CN108217599A - A kind of reaction unit that hydrogen fluoride is prepared suitable for calcirm-fluoride - Google Patents

A kind of reaction unit that hydrogen fluoride is prepared suitable for calcirm-fluoride Download PDF

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Publication number
CN108217599A
CN108217599A CN201810222840.0A CN201810222840A CN108217599A CN 108217599 A CN108217599 A CN 108217599A CN 201810222840 A CN201810222840 A CN 201810222840A CN 108217599 A CN108217599 A CN 108217599A
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China
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reactor
fluoride
hydrogen fluoride
calcirm
reaction unit
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CN201810222840.0A
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Inventor
周贞锋
董寒杰
应盛荣
姜战
应悦
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Dingsheng Chemical & Technology Co Ltd
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Dingsheng Chemical & Technology Co Ltd
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Priority to CN201810222840.0A priority Critical patent/CN108217599A/en
Publication of CN108217599A publication Critical patent/CN108217599A/en
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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

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Devices And Processes Conducted In The Presence Of Fluids And Solid Particles (AREA)

Abstract

The present invention relates to a kind of reaction unit that hydrogen fluoride is prepared suitable for calcirm-fluoride, reactor and heat energy apparatus;The reactor is hermetically sealed vertical type hollow structure;First material import and gas vent are provided at the top of the reactor, bottom is provided with material delivery outlet;Blender and loading device are additionally provided in the reactor;The heat energy apparatus is used to provide thermal energy to the loading device;The heat energy apparatus includes thermal medium input pipe and thermal medium efferent duct;The bottom surface of the loading device is provided with the heat transfer layer of enclosed construction;The thermal medium input pipe and thermal medium efferent duct connect respectively with the heat transfer layer.Present device heat transfer area bigger and heat-transfer effect is more preferable;Save energy consumption;In equal production capacity, power consumption is saved.It is suitble to fine calcium fluoride powder production hydrogen fluoride;Will not generate airborne dust in into reactor, hydrogen fluoride gas be across wet-milling after send out reactor, dust will not be taken away.

