CN204588694U - A kind of production system of used in electronic industry hydrofluoric acid - Google Patents

A kind of production system of used in electronic industry hydrofluoric acid Download PDF

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Publication number
CN204588694U
CN204588694U CN201520245539.3U CN201520245539U CN204588694U CN 204588694 U CN204588694 U CN 204588694U CN 201520245539 U CN201520245539 U CN 201520245539U CN 204588694 U CN204588694 U CN 204588694U
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China
Prior art keywords
retort
tank
hydrofluoric acid
absorption liquid
production system
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Expired - Fee Related
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CN201520245539.3U
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Chinese (zh)
Inventor
夏杰
刘雪江
沙其勇
贾云
张赟
董元峰
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Nanjing Kai Yan Chemical Co Ltd
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Nanjing Kai Yan Chemical Co Ltd
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Abstract

The utility model relates to a kind of production system of used in electronic industry hydrofluoric acid, comprise anhydrous hydrogen fluoride pretreatment unit, retort, cold-hot water circulation device, spray-absorption liquid circulating device and multiple pan tank, anhydrous hydrogen fluoride pretreatment unit comprises raw material storage bottle and heating bucket, raw material storage bottle is arranged in heating bucket, raw material storage bottle is connected with a surge tank, surge tank is connected with retort, and retort inside is provided with heat exchange coil and ventpipe, is provided with microporous membrane filters bottom retort; Cold-hot water circulation device comprises water tank and the circulation vacuum primingpump of band having heaters; Spray-absorption liquid circulating device comprises absorption liquid storage tank and recycle pump, and absorption liquid storage tank is connected with retort on the one hand, is connected to the spray header of retort on the other hand, is connected in addition with pan tank by recycle pump.This production system is easily implemented, easy to operate, and production cost is low, and prepared product has multiple concentration, and output is high, meets environmental requirement.

