preferred scheme is that heat is by sulfur trioxide needed for reaction as unstripped gas from sulfur trioxide with vapor gaseous mixture There is provided with water reaction generation sulfuric acid heat release, additional closing heating shell can be changed to lagging casing or still using closing heating shell, Use electrical heat tracing.
Using the method for the present invention, high-purity anhydrous hydrogen fluoride can be produced.
The characteristics of present invention has following prominent compared with prior art and effect:
1st, solid-phase reactant quickly flows in reactor, it is to avoid agglomerate glues the appearance of the anomalies such as wall, improves Mass transfer, heat transfer efficiency, being capable of the effectively save energy.
2nd, the Fluorspar Powder of different-grain diameter is separated using cyclone separator, the residence time of big particle diameter is short, and conversion ratio is low, enters Enter cyclic part to be circulated;The degree of wear of small particle is high, and the residence time is long, and conversion ratio is also high, close to reaction completely, enters Solid segregation section isolates system as solid reaction product.The reaction late phase reaction for so solving the presence of other techniques is stranded Difficulty, the problem of reaction time is long.Simultaneously can be by controlling control valve aperture control on tolerance size and inclined tube ciculation fluidized The cycling rate of bed, controls the solid product ratio isolated to control solid reaction degree.
3rd, liquid condensation is controlled by condensate temperature and consumption, when charging proportioning generation problem causes to contain in gaseous product Product quality can be controlled during other impurities by installing multi-stage condensing device additional by having.
Brief description of the drawings
Fig. 1 is the circulating fluidized bed device schematic diagram that Fluorspar Powder of the present invention produces hydrogen fluoride;
Description of reference numerals:
1 reactor, 2 primary cyclones, 3 solids deposition section, 4 inclined tubes, 5 control valves, 6 secondary cyclones, 7 Counterbalance valve, 8 solid receiving tanks, 9 condensers, 10 Liquid acquisition tanks.
Embodiment
Following examples are the scopes being not intended to limit the present invention in order to further illustrate the present invention.
Reacting gas with solid circle is reacted into 1 reactor, and output is anti-with incomplete reaction solid Product is answered to enter cyclic part, 2 primary cyclones isolate the larger not reaction solid particle completely of particle diameter and enter 3 solids Settling section, and gas and the smaller solid particle of high conversion rate enter solid segregation section.Solid into solid settling section passes through The inclined tube of lower section 4 and 5 control valves thereon enter air inlet pipe and return reactor with reacting gas mixing circulation.Cyclic part is isolated Gas and the smaller solid particle of high conversion rate enter 6 secondary cyclones of solid segregation section, upper and lower ends divide respectively From gas-solid phase reaction product is obtained, gas-phase product enters condensation portion, and solid product enters 8 solid receiving tanks by 7 counterbalance valves. Gas phase reaction product enters 10 Liquid acquisition tanks after entering the condensation of 9 condensers.
Embodiment 1
Mol ratio 1:1:1.5 sulfur trioxide, vapor and HF gaseous mixtures is previously heated to 300 Celsius as unstripped gas Degree, with 10.0m3/ h gas velocity enters reactor air inlet pipe, is mixed into reactor with solid circle and is reacted.Reactor is operated 350 degrees Celsius of temperature, pressure 1.2bar.Reaction product of the output with not reaction solid completely enters cyclic part, enters one-level Cyclone separator isolates the larger incomplete reaction solid particle of particle diameter.Primary cyclone pressure drop 0.05bar.Sink solid Body enters solid settling section, and gas and the smaller solid particle of high conversion rate enter solid segregation section.Into solid settling section Solid control valve by lower diagonal and thereon enter air inlet pipe and return reactor with reacting gas mixing circulation.Inclined tube is long 25cm, upper and lower ends difference in height 20cm.The gas and the smaller solid particle of high conversion rate that cyclic part is isolated enter solid The secondary cyclone of segregation section, secondary cyclone pressure drop 0.05bar.Its upper and lower ends distinguishes isolated gas-solid phase Reaction product, gas-phase product enters condensation portion, and solid product enters solid receiving tank by counterbalance valve.Gas phase reaction product enters Enter Liquid acquisition tank after entering condenser condensation.Condenser using 5 degrees Celsius of chilled brines condense obtaining hydrogen fluoride liquid.
