CN106406256A - Full-automatic hydrofluoric acid production system - Google Patents

Full-automatic hydrofluoric acid production system Download PDF

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Publication number
CN106406256A
CN106406256A CN201610842387.4A CN201610842387A CN106406256A CN 106406256 A CN106406256 A CN 106406256A CN 201610842387 A CN201610842387 A CN 201610842387A CN 106406256 A CN106406256 A CN 106406256A
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hydrofluoric acid
hydrogen fluoride
gas
tank
acid
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CN201610842387.4A
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CN106406256B (en
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戈烨铭
谢国彤
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Jiangsu Sino German Mstar Technology Ltd
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Jiangsu Sino German Mstar Technology Ltd
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    • GPHYSICS
    • G05CONTROLLING; REGULATING
    • G05BCONTROL OR REGULATING SYSTEMS IN GENERAL; FUNCTIONAL ELEMENTS OF SUCH SYSTEMS; MONITORING OR TESTING ARRANGEMENTS FOR SUCH SYSTEMS OR ELEMENTS
    • G05B19/00Programme-control systems
    • G05B19/02Programme-control systems electric
    • G05B19/418Total factory control, i.e. centrally controlling a plurality of machines, e.g. direct or distributed numerical control [DNC], flexible manufacturing systems [FMS], integrated manufacturing systems [IMS] or computer integrated manufacturing [CIM]
    • G05B19/41865Total factory control, i.e. centrally controlling a plurality of machines, e.g. direct or distributed numerical control [DNC], flexible manufacturing systems [FMS], integrated manufacturing systems [IMS] or computer integrated manufacturing [CIM] characterised by job scheduling, process planning, material flow
    • 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
    • GPHYSICS
    • G05CONTROLLING; REGULATING
    • G05BCONTROL OR REGULATING SYSTEMS IN GENERAL; FUNCTIONAL ELEMENTS OF SUCH SYSTEMS; MONITORING OR TESTING ARRANGEMENTS FOR SUCH SYSTEMS OR ELEMENTS
    • G05B19/00Programme-control systems
    • G05B19/02Programme-control systems electric
    • G05B19/418Total factory control, i.e. centrally controlling a plurality of machines, e.g. direct or distributed numerical control [DNC], flexible manufacturing systems [FMS], integrated manufacturing systems [IMS] or computer integrated manufacturing [CIM]
    • G05B19/41875Total factory control, i.e. centrally controlling a plurality of machines, e.g. direct or distributed numerical control [DNC], flexible manufacturing systems [FMS], integrated manufacturing systems [IMS] or computer integrated manufacturing [CIM] characterised by quality surveillance of production
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00Physical properties of inorganic compounds
    • C01P2006/80Compositional purity
    • 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
    • Y02P90/00Enabling technologies with a potential contribution to greenhouse gas [GHG] emissions mitigation
    • Y02P90/02Total factory control, e.g. smart factories, flexible manufacturing systems [FMS] or integrated manufacturing systems [IMS]

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  • Engineering & Computer Science (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • General Engineering & Computer Science (AREA)
  • Manufacturing & Machinery (AREA)
  • Quality & Reliability (AREA)
  • Physics & Mathematics (AREA)
  • General Physics & Mathematics (AREA)
  • Automation & Control Theory (AREA)
  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)

Abstract

The invention discloses a full-automatic hydrofluoric acid production system, which is characterized by comprising a tank truck, a raw material storage tank, a rectification system, an intermediate tank circulation cooling and absorption system, a tail discharge system, a PLC control system and the like. The whole production process of hydrofluoric acid is controlled by the PLC control system, wherein the rectification system comprises a preheating tower, two filtering towers arranged in a two-stage parallel manner, reaction stills and a rectifying tower; and the intermediate tank circulation cooling and absorption system comprises intermediate tanks, two-stage cooling towers, second filtering towers and a center control detection system. The full-automatic hydrofluoric acid production system adopts liquid anhydrous hydrogen fluoride for preparing hydrofluoric acid, the design is novel and reasonable, the production process is controlled by the PLC control system, the safety is high, the purity of the prepared hydrofluoric acid is high, and the practical value is high.