Description

A kind of production system of used in electronic industry hydrofluoric acid
Technical field
The utility model relates to Acid of Hydrofluoric Acid Production field, specifically a kind of production system of used in electronic industry hydrofluoric acid.
Background technology
The purposes of hydrofluoric acid is very extensive, hydrofluoric acid can produce fluorine refrigerant, fluoropolymer, fluorine-containing medicines as the important source material of fluorine chemistry industry, the aluminum fluoride produced with its and sodium aluminum fluoride are the requisite auxiliary agents of aluminum smelting industry, the Stainless Steel Cleaner of it or the alkylation catalyst of refinery, Steel Plant.The industries such as food protection, specialty metal smelting, leather and textile treatment, Saving specimen and nuclear industry are widely used in addition with the fluoride salt of Acid of Hydrofluoric Acid Production.Used in electronic industry hydrofluoric acid is high-pure hydrofluoric acid, as strongly-acid cleaning, etching reagent, can configure with nitric acid, hydrogen peroxide, Glacial acetic acid etc. and use, being mainly used in cleaning and the corrosion of unicircuit and VLSI (very large scale integrated circuit) chip, is one of key basic chemical industry material in microelectronic industry making processes.
Hydrofluoric acid is the aqueous solution of hydrogen fluoride gas, and molecular formula is HF-H 2o, for water white transparency is to faint yellow fuming liquid.The common method preparing high-pure hydrofluoric acid at present is both at home and abroad by industrial anhydrous hydrofluoric acid (its high purity 99.95% or higher, but wherein containing the anions and canons impurity that silicon, phosphorus, nitrogen, chlorine, sulphur, arsenic, boron and metallic element etc. are formed) carry out oxidation and rectifying removal of impurities further, main purification techniques has the technology such as rectifying, distillation, sub-boiling distillation, gas absorption, these purification techniquess respectively have characteristic, have his own strong points.Some purification techniquess such as sub-boiling distillation technology can only for the preparation of the few product of amount, and some purification techniquess such as gas absorption techniques may be used for large-scale production.That the tower top of rectifying tower is provided with overhead condenser in the production equipment of current high-pure hydrofluoric acid, rectifying tower gas out condensation separation in overhead condenser, then hydrofluoric acid condensation in overhead condenser that liquefaction temperature is higher is back in rectifying tower, and the impurity that liquefaction temperature is lower is still then that gaseous state directly removes from overhead condenser top discharge.But when finding to adopt which to carry out condensation for gas out in hydrofluoric acid rectifying tower by research, gas is easy to be excessively cold, the impurity making liquefaction temperature lower is also liquefied as liquid, such partial impurities also can condensing reflux in rectifying tower, affect the quality of product, the purity of obtained product is lower.
Summary of the invention
The utility model, just for the technical problem existed in prior art, provides a kind of production system of used in electronic industry hydrofluoric acid, and this production system one-piece construction is simple, easy to operate, production cost is low, and prepared product has multiple concentration, output is high, meets environmental requirement.
To achieve these goals, the technical solution adopted in the utility model is, a kind of production system of used in electronic industry hydrofluoric acid, comprise anhydrous hydrogen fluoride pretreatment unit, retort, cold-hot water circulation device, spray-absorption liquid circulating device and multiple pan tank, described anhydrous hydrogen fluoride pretreatment unit comprises raw material storage bottle and heating bucket, described raw material storage bottle is arranged in heating bucket, the discharge hole of described raw material storage bottle is connected by the opening for feed of pipeline with a surge tank, the discharge hole of described surge tank is connected with the raw material inlet hole of retort by pipeline, described retort inside is provided with heat exchange coil and ventpipe, described retort top is provided with oxidizing reaction additive filling tube, discharge hole place bottom described retort is provided with microporous membrane filters, described microporous membrane filters is connected with pan tank by pipeline, described cold-hot water circulation device comprises water tank, well heater and circulation vacuum primingpump, described well heater adopts the form of chuck to be arranged on the outer wall of described water tank, described water tank is connected with the heat exchange coil water-in in described retort by circulation vacuum primingpump, and described heat exchange coil water outlet is connected directly to water tank by pipeline, described spray-absorption liquid circulating device comprises absorption liquid storage tank and recycle pump, described absorption liquid storage tank is connected by the discharge nozzle of pipeline with described retort on the one hand, the spray header of inside, retort top is connected on the other hand by recycle pump, be connected with described pan tank in addition, pan tank is connected with recycle pump by pipeline, the ingenious practicality of whole Technical Design, production technique is simple, and it is available that the high and obtained hydrofluoric acid of output has multiple concentration.
Improve as one of the present utility model, described retort and pan tank adopt carbon steel lining teflon material to make, due to the severe corrosive of hydrofluoric acid, and corrosion can be more serious when technological temperature is higher, therefore this material preparation feedback tank of material and pan tank can strengthen their erosion resistance, thus increase the service life.
Improve as one of the present utility model, the spray-absorption liquid that the circulation device of described spray-absorption liquid exports is the deionized water that resistivity is not less than 17M Ω .cm, and belong to electronic grade high-purity water, purity is high, free from foreign meter, can not cause secondary pollution to system.
Improve as one of the present utility model, described microporous membrane filters adopts stainless material to make, and its aperture is 0.05 micron, and the volume of this microporous membrane filters is little, aperture is homogeneous, filtering velocity is fast and adsorptive capacity is few.
Improve as one of the present utility model, stainless steel magnetic drive pump selected by described recycle pump, adopts magnetic coupling to transmit power, complete No leakage, is applicable to conveying not containing solid particle erosion liquid, strong acid-base solution etc.
Improve as one of the present utility model, described anhydrous hydrogen fluoride pretreatment unit, retort and pan tank are provided with the detection of hydrofluoric acid concentration of toxic gases and central alarm unit, for whether having poisonous gas in the whole production process of Real-Time Monitoring leak, thus ensure the personnel safety of operator.