Using 35 μm of average grain diameter, the Fluorspar Powder of Calcium Fluoride Content 94% as supplement solid below solid settling section plus Enter.It is 5.42kg/min that it, which supplements flow,.
Obtain containing in solid product and contain hydrogen fluoride more than 90% in calcirm-fluoride 0.8%, the condensate liquid of gaseous product.
Embodiment 2
The sulfuric acid vapor and HF gases of mass fraction 98% are with mol ratio 1:1.5 mixing are previously heated to as unstripped gas 350 degrees Celsius, with 8.0m3/ h gas velocity enters reactor air inlet pipe, is mixed into reactor with solid circle and is reacted.Reaction 350 degrees Celsius of device operation temperature, pressure 0.95bar.Tiny structure can reduce the leakage probability of hazardous reaction thing and product.Reactor Output with not completely reaction solid reaction product enter cyclic part, by primary cyclone isolate particle diameter compared with Big does not react solid particle completely.Primary cyclone pressure drop 0.05bar.Sinking solids enter solid settling section, and gas Body and the smaller solid particle of high conversion rate enter solid segregation section.Solid into solid settling section passes through lower diagonal and its On control valve enter air inlet pipe and return reactor with reacting gas mixing circulation.The long 25cm of inclined tube, upper and lower ends difference in height 15cm.The gas and the smaller solid particle of high conversion rate that cyclic part is isolated enter two grades of cyclonic separations of solid segregation section Device, secondary cyclone pressure drop 0.05bar.Its upper and lower ends distinguishes isolated gas-solid phase reaction product, and gas-phase product enters Enter condensation portion, solid product enters solid receiving tank by counterbalance valve.Gas phase reaction product enters after entering condenser condensation Liquid acquisition tank.One section of condenser, 20 degrees Celsius of use cooling water, two sections of uses, 10 degrees Celsius of cooling waters are successively condensed, and are obtained To hydrogen fluoride liquid.
Using 30 μm of average grain diameter, the Fluorspar Powder of Calcium Fluoride Content 97% as supplement solid below solid settling section plus Enter.It is 5.21kg/min that it, which supplements flow,.
Obtain containing in solid product and contain hydrogen fluoride more than 90% in calcirm-fluoride 0.8%, the condensate liquid of gaseous product.

Claims (9)

1. a kind of circulating fluidized bed system that hydrogen fluoride is produced with Fluorspar Powder, including:
1) reactor, the expanding reach more than direct tube section, direct tube section, the section of the undergauge below direct tube section and closing heating shell structure Into undergauge section has the internal diameter being gradually reduced downwards, and is provided with air inlet pipe in its bottom, and whole reactor is heated outer by closing Shell is isolated from the outside, and expanding reach side has outlet to be used to connect cyclic part;
2) cyclic part, by primary cyclone, solid settling section, is connected to the inclined tube of reactor air inlet pipe section, on inclined tube Control valve and lagging casing constitute, primary cyclone import is connected with reactor expanding reach side exit, solid Settling section is the straight tube that one side supplements adapter provided with solid, solid settling section upper end and primary cyclone outlet at bottom phase Even, lower end is connected with inclined tube section, and inclined tube section is connected with the air inlet pipe side wall of reactor undergauge section bottom;Whole cyclic part by Lagging casing is coated;
3) solid segregation section, is made up of secondary cyclone and solid receiving tank, and secondary cyclone entrance revolves with one-level Wind separator top exit is connected, and solid receiving tank is connected with secondary cyclone outlet at bottom, the separation of solid separate section Gas-particle two-phase product, and the complete solid of reaction is collected, it is used as solid product;
4) gas condensation portion, by condenser, Liquid acquisition tank is constituted, and gas condensation portion will separate remaining in solid segregation section The gas-phase product gone out liquefies and collected.