Description

A kind of reaction unit that hydrogen fluoride is prepared suitable for calcirm-fluoride
Technical field
The present invention relates to the preparation facilities technical fields of hydrogen fluoride, are suitable for calcirm-fluoride more particularly, to one kind and prepare fluorination The reaction unit of hydrogen.
Background technology
Hydrogen fluoride (Hydrogen Fluoride), chemical molecular formula HF, molecular weight 20.01, soluble easily in water, ethyl alcohol.Nothing It is colourless transparent liquid under water hydrogen fluoride (abbreviation AHF) low temperature or pressure, 19.4 DEG C of boiling point, -83.37 DEG C of fusing point, density 1.008g/cm3(water=1).In room temperature and highly volatile under room temperature into white smoke.Its chemical property is extremely active, can with alkali, The reactions such as metal, oxide and silicate.Hydrogen fluoride is the basis of modern fluorination work, is to produce element fluorine, various fluorine refrigeration The most basic raw material of agent, fluorine-containing new material, inorganic fluorine salt dissolving, various organic fluorides etc..
The method for producing hydrogen fluoride in industrial production has sulfuric acid process:By dried Fluorspar Powder and sulfuric acid by proportioning 1:(1.2 ~1.3) it mixes, is sent into swinging reacting furnace and is reacted, gas phase temperature control is at 280 DEG C ± 50 DEG C in stove.After reaction Gas enters topping still, removes sulfuric acid, moisture and Fluorspar Powder in gas, prepares thick hydrogen fluoride gas.Thick hydrogen fluoride gas Degassed tower is condensed into liquid again, subsequently into rectifying column rectifying.Hydrogen fluoride after refined is absorbed with water to be produced to get hydrofluoric acid Product.
Traditional calcirm-fluoride has compared with strict requirements the fineness of calcium fluoride powder during preparing hydrogen fluoride, due to reacting Airborne dust in stove, meticulous calcium fluoride powder can leave reactor together with hydrogen fluoride gas, into aftertreatment systems, after causing The blocking of the equipment such as continuous process pipe, scrubbing tower and condenser.This problem limits ultra-fine calcirm-fluoride as raw material system always Standby hydrofluoric acid.However as the development of circular economy, the calcium fluoride powder extracted from calcium fluoride sludge, non-ferro metals debris extraction Calcium fluoride powder etc. be ultra-fine calcirm-fluoride, it is current Acid of Hydrofluoric Acid Production that ultra-fine calcirm-fluoride how to be allowed, which to enter Acid of Hydrofluoric Acid Production system, Technology urgent problem to be solved.
Therefore, it is necessary to research and develop a kind of new reaction unit for being suitable for calcirm-fluoride and preparing hydrogen fluoride.
Invention content
The present invention provides a kind of new reaction unit for being suitable for calcirm-fluoride and preparing hydrogen fluoride.
The present invention also provides a kind of reaction unit that hydrogen fluoride is prepared suitable for fine calcium fluoride powder, to solve the prior art In fine calcium fluoride powder the problem of be easy to causeing the blocking of swinging reacting furnace and subsequent technique pipe-line equipment.
Technical problem solved by the invention is realized using following technical scheme:
A kind of reaction unit that hydrogen fluoride is prepared suitable for calcirm-fluoride, including:Reactor and heat energy apparatus;
The reactor is hermetically sealed vertical type hollow structure;Be provided at the top of the reactor first material into Mouth and gas vent, bottom are provided with material delivery outlet;Blender and loading device are additionally provided in the reactor;
The heat energy apparatus is used to provide thermal energy to the loading device;The heat energy apparatus include thermal medium input pipe and Thermal medium efferent duct;The bottom surface of the loading device is provided with the heat transfer layer of enclosed construction;The thermal medium input pipe and heat are situated between Matter efferent duct connects respectively with the heat transfer layer.
As preferred technical solution, feeder is further included, the feeder is arranged on the top of the reactor, and with The first material import is connected;The feeder includes feeder ontology, and the is equipped in one end of the feeder ontology Two material inlets and third material inlet, the other end are connected with the first material import, are set in the feeder ontology There is mixing device.
As preferred technical solution, the mixing device is spiral blender or paddle formula blender.In batch mixing mistake The chemical reaction of part occurs for Cheng Zhong.
As preferred technical solution, the blender includes rotation axis, the material scraping plate being arranged in the rotation axis, institute It is multigroup to state material scraping plate, above the loading device, and is contacted in the form of dead weight with the loading device, the bearing material dress It puts and is fixed on outer support frame, feed opening is equipped on loading device, the material on the loading device of upper strata is pushed away by the material scraping plate It is dynamic to descend lower floor's material bearing disc or discharge from the reaction unit;The rotation axis is vertically-mounted, and the material scraping plate is along institute State the vertical direction installation of rotation axis.
As preferred technical solution, the material scraping plate is distributed at equal intervals along the vertical direction of the rotation axis.
As preferred technical solution, the diameter of the loading device and the internal diameter of the reactor match;It is described anti- It is 2~50 to answer the quantity of loading device that device is equipped with.
As preferred technical solution, it is equipped with chuck in the outside of the reactor, the chuck is equipped with thermal medium the The second delivery outlet of two input ports and thermal medium.