Improve as one of the present utility model, described retort is provided with temperature sensor and exhaust collection pipe, and described exhaust collection Guan Yuyi tail gas absorber is connected, and the tail gas that system response produces can qualified discharge after tail gas absorber process.
Relative to prior art, production cost of the present utility model is low, easy to implement, can realize continous way scale operation, simple to operation, and supporting automatic control system, realize serialization and automatically produce, efficiency is high, output is high and safety and environmental protection; Whole production unit adopts and flows vertically to layout, and raw material can rely on self gravitation to flow from top to bottom, and the reactor of preparing product is located at middle part, the filtration of product, is fillingly located at bottom, thus can reduce pump delivery, saves energy consumption, reduces production cost.
Accompanying drawing explanation
Fig. 1 is structural representation of the present utility model.
Fig. 2 is production technological process of the present utility model.
In figure: 1-raw material storage bottle, 2-heats bucket, 3-platform scale, 4-surge tank, 5-ventpipe, 6-retort, 7-heat exchange coil, 8-oxidizing reaction additive filling tube, 9-spray header, 10-plastic tank, 11-water tank, 12-well heater, 13-circulation vacuum primingpump, 14-pan tank, 15-recycle pump, 16-absorption liquid storage tank, 17-concentration of toxic gases surveymeter, 18-tail gas absorber, 19-microporous membrane filters.
Embodiment
In order to deepen understanding and cognition of the present utility model, below in conjunction with accompanying drawing the utility model be further described and introduce.
As shown in Fig. 1-Fig. 2, a kind of production system of used in electronic industry hydrofluoric acid, comprises anhydrous hydrogen fluoride pretreatment unit, retort, cold-hot water circulation device, spray-absorption liquid circulating device and three pan tanks.The raw material storage bottle 1 that employing carbon steel in described anhydrous hydrogen fluoride pretreatment unit is made is arranged in heating bucket 2, and is provided with a platform scale 3 in the bottom of heating bucket, for the weight of anhydrous hydrogen fluoride in real time measure storage bottle.Vaporization is there is and forms hydrogen fluoride gas in the anhydrous hydrogen fluoride be stored in raw material storage bottle 1 after the hot water heating in heating bucket 2.The discharge hole of described surge tank 4 is connected with the raw material inlet hole of retort 6 by pipeline, a polytetrafluoroethylplastic plastic bucket 10 is connected with in the bottom of described surge tank, for receiving the liquefied hy-drogen fluoride in surge tank, described retort 6 inside is provided with heat exchange coil 7 and ventpipe 5, described ventpipe 5 is arranged on raw material inlet hole place, described retort 6 top is provided with oxidizing reaction additive (adopting fluorine gas in the present embodiment) filling tube 8, discharge hole place bottom described retort 6 is provided with microporous membrane filters 19, and described microporous membrane filters 19 is connected with pan tank 14 by pipeline.Described cold-hot water circulation device comprises water tank 11, well heater 12 and circulation vacuum primingpump 13, described well heater adopts jacketed type well heater and is trapped among on the outer wall of described water tank, described water tank 11 is connected with heat exchange coil 7 water-in in described retort 6 by circulation vacuum primingpump 13, and described heat exchange coil 7 water outlet is connected directly to water tank 11 by pipeline.Described spray-absorption liquid circulating device comprises absorption liquid storage tank 16 and recycle pump 15, described absorption liquid storage tank 16 1 aspect is connected by the discharge nozzle of pipeline with described retort 6, the spray header 9 of inside, retort 6 top is connected on the other hand by recycle pump 15, be connected with described pan tank 14 in addition, pan tank 14 is connected with recycle pump 15 by pipeline.In whole production system, the pressure of equipment is normal pressure, and security is high.
Preferably, the limit of described anhydrous hydrogen fluoride pretreatment unit, retort 6 and pan tank 14 is provided with hydrofluoric acid concentration of toxic gases surveymeter 17 and coupled central alarm unit, for monitoring the security of production system in real time.
Preferably, described retort 6 and pan tank 14 adopt corrosion resistant carbon steel lining teflon material to make, and in retort 6, being provided with temperature sensor and exhaust collection pipe, described exhaust collection Guan Yuyi tail gas absorber 18 is connected, the waste gas qualified discharge after treatment of generation.
Preferably, the spray-absorption liquid that the circulation device of described spray-absorption liquid exports adopts resistivity to be not less than the deionized water of 17M Ω .cm, and purity is high, can not cause secondary pollution to the hydrofluoric acid produced.
Preferably, described microporous membrane filters 19 adopts stainless material to make, and the aperture of its filtering membrane is 0.05 micron, and the volume of this microporous membrane filters is little, thus is easy to lay, and the aperture ratio of filtering membrane is comparatively even, and not only filtering velocity is fast but also few to the adsorptive capacity of filtrate.
Preferably, stainless steel magnetic drive pump selected by described recycle pump 15, and adopt magnetic coupling to transmit power, powerful, and the complete Full-sealed no-leakage of structure, further increase the security of production process.
As shown in Figure 2, vaporization is there is and forms hydrogen fluoride gas in the anhydrous hydrogen fluoride in raw material storage bottle after the hot water heating in heating bucket, this gas is by carrying out buffer in Cemented filling to surge tank, and gas flows in retort through ventpipe from surge tank, in retort, add fluorine gas simultaneously, oxidizing reaction is there is after hydrogen fluoride gas and fluorine gas, by the heat exchange coil established in cold-hot water circulation device and retort, the temperature in tank is maintained 0 ~ 20 DEG C of for some time, thus remove a part of non-volatility impurity by oxidizing reaction; And then the temperature in retort raised and temperature maintained 50 ~ 80 DEG C of for some time, removing volatile impunty; Then the hydrofluoric acid spraying high density by spray header in retort washs, and again removes impurity wherein.Make the used in electronic industry hydrofluoric acid of 30%, 40%, 50% and 55% concentration finally by deionized water absorption and be stored in pan tank.
It should be noted that above-described embodiment, be not used for limiting protection domain of the present utility model, equivalents done on the basis of technique scheme or the alternative scope all falling into the utility model claim and protect.In the claims, word " comprises " and does not get rid of existence and do not arrange parts in the claims.