Description

Full-automatic Acid of Hydrofluoric Acid Production system
Technical field
The present invention relates to chemical mechanical equipment technical field, more particularly to a kind of full-automatic Acid of Hydrofluoric Acid Production system.
Background technology
Anhydrous hydrogen fluoride for industrial use is a kind of broad-spectrum chemical products, outward appearance is more than the 99% of colourless fuming liquidss Fluohydric acid., at low temperature for water white liquid, easily gasifies under decompression or high temperature, is mainly used as producing villiaumite, fluorine alkyl halide Hydrocarbon, fluorine refrigerant, etching glass, impregnated timber and electrolysis element fluorine etc..Anhydrous hydrogen fluoride is the extremely strong material of reactivity, can be with Various materials react, soluble in water, make Fluohydric acid..Highly purified Fluohydric acid. can as highly acid abluent, caustic, Can configure with nitric acid, glacial acetic acid, hydrogen peroxide and ammonium hydroxide etc. and use, be mainly used in integrated circuit(IC)With ultra-large collection Become circuit(VLSI)The cleaning of chip and corrosion, are one of key basic chemical industry materials in microelectronic industry manufacturing process, Its purity and cleanliness factor all play a very important role to the yield rate of integrated circuit, electrical property and reliability.Therefore hydrogen fluorine The security requirement of the preparation system of acid is extremely strict, prevents to personnel and environmental pollution, and requires prepared purer Fluohydric acid., need to design the production system that a kind of automatic control effect is good, security performance is high.
Content of the invention
For above-mentioned technical problem, the invention provides a kind of full-automatic Acid of Hydrofluoric Acid Production system, anhydrous using liquid Fluohydric acid gas prepares Fluohydric acid., and it is novel in design rationally, and production process is automatically controlled by PLC control system, high safety, preparation Fluohydric acid. purity is high, and practical value is high.
For realizing above-mentioned technical purpose, the technical solution used in the present invention is as follows:
A kind of full-automatic Acid of Hydrofluoric Acid Production system, using liquid phase anhydrous hydrogen fluoride produce Fluohydric acid. it is characterised in that:Including groove tank Car, raw material storage tank, standby raw material storage tank, distillation system, medial launder circulating cooling absorption system, tail heat-extraction system, finished pot, finished product Pump, filter and PLC control system, the whole production process of Fluohydric acid. by PLC control system control, wherein,
Described groove tank car is provided with water and rushes vacuum pump apparatus, and the in-car liquid phase anhydrous hydrogen fluoride of groove tank is unloaded by inert gas pressure Mode transfer to raw material storage tank, in the arm of unloading of groove tank car, to rush vacuum pump apparatus by water clear for the liquid phase anhydrous hydrogen fluoride of residual Wash;The outside of described raw material storage tank arranges a POP, with inert gas pressure for conveying power by liquid phase anhydrous hydrogen fluoride Enter distillation system through conveyance conduit;
Described distillation system includes pre-add thermal tower, some filtration tanks, reactor and rectifying column, and pre-add thermal tower is in preventing trace amount of steam mode Heating and gasifying is carried out to liquid phase anhydrous hydrogen fluoride, sends into filtration tank after gasification and carry out single filter, obtain relatively after single filter The liquid phase anhydrous hydrogen fluoride that pure gas phase fluorination hydrogen and part do not gasify enter in reactor, reactor added with deionized water and Strong oxidizer, such as potassium permanganate solution, and second heating is carried out by steam, after strong oxidizer is used for precipitating oxidation of impurities Discharge, deionized water is used for cleaning liquid phase anhydrous hydrogen fluoride, obtains more pure gas phase fluorination hydrogen after reacted kettle, complete the Rectification, is then fed into rectifying column and carries out second rectification;
If described medial launder circulating cooling absorption system includes medial launder dry cooling tower, the second filtration tank and middle control detection means, Medial launder is beaten by way of circulation the gas phase fluorination hydrogen after to rectification by deionized water and is absorbed, and gas phase fluorination hydrogen is dissolved in aquatic Become Fluohydric acid., heat is taken away by liberated heat by cooling tower, filters out the granule foreign in Fluohydric acid. in the second filtration tank;