As preferred technical solution, the thermal medium of the heat energy apparatus is included in hot-air, conduction oil, steam, fused salt Any one medium.
As preferred technical solution, the diameter of the loading device and the internal diameter of the reactor match.
As preferred technical solution, the thermal medium input pipe and thermal medium efferent duct of the heat energy apparatus respectively with device Heating system in addition is connected, to ensure the thermal energy needed for reaction.
As preferred technical solution, the gas vent is connected by pipeline with negative pressure device, in technical process, In the reactor hydrogen fluoride gas is preferably recycled under negative pressure state in tiny structure to realize always.
As preferred technical solution, the reactor is assembled by the way of splicing;The loading device is using splicing Mode assemble.
As preferred technical solution, the reactor diameter is 1 meter~10 meters;Highly 5 meters~60 meters.
As preferred technical solution, insulating layer is additionally provided on the outside of the chuck, to reduce hot loss of energy.
The invention has the advantages that:
1) technical solution of the invention, the enclosed construction heat transfer layer being provided with by the bottom surface of loading device, heat transfer Area bigger and heat-transfer effect is more preferable;Heat insulation effect is more preferable;Save energy consumption;In equal production capacity, tumbler power is significantly Less than the rotary reaction furnace of the prior art, power consumption is saved.
2) another technical solution of the invention is suitble to fine calcium fluoride powder to produce hydrogen fluoride;It is particularly suitable for from calcirm-fluoride dirt The utilization of calcium fluoride powder, the calcium fluoride powder of non-ferro metals debris extraction extracted in mud, after blending together " wet-milling " in advance in feeder, Will not generate airborne dust in into reactor, hydrogen fluoride gas be across wet-milling after send out reactor, dust will not be taken away.
3) more advantageous to the subsequent purification processing of hydrogen fluoride gas since hydrogen fluoride gas does not carry dust, scrubbing tower is not It can block, suspended matter and sediment are reduced in washing acid, can extend the acid pump service life.
4) the thermal medium selectivity in the present invention is wider, and the thermal medium of this technology can be high-temperature hot-air or height Warm steam, conduction oil, fused salt etc..
5) reaction unit is to stand, and facilitates splicing;Material bearing disc is also what is stood, can also be spliced;It therefore can be anti- The diameter of device is answered to accomplish very greatly, the production capacity of list covering device can be very big.In the case of equal production capacity, the prior art may Need 2 sets or more covering devices, as long as and this technology set of device, investment can be greatlyd save.Due to that can splice, set Standby manufacture, transport and installation is all more simple and convenient so that the diameter of reaction unit can select in 1 meter~10 meters;It is high Degree selects in 5 meters~60 meters.
Description of the drawings
It, below will be to embodiment in order to illustrate more clearly of embodiment of the present invention or technical solution of the prior art Or attached drawing needed to be used in the description of the prior art is briefly described, it should be apparent that, the accompanying drawings in the following description is only It is some embodiments of the present invention, for those of ordinary skill in the art, in the premise of not making the creative labor property Under, it can also be obtained according to these attached drawings other attached drawings.
Fig. 1 is the present invention:A kind of the first structure diagram for the reaction unit that hydrogen fluoride is prepared suitable for calcirm-fluoride;
Fig. 2 is the present invention:A kind of second of structure diagram of the reaction unit that hydrogen fluoride is prepared suitable for calcirm-fluoride.
Specific embodiment
In order to be easy to understand the technical means, the creative features, the aims and the efficiencies achieved by the present invention, tie below Conjunction is specifically illustrating, and the present invention is further explained.
Embodiment 1
With reference to shown in Fig. 1, a kind of reaction unit that hydrogen fluoride is prepared suitable for calcirm-fluoride, including reactor 1 and thermal energy Device.Wherein reactor 1 is hermetically sealed vertical type hollow structure, and the reactor in the present embodiment is vertical cylindrical structure. First material import 11 and gas vent 12 are provided at the top of reactor 1, bottom is provided with material delivery outlet 13, i.e. sulfuric acid Calcium exports.Blender 15 and loading device 153 are additionally provided in reactor 1.Heat energy apparatus is used to provide heat to loading device 153 Energy.The heat energy apparatus includes thermal medium input pipe 143 and thermal medium efferent duct 144;The bottom surface of loading device 153 is provided with closing The heat transfer layer 155 of structure, thermal medium input pipe 143 and thermal medium efferent duct 144 connect respectively with heat transfer layer 155 so that material It is reacted at a suitable temperature.This kind of mode so that heat transfer area bigger, heat-transfer effect is more preferable, saves energy consumption.And heat The range of choice of medium is more extensive, for example can use any one medium included in hot-air, conduction oil, steam, fused salt. And can only be in the prior art high-temperature hot-air technology, limit application range.Thermal medium input pipe 143 and thermal medium efferent duct 144 are connected respectively with the heating system other than device, to ensure the thermal energy needed for reaction.