2. the method that a kind of Fluorspar Powder of system described in use claim 1 produces hydrogen fluoride, it is characterised in that including following step Suddenly:
1) reacting gas with solid circle is made to be reacted into reactor, output is with the not reaction of reaction solid completely Product;
2) reaction product with unreacted solid of output enters cyclic part, primary cyclone above above-mentioned reactor The larger not reaction solid particle completely of particle diameter is isolated, into solid settling section, and gas and the smaller solid of high conversion rate Particle enters solid segregation section, and the solid control valve by lower diagonal and thereon into solid settling section enters air inlet pipe Reactor is returned with reacting gas mixing circulation;
3) gas and the smaller solid particle of high conversion rate that cyclic part is isolated enter two grades of whirlwind point of solid segregation section From device, upper and lower ends respectively obtain gas-solid phase reaction product, and gas-phase product enters condensation portion, and solid phase reaction product enters solid Receiving tank;
4) the isolated gas phase reaction product of above-mentioned secondary cyclone enters Liquid acquisition tank after entering condenser condensation.
3. method as claimed in claim 2, it is characterised in that:Step 1) in, 170-400 degrees Celsius of reactor operation temperature, Operating pressure 0.5-2bar, operating gas velocity 0.07-0.15m/s.
4. method as claimed in claim 2, it is characterised in that:Step 1) in, 250-350 degrees Celsius of reactor operation temperature, Operating pressure 0.8-1.2bar, operating gas velocity 0.9-0.12m/s.
5. method as claimed in claim 2, it is characterised in that:Step 2) in, cyclic part primary cyclone operation pressure Power 0.5-2bar,;Solid settling section operating pressure 0.5-2bar, 30-70 ° of angle between inclined tube and horizontal plane, upper and lower ends height Difference is more than control valve aperture 0.1-0.7 on 10cm, inclined tube.
6. method as claimed in claim 2, it is characterised in that:Step 2) in, cyclic part primary cyclone operation pressure Power 0.7-1.1bar;Solid settling section operating pressure 0.7-1.1bar, 50-60 ° of angle between inclined tube and horizontal plane, upper and lower ends are high Degree difference is more than control valve aperture 0.3-0.5 on 10cm, inclined tube.
7. method as claimed in claim 2, it is characterised in that:
Reactor predetermined amount of flow is reaction solid does not enter solid deposition section flow plus supplement from primary cyclone completely Fluorspar Powder amount of solid, above-mentioned supplement Fluorspar Powder amount of solid be equal to step 3) in secondary cyclone bottom obtain solid reaction production 0.9-1.2 times of object amount.
8. method as claimed in claim 2, it is characterised in that:From sulfuric acid vapor as unstripped gas, envelope is installed additional outside reactor Heating shell is closed, electrical heating is used.
9. method as claimed in claim 2, it is characterised in that:From sulfur trioxide and vapor gaseous mixture as unstripped gas, Heat needed for reaction is provided by sulfur trioxide and water reaction generation sulfuric acid heat release, and additional closing heating shell is changed to lagging casing or still Shell is heated using closing, electrical heat tracing is used.
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Cited By (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108862201A (en) * 2018-09-12 2018-11-23 浙江大学 A method of hydrogen fluoride is prepared using prodan
CN108910826A (en) * 2018-10-17 2018-11-30 杨松 It is a kind of to prepare hydrogen fluoride recirculating fluidized bed reacting furnace
CN108910827A (en) * 2018-10-17 2018-11-30 杨松 It is a kind of to prepare hydrogen fluoride process unit
CN108975275A (en) * 2018-10-17 2018-12-11 杨松 It is a kind of to prepare hydrogen fluoride reaction device
CN109019517A (en) * 2018-10-17 2018-12-18 杨松 A kind of application method preparing hydrogen fluoride recirculating fluidized bed reacting furnace