Claims (7)

1. the production system of a used in electronic industry hydrofluoric acid, it is characterized in that: comprise anhydrous hydrogen fluoride pretreatment unit, retort, cold-hot water circulation device, spray-absorption liquid circulating device and multiple pan tank, described anhydrous hydrogen fluoride pretreatment unit comprises raw material storage bottle and heating bucket, described raw material storage bottle is arranged in heating bucket, the discharge hole of described raw material storage bottle is connected by the opening for feed of pipeline with a surge tank, the discharge hole of described surge tank is connected with the raw material inlet hole of retort by pipeline, described retort inside is provided with heat exchange coil and ventpipe, described retort top is provided with oxidizing reaction additive filling tube, discharge hole place bottom described retort is provided with microporous membrane filters, described microporous membrane filters is connected with pan tank by pipeline, described cold-hot water circulation device comprises water tank, well heater and circulation vacuum primingpump, described well heater adopts the form of chuck to be arranged on the outer wall of described water tank, described water tank is connected with the heat exchange coil water-in in described retort by circulation vacuum primingpump, and described heat exchange coil water outlet is connected directly to water tank by pipeline, described spray-absorption liquid circulating device comprises absorption liquid storage tank and recycle pump, described absorption liquid storage tank is connected by the discharge nozzle of pipeline with described retort on the one hand, the spray header of inside, retort top is connected on the other hand by recycle pump, be connected with described pan tank in addition, pan tank is connected with recycle pump by pipeline.
2. the production system of a kind of used in electronic industry hydrofluoric acid as claimed in claim 1, is characterized in that, described anhydrous hydrogen fluoride pretreatment unit, retort and pan tank are provided with the detection of hydrofluoric acid concentration of toxic gases and central alarm unit.
3. the production system of a kind of used in electronic industry hydrofluoric acid as claimed in claim 1 or 2, is characterized in that, described retort and pan tank adopt carbon steel lining teflon material to make.
4. the production system of a kind of used in electronic industry hydrofluoric acid as claimed in claim 1, is characterized in that, the spray-absorption liquid that the circulation device of described spray-absorption liquid exports is the deionized water that resistivity is not less than 17M Ω .cm.
5. the production system of a kind of used in electronic industry hydrofluoric acid as claimed in claim 1, is characterized in that, described microporous membrane filters adopts stainless material to make, and its aperture is 0.05 micron.
6. the production system of a kind of used in electronic industry hydrofluoric acid as claimed in claim 3, is characterized in that, described retort is provided with temperature sensor and exhaust collection pipe, and described exhaust collection Guan Yuyi tail gas absorber is connected.
7. the production system of a kind of used in electronic industry hydrofluoric acid as claimed in claim 1, it is characterized in that, stainless steel magnetic drive pump selected by described recycle pump.
CN201520245539.3U 2015-04-22 2015-04-22 A kind of production system of used in electronic industry hydrofluoric acid Expired - Fee Related CN204588694U (en)

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105921090A (en) * 2016-06-02 2016-09-07 赵正芳 Reaction kettle
CN106406256A (en) * 2016-09-23 2017-02-15 江苏中德电子材料科技有限公司 Full-automatic hydrofluoric acid production system
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
TWI717295B (en) * 2020-06-24 2021-01-21 陳義平 Electronic grade hydrofluoric acid manufacturing system and method for manufacturing electronic grade hydrofluoric acid using the system
CN112279225A (en) * 2020-11-16 2021-01-29 河南骏化发展股份有限公司 Production system and process for co-production of industrial-grade nitric acid and electronic-grade nitric acid

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105921090A (en) * 2016-06-02 2016-09-07 赵正芳 Reaction kettle
CN106406256A (en) * 2016-09-23 2017-02-15 江苏中德电子材料科技有限公司 Full-automatic hydrofluoric acid production system
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
TWI717295B (en) * 2020-06-24 2021-01-21 陳義平 Electronic grade hydrofluoric acid manufacturing system and method for manufacturing electronic grade hydrofluoric acid using the system
CN112279225A (en) * 2020-11-16 2021-01-29 河南骏化发展股份有限公司 Production system and process for co-production of industrial-grade nitric acid and electronic-grade nitric acid

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Granted publication date: 20150826

Termination date: 20160422