In order to solve the defects of existing equipment is difficult to ultra-fine calcirm-fluoride preparing hydrogen fluoride as raw material, in the present embodiment Further include feeder 2.The feeder 2 includes feeder ontology 21, and second material import is equipped in one end of feeder ontology 21 22 (i.e. calcium fluoride powder imports) and third material inlet 23 (i.e. sulfuric acid import), the other end is connected with first material import 11, Mixing device 24 is equipped in feeder ontology 21.Wherein mixing device 24 can select spiral blender or paddle formula batch mixing Device, mixing device 24 is spiral blender in the present embodiment, using spiral blender so that batch mixing is uniform.The feeder 2 The top of reactor 1 is arranged on, and is connected with the first material import 11 of reactor 1.Raw material is by feeder 2, in batch mixing In the process, the chemical reaction of part occurs.
Blender 15 in this implementation column includes rotation axis 151 and material scraping plate 152.Material scraping plate 152 is fixed on rotation axis 151 On, above loading device 153, and contacted in the form of dead weight with loading device 153.The loading device 153 is fixed on outer branch In support (not shown), feed opening 154 is equipped on loading device 153, the material on upper strata loading device 153 is by scraper The promotion of plate 152 can descend lower floor's material bearing disc 153, and eventually by the material delivery outlet 13 of reactor 1, calcium sulfate is drawn off reactor 1.The rotation axis 151 is vertically-mounted, and material scraping plate 152 is installed along the vertical direction of rotation axis 151.Above-mentioned material scraping plate according to It needs to be set as multigroup, and is distributed at equal intervals along the vertical direction of rotation axis 151.
The internal diameter of the diameter and reactor 1 of loading device 153 in the present embodiment matches, and can be slightly smaller than reactor 1 Internal diameter;The quantity for the loading device that the reactor is equipped with is 2-50.
In order to enable always in micro-vacuum state in reactor 1, gas vent 12 is by pipeline and negative pressure device (in figure It is not shown) it is connected, in technical process, preferably returned under negative pressure state in tiny structure with realizing always in reactor 1 Receive hydrogen fluoride gas.
Above-mentioned reaction unit is to stand, therefore facilitate splicing;Material bearing disc is also what is stood, can also be spliced;It therefore can Very big the diameter of reaction unit is accomplished, the production capacity of list covering device can be very big.In the case of equal production capacity, existing skill Art may need 2 sets or more covering devices, as long as and this technology set of device, investment can be greatlyd save.Due to that can splice, Therefore the manufacture of equipment, transport and installation are all more simple and convenient so that reaction unit can be in a diameter of 1 meter~10 meters Selection;Height selects in 5 meters~60 meters.And the rotary furnace of the prior art, when diameter reaches 3.8 meters, gross weight is up to hundreds of tons; Manufacture, transport, installation are required for dedicated equipment and vehicle;Moreover, being limited by transportation clearance, revolution can not possibly be improved again Stove diameter, the structure of rotary furnace also determine that device can not possibly be spliced, that is to say, that the reaction dress of this form of rotary furnace It puts, the production capacity of list covering device can not possibly be improved again.
Reaction unit in the present embodiment is suitble to fine calcium fluoride powder to produce hydrogen fluoride;It is particularly suitable for from calcium fluoride sludge The utilization of the calcium fluoride powder of extraction, the calcium fluoride powder of non-ferro metals debris extraction, after blending together " wet-milling " in advance in feeder, enters Will not generate airborne dust in reactor, hydrogen fluoride gas be across wet-milling after send out reactor, dust will not be taken away;It is filled by bearing material The enclosed construction heat transfer layer that the bottom surface put is provided with, heat transfer area bigger and heat-transfer effect is more preferable;Heat insulation effect is more preferable;It saves Energy consumption;In equal production capacity, power is significantly less than the rotary reaction furnace of the prior art, saves power consumption;Thermal medium selects Property is wider, and the thermal medium of this technology can be high-temperature hot-air or high-temperature steam, conduction oil, fused salt etc.;Due to hydrogen fluoride Gas does not carry dust, more advantageous to the subsequent purification processing of hydrogen fluoride gas, and scrubbing tower will not block, suspended matter in washing acid It is reduced with sediment, the acid pump service life can be extended;Using split type package assembly, manufacture, transport, the installation of equipment are all simpler It is single, more convenient;The production capacity of single set equipment can reach several times of prior-art devices.
Embodiment 2
As shown in Fig. 2, another scheme of the present invention is, the present invention is equipped with chuck 14, chuck 14 in the outside of reactor 1 It is equipped with the second input port of thermal medium 141 of heating medium inflow and outflow and the second delivery outlet of thermal medium 142.In the outer of chuck 14 Side is additionally provided with insulating layer (not shown), to reduce hot loss of energy.
The basic principles, main features and the advantages of the invention have been shown and described above.The technology of the industry Personnel are it should be appreciated that the present invention is not limited to the above embodiments, and the above embodiments and description only describe this The principle of invention, without departing from the spirit and scope of the present invention, various changes and improvements may be made to the invention, these changes Change and improvement all fall within the protetion scope of the claimed invention.The claimed scope of the invention by appended claims and its Equivalent thereof.