Described raw material storage tank, distillation system and medial launder circulating cooling absorption system are equipped with tail heat-extraction system, and tail heat-extraction system includes Waste gas detector, go washing tail gas device and tail gas absorption groove, waste gas detector is used for having in detecting system leak free Gas or unabsorbed gas phase fluorination hydrogen, go washing tail gas device to remove the tail gas of leakage, tail row system in spray-absorption mode System will not absorb completely hydrogen fluoride gas and suck tail gas absorption groove, and after absorbing saturation, middle control detection means carries out middle control detection, Through in control detection qualified after, the Fluohydric acid. in medial launder is squeezed into finished pot, the Fluohydric acid. in finished pot is through discharge pump and filtration Carry out subpackage after device.
Preferably, described water rushes vacuum pump apparatus is provided with absorbing liquid concentration detection apparatus, true for the punching of periodic detection water Absorbing liquid concentration in empty pump.
Preferably, described filtration tank is built with tetrafluoro filler.
Preferably, described filtration tank is arranged with twin-stage parallel way.
This Fluohydric acid. system is produced by PLC control, and technological process is divided into four parts:Groove tank car is to head tank, former Batch can, to distillation system, arrives intercooling and absorbs after rectification, the middle control qualified rear medial launder of detection to finished pot, and whole process can be led to Cross PLC screen to be operated it is also possible to be switched to manual operation, with noble gases for conveying power, be designed with tail row system simultaneously System, can effectively play decompression protection and Environmental security effect, in process of production, gas phase fluorination hydrogen absorbs through three times, protects Demonstrate,prove absorption efficiency, prepared Fluohydric acid. purity is higher, and production process automatic control effect is good, high safety.
Due to employing technique scheme, the present invention has the following technical effect that:The present invention adopts the anhydrous fluorine of liquid Change hydrogen and prepare Fluohydric acid., it is novel in design rationally, and production process is automatically controlled by PLC control system, high safety, the hydrogen of preparation Fluoric acid purity is high, and practical value is high.
Brief description
Examples of the present invention will be described by way of reference to the accompanying drawings, wherein:
Fig. 1 is the structural representation of the present invention.
Specific embodiment
All features disclosed in this specification, or disclosed all methods or during step, except mutually exclusive Feature and/or step beyond, all can combine by any way.
Any feature disclosed in this specification, unless specifically stated otherwise, all can be equivalent or there is similar purpose by other Alternative features are replaced.I.e., unless specifically stated otherwise, each feature is a series of equivalent or one of similar characteristics example ?.
A kind of full-automatic Acid of Hydrofluoric Acid Production system as shown in Figure 1, produces Fluohydric acid. using liquid phase anhydrous hydrogen fluoride, including Groove tank car 1, raw material storage tank 2, standby raw material storage tank 3, distillation system 4, medial launder circulating cooling absorption system 5, tail heat-extraction system 6, Finished pot 7, discharge pump 8 and PLC control system, the whole production process of Fluohydric acid. is by PLC control system control it is also possible to switch To manual operation, wherein, groove tank car 1 is provided with water and rushes vacuum pump apparatus 11, and the liquid phase anhydrous hydrogen fluoride in groove tank car 1 passes through inertia The mode of gas pressure unloading transfers to raw material storage tank 2, controls the pressure of groove tank car to be unloaded in 0.1MPa, multiple valve every Disconnected, in the arm of unloading of groove tank car 1, the liquid phase anhydrous hydrogen fluoride of residual rushes the cleaning of vacuum pump 11 device by water.Water rushes vacuum pump dress Put 11 and be provided with absorbing liquid concentration detection apparatus, rush the absorbing liquid concentration in vacuum pump 11 for periodic detection water, and changed, Absorbing liquid can be recycled as industrial stage hydrofluoric acid, and it is anhydrous that water rushes the liquid phase that vacuum pump apparatus 11 can solve the problem that in pipeline The problem that fluohydric acid gas difficulty clears, reduces the injury to people.The outside of raw material storage tank 2 arranges a POP, with noble gases pressure Power is that liquid phase anhydrous hydrogen fluoride is entered distillation system 4 through conveyance conduit by conveying power, and noble gases preferably employ nitrogen, raw material Storage tank 2 is totally enclosed type.Technical grade 99% liquid phase anhydrous hydrogen fluoride is adopted as raw material, the input and output material of raw material storage tank 2 in the present invention Can be controlled by two electromagnetic valves, signal is provided by PLC control system, raw material storage tank 2 can adopt horizontal type structure, all of method Blue mouth is all disposed within the upper end of bedroom storage tank, can effective prevent leakage, magnetic turnover panel liquid level is all installed in the both sides of raw material storage tank 2 Meter, can monitor in real time liquid level, high level and low liquid level are processed accordingly.