CN109250688A (en) * 2018-10-17 2019-01-22 杨松 It is a kind of to prepare hydrogen fluoride recirculating fluidized bed degasser
CN109260742A (en) * 2018-10-17 2019-01-25 杨松 A kind of application method preparing hydrogen fluoride recirculating fluidized bed rectifier unit
CN112142009A (en) * 2020-09-22 2020-12-29 宜章弘源化工有限责任公司 Method and equipment for producing anhydrous hydrogen fluoride
CN113262750A (en) * 2021-07-19 2021-08-17 联仕(昆山)化学材料有限公司 Electronic-grade hydrofluoric acid production device
CN115722158A (en) * 2022-11-28 2023-03-03 兰州理工大学 Multilayer expanded fluidized bed reactor system and process for producing hydrogen fluoride
CN115990439A (en) * 2022-11-28 2023-04-21 兰州理工大学 Anhydrous hydrogen fluoride production equipment and process based on expansion fluidized bed

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4310501A (en) * 1979-07-13 1982-01-12 Metallgesellschaft A.G. Process for producing hydrogen fluoride
CN102757018A (en) * 2012-08-06 2012-10-31 福州大学 Method for producing hydrogen fluoride by using fluorite powders
CN102923664A (en) * 2012-11-27 2013-02-13 福州大学 Method for producing hydrogen fluoride by virtue of gas-solid-liquid associative reaction method
CN103332655A (en) * 2013-07-09 2013-10-02 衢州市鼎盛化工科技有限公司 Hydrogen fluoride preparation method and apparatus thereof
CN105645358A (en) * 2016-03-14 2016-06-08 衢州市鼎盛化工科技有限公司 Method for preparing hydrogen fluoride from fluosilicic acid

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4310501A (en) * 1979-07-13 1982-01-12 Metallgesellschaft A.G. Process for producing hydrogen fluoride
CN102757018A (en) * 2012-08-06 2012-10-31 福州大学 Method for producing hydrogen fluoride by using fluorite powders
CN102923664A (en) * 2012-11-27 2013-02-13 福州大学 Method for producing hydrogen fluoride by virtue of gas-solid-liquid associative reaction method
CN103332655A (en) * 2013-07-09 2013-10-02 衢州市鼎盛化工科技有限公司 Hydrogen fluoride preparation method and apparatus thereof
CN105645358A (en) * 2016-03-14 2016-06-08 衢州市鼎盛化工科技有限公司 Method for preparing hydrogen fluoride from fluosilicic acid

Cited By (15)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108862201A (en) * 2018-09-12 2018-11-23 浙江大学 A method of hydrogen fluoride is prepared using prodan
CN109260742A (en) * 2018-10-17 2019-01-25 杨松 A kind of application method preparing hydrogen fluoride recirculating fluidized bed rectifier unit
CN109260742B (en) * 2018-10-17 2021-06-04 杨松 Use method of circulating fluidized bed rectification device for preparing hydrogen fluoride
CN108975275A (en) * 2018-10-17 2018-12-11 杨松 It is a kind of to prepare hydrogen fluoride reaction device
CN109019517A (en) * 2018-10-17 2018-12-18 杨松 A kind of application method preparing hydrogen fluoride recirculating fluidized bed reacting furnace
CN109250688A (en) * 2018-10-17 2019-01-22 杨松 It is a kind of to prepare hydrogen fluoride recirculating fluidized bed degasser
CN108910826A (en) * 2018-10-17 2018-11-30 杨松 It is a kind of to prepare hydrogen fluoride recirculating fluidized bed reacting furnace
CN108910826B (en) * 2018-10-17 2019-12-24 杨松 Circulating fluidized bed reaction furnace for preparing hydrogen fluoride
CN108910827A (en) * 2018-10-17 2018-11-30 杨松 It is a kind of to prepare hydrogen fluoride process unit
CN112142009A (en) * 2020-09-22 2020-12-29 宜章弘源化工有限责任公司 Method and equipment for producing anhydrous hydrogen fluoride
CN113262750A (en) * 2021-07-19 2021-08-17 联仕(昆山)化学材料有限公司 Electronic-grade hydrofluoric acid production device
CN113262750B (en) * 2021-07-19 2021-11-02 联仕(昆山)化学材料有限公司 Electronic-grade hydrofluoric acid production device
CN115722158A (en) * 2022-11-28 2023-03-03 兰州理工大学 Multilayer expanded fluidized bed reactor system and process for producing hydrogen fluoride
CN115990439A (en) * 2022-11-28 2023-04-21 兰州理工大学 Anhydrous hydrogen fluoride production equipment and process based on expansion fluidized bed
CN115722158B (en) * 2022-11-28 2024-07-16 兰州理工大学 Multilayer expansion fluidized bed reactor system and process for producing hydrogen fluoride

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