Claims (10)

1. a kind of reaction unit that hydrogen fluoride is prepared suitable for calcirm-fluoride, which is characterized in that including:Reactor and thermal energy dress It puts;
The reactor is hermetically sealed vertical type hollow structure;Be provided at the top of the reactor first material import and Gas vent, bottom are provided with material delivery outlet;Blender and loading device are additionally provided in the reactor;
The heat energy apparatus is used to provide thermal energy to the loading device;The heat energy apparatus includes thermal medium input pipe and heat is situated between Matter efferent duct;The bottom surface of the loading device is provided with the heat transfer layer of enclosed construction;The thermal medium input pipe and thermal medium are defeated Outlet pipe connects respectively with the heat transfer layer.
2. a kind of reaction unit that hydrogen fluoride is prepared suitable for calcirm-fluoride according to claim 1, which is characterized in that also wrap Feeder is included, the feeder is arranged on the top of the reactor, and is connected with the first material import;The charging Device includes feeder ontology, and second material import and third material inlet, the other end are equipped in one end of the feeder ontology It is connected with the first material import, mixing device is equipped in the feeder ontology.
3. a kind of reaction unit that hydrogen fluoride is prepared suitable for calcirm-fluoride according to claim 2, which is characterized in that described Mixing device is spiral blender or paddle formula blender.
4. a kind of reaction unit that hydrogen fluoride is prepared suitable for calcirm-fluoride according to claim 1 or 2, which is characterized in that The blender includes rotation axis, the material scraping plate being arranged in the rotation axis, and the material scraping plate is multigroup, positioned at the bearing material It above device, and is contacted in the form of dead weight with the loading device, the loading device is fixed on outer support frame, is filled in bearing material It puts equipped with feed opening, the material on the loading device of upper strata can be descended lower floor's material bearing disc or from described anti-by material scraping plate promotion Device is answered to discharge;The rotation axis is vertically-mounted, and the material scraping plate is installed along the vertical direction of the rotation axis.
5. a kind of reaction unit that hydrogen fluoride is prepared suitable for calcirm-fluoride according to claim 4, which is characterized in that described Material scraping plate is distributed at equal intervals along the vertical direction of the rotation axis.
6. a kind of reaction unit that hydrogen fluoride is prepared suitable for calcirm-fluoride according to claim 1, which is characterized in that described The diameter of loading device and the internal diameter of the reactor match;The quantity for the loading device that the reactor is equipped with is 2~50 It is a.
7. a kind of reaction unit that hydrogen fluoride is prepared suitable for calcirm-fluoride according to claim 1 or 2, which is characterized in that Chuck is equipped in the outside of the reactor, the chuck is equipped with the second delivery outlet of the second input port of thermal medium and thermal medium.
8. a kind of reaction unit that hydrogen fluoride is prepared suitable for calcirm-fluoride according to claim 1, which is characterized in that described The thermal medium of heat energy apparatus includes any one medium in hot-air, conduction oil, steam, fused salt.
9. a kind of reaction unit that hydrogen fluoride is prepared suitable for calcirm-fluoride according to claim 1 or 2, which is characterized in that The gas vent is connected by pipeline with negative pressure device.
10. a kind of reaction unit that hydrogen fluoride is prepared suitable for calcirm-fluoride according to claim 1 or 2, which is characterized in that The reactor is assembled by the way of splicing;The loading device is assembled by the way of splicing.
CN201810222840.0A 2018-03-19 2018-03-19 A kind of reaction unit that hydrogen fluoride is prepared suitable for calcirm-fluoride Pending CN108217599A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108609586A (en) * 2018-08-08 2018-10-02 宣城亨泰电子化学材料有限公司 A kind of reagent stage hydrofluoric acid producing device
CN111892023A (en) * 2020-07-30 2020-11-06 甘元松 Anti-channeling hydrogen fluoride reacting furnace
CN112645286A (en) * 2020-12-22 2021-04-13 内蒙古东岳金峰氟化工有限公司 High-efficient purification processing integrated device of hydrogen fluoride