As shown in figure 1, distillation system 4 includes pre-add thermal tower 41, with two filtration tanks 42 of twin-stage parallel way setting, anti- Answer kettle 43 and rectifying column 44, pre-add thermal tower 41 carries out heating and gasifying, rectification temperature in preventing trace amount of steam mode to liquid phase anhydrous hydrogen fluoride Degree controls at 30 DEG C about, sends into filtration tank 42 and carries out single filter, filtration tank is built with tetrafluoro filler, single filter after gasification The purer gas phase fluorination hydrogen obtaining afterwards and the liquid phase anhydrous hydrogen fluoride partly not gasified enter reactor 43, in reactor 43 Added with deionized water and strong oxidizer, such as potassium permanganate solution etc., and second heating is carried out by steam, will above preheat Completely liquid phase anhydrous hydrogen fluoride is not gasified for gasification, and strong oxidizer is periodically discharged after being used for precipitating oxidation of impurities, special It is not the trivalent arsenic in Fluohydric acid., deionized water is used for cleaning liquid phase anhydrous hydrogen fluoride, obtains more pure after reacted kettle 43 Gas phase fluorination hydrogen, complete first time rectification, be then fed into rectifying column 44 and carry out second rectification.
As shown in figure 1, in the present invention, medial launder circulating cooling absorption system 5 include medial launder 51, two grade cooling towers 52, Second filtration tank 53 and middle control detection means, medial launder 51 beats by way of circulation the gas phase fluorination after to rectification by deionized water Hydrogen is absorbed the efficiency it is ensured that being absorbed.Gas phase fluorination hydrogen is dissolved in water generating Fluohydric acid., and liberated heat passes through two grade cooling towers Heat is taken away by 52, filters out the granule foreign in Fluohydric acid., can be filled with superfinishing in the second filtration tank 53 in the second filtration tank 53 Thin 0.1 μm of tetrafluoro filtering material.
In the present invention, raw material storage tank 2, distillation system 4 and medial launder circulating cooling absorption system 5 are equipped with tail heat-extraction system 6, Tail heat-extraction system 6 includes waste gas detector, goes washing tail gas device 61 and tail gas absorption groove 62, and waste gas detector is used for detecting There are leak free gas or unabsorbed gas phase fluorination hydrogen in system, go washing tail gas device 61 to remove in spray-absorption mode The tail gas of leakage.Reactor 43 also is provided with tail row's design, when the pressure in reactor 43 is excessive, pressure release can be carried out guarantee be System safety.Tail heat-extraction system 6 will not absorb completely hydrogen fluoride gas and suck tail gas absorption groove 62, after absorbing saturation, middle control detection Device carry out middle control detection, through in control detect qualified after, the Fluohydric acid. in medial launder 51 is squeezed into finished pot, the hydrogen in finished pot Fluoric acid carries out subpackage after discharge pump 8 and filter 9, and Fluohydric acid. finished product need to be passed through filter and be filtered again, obtain ultra-clean High-pure hydrofluoric acid finished product.
Tail heat-extraction system design in the present invention, automatization's effect is good, can farthest reduce to personnel and environment Injury.
This Fluohydric acid. system is produced by PLC control, and technological process is divided into four parts:Groove tank car is to head tank, former Batch can, to distillation system, arrives intercooling and absorbs after rectification, the middle control qualified rear medial launder of detection to finished pot, and whole process can be led to Cross PLC screen to be operated it is also possible to be switched to manual operation, with noble gases for conveying power, be designed with tail row system simultaneously System, can effectively play decompression protection and Environmental security effect, in process of production, gas phase fluorination hydrogen absorbs through three times, protects Demonstrate,prove absorption efficiency, prepared Fluohydric acid. purity is higher, and production process automatic control effect is good, high safety.
The invention is not limited in aforesaid specific embodiment.The present invention expands to and any discloses in this manual New feature or any new combination, and the arbitrary new method of disclosure or the step of process or any new combination.

Claims (4)

1. a kind of full-automatic Acid of Hydrofluoric Acid Production system, using liquid phase anhydrous hydrogen fluoride produce Fluohydric acid. it is characterised in that:Including groove Tank car, raw material storage tank, standby raw material storage tank, distillation system, medial launder circulating cooling absorption system, tail heat-extraction system, finished pot, one-tenth Product pump, filter and PLC control system, the whole production process of Fluohydric acid. by PLC control system control, wherein,
Described groove tank car is provided with water and rushes vacuum pump apparatus, and the in-car liquid phase anhydrous hydrogen fluoride of groove tank is unloaded by inert gas pressure Mode transfer to raw material storage tank, in the arm of unloading of groove tank car, to rush vacuum pump apparatus by water clear for the liquid phase anhydrous hydrogen fluoride of residual Wash;The outside of described raw material storage tank arranges a POP, with inert gas pressure for conveying power by liquid phase anhydrous hydrogen fluoride Enter distillation system through conveyance conduit;
Described distillation system includes pre-add thermal tower, some filtration tanks, reactor and rectifying column, and pre-add thermal tower is in preventing trace amount of steam mode Heating and gasifying is carried out to liquid phase anhydrous hydrogen fluoride, sends into filtration tank after gasification and carry out single filter, obtain relatively after single filter The liquid phase anhydrous hydrogen fluoride that pure gas phase fluorination hydrogen and part do not gasify enter in reactor, reactor added with deionized water and Strong oxidizer, and second heating is carried out by steam, strong oxidizer is discharged after being used for precipitating oxidation of impurities, and deionized water is used In cleaning liquid phase anhydrous hydrogen fluoride, obtain more pure gas phase fluorination hydrogen after reacted kettle, complete first time rectification, then send Enter rectifying column and carry out second rectification;
If described medial launder circulating cooling absorption system includes medial launder dry cooling tower, the second filtration tank and middle control detection means, Medial launder is beaten by way of circulation the gas phase fluorination hydrogen after to rectification by deionized water and is absorbed, and gas phase fluorination hydrogen is dissolved in aquatic Become Fluohydric acid., heat is taken away by liberated heat by cooling tower, filters out the granule foreign in Fluohydric acid. in the second filtration tank;
Described raw material storage tank, distillation system and medial launder circulating cooling absorption system are equipped with tail heat-extraction system, and tail heat-extraction system includes Waste gas detector, go washing tail gas device and tail gas absorption groove, waste gas detector is used for having in detecting system leak free Gas or unabsorbed gas phase fluorination hydrogen, go washing tail gas device to remove the tail gas of leakage, tail row system in spray-absorption mode System will not absorb completely hydrogen fluoride gas and suck tail gas absorption groove, and after absorbing saturation, middle control detection means carries out middle control detection, Through in control detection qualified after, the Fluohydric acid. in medial launder is squeezed into finished pot, the Fluohydric acid. in finished pot is through discharge pump and filtration Carry out subpackage after device.
2. a kind of full-automatic Acid of Hydrofluoric Acid Production system according to claim 1 it is characterised in that:Described water rushes vacuum pump dress Install absorbing liquid concentration detection apparatus, rush the absorbing liquid concentration in vacuum pump for periodic detection water.
3. a kind of full-automatic Acid of Hydrofluoric Acid Production system according to claim 1 it is characterised in that:Described filtration tank built with Tetrafluoro filler.
4. a kind of full-automatic Acid of Hydrofluoric Acid Production system according to claim 1 it is characterised in that:Described filtration tank is with twin-stage Parallel way is arranged.
CN201610842387.4A 2016-09-23 2016-09-23 Full-automatic Acid of Hydrofluoric Acid Production system Active CN106406256B (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111892023A (en) * 2020-07-30 2020-11-06 甘元松 Anti-channeling hydrogen fluoride reacting furnace

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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

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