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Publication number Priority date Publication date Assignee Title
GB462131A (en) * 1935-09-02 1937-03-02 Du Pont Improvements in or relating to the manufacture of hydrofluoric acid
US3282644A (en) * 1965-02-15 1966-11-01 Du Pont Process for the manufacture of hydrogen fluoride
CN85104494A (en) * 1984-05-18 1986-12-10 阿托化学公司 Sulfuric acid and fluorite are produced the method for hydrofluoric acid at the rotary oven internal reaction
CN101913565A (en) * 2010-08-12 2010-12-15 衢州市鼎盛化工科技有限公司 Method for preparing hydrogen fluoride from flousper powder and sulfuric acid
CN203790928U (en) * 2014-03-15 2014-08-27 宜章弘源化工有限责任公司 Fluidized bed tail gas utilization device in dry-method aluminum fluoride production
CN106660791A (en) * 2014-07-11 2017-05-10 大金工业株式会社 Method for producing hydrogen fluoride

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB462131A (en) * 1935-09-02 1937-03-02 Du Pont Improvements in or relating to the manufacture of hydrofluoric acid
US3282644A (en) * 1965-02-15 1966-11-01 Du Pont Process for the manufacture of hydrogen fluoride
CN85104494A (en) * 1984-05-18 1986-12-10 阿托化学公司 Sulfuric acid and fluorite are produced the method for hydrofluoric acid at the rotary oven internal reaction
CN101913565A (en) * 2010-08-12 2010-12-15 衢州市鼎盛化工科技有限公司 Method for preparing hydrogen fluoride from flousper powder and sulfuric acid
CN203790928U (en) * 2014-03-15 2014-08-27 宜章弘源化工有限责任公司 Fluidized bed tail gas utilization device in dry-method aluminum fluoride production
CN106660791A (en) * 2014-07-11 2017-05-10 大金工业株式会社 Method for producing hydrogen fluoride

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108609586A (en) * 2018-08-08 2018-10-02 宣城亨泰电子化学材料有限公司 A kind of reagent stage hydrofluoric acid producing device
CN108609586B (en) * 2018-08-08 2021-11-02 宣城亨泰电子化学材料有限公司 Reagent-grade hydrofluoric acid manufacturing device
CN111892023A (en) * 2020-07-30 2020-11-06 甘元松 Anti-channeling hydrogen fluoride reacting furnace
CN111892023B (en) * 2020-07-30 2021-08-06 烟台中瑞化工有限公司 Anti-channeling hydrogen fluoride reacting furnace
CN112645286A (en) * 2020-12-22 2021-04-13 内蒙古东岳金峰氟化工有限公司 High-efficient purification processing integrated device of hydrogen fluoride
CN112645286B (en) * 2020-12-22 2023-10-27 内蒙古东岳金峰氟化工有限公司 Hydrogen fluoride high-efficient purification processing integrated device

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