CN109200765B - Preparation electronic level hydrogen fluoride washing absorbing device - Google Patents

Preparation electronic level hydrogen fluoride washing absorbing device Download PDF

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Publication number
CN109200765B
CN109200765B CN201811207316.2A CN201811207316A CN109200765B CN 109200765 B CN109200765 B CN 109200765B CN 201811207316 A CN201811207316 A CN 201811207316A CN 109200765 B CN109200765 B CN 109200765B
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tail gas
liquid
tower
storage tank
hydrofluoric acid
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CN109200765A (en
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杨松
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Sanlifu New Materials (Fujian) Co.,Ltd.
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Xie Mulan
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/14—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by absorption
    • B01D53/18—Absorbing units; Liquid distributors therefor
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/002—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by condensation
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/14—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by absorption
    • B01D53/1412—Controlling the absorption process
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/14—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by absorption
    • B01D53/1456—Removing acid components
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2252/00—Absorbents, i.e. solvents and liquid materials for gas absorption
    • B01D2252/10—Inorganic absorbents
    • B01D2252/103—Water

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Analytical Chemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Treating Waste Gases (AREA)
  • Gas Separation By Absorption (AREA)

Abstract

The invention relates to the technical field of fluorine chemical industry, in particular to a washing and absorbing device for preparing electronic-grade hydrogen fluoride. The method is characterized in that: comprises a washing absorption tower, a circulating storage tank, a circulating pump assembly and a condensing tower. The bottoms of the washing absorption tower and the condensing tower are communicated with the circulating storage tank to form a U-shaped communicating vessel.

Description

Preparation electronic level hydrogen fluoride washing absorbing device
Technical Field
The invention relates to the technical field of fluorine chemical industry, in particular to a washing and absorbing device for preparing electronic-grade hydrogen fluoride.
Background
Electronic grade hydrogen fluoride is mainly used as a cleaning agent and an etching agent in the industries of photovoltaics, integrated circuits and the like, is one of key auxiliary materials in the industries, and because arsenic impurity has a serious influence on the performance of electronic devices, the removal of arsenic is a key technology for purifying hydrogen fluoride. The Chinese invention patent (with the patent number of CN201110276860.4, the patent name is a method for preparing electronic-grade hydrofluoric acid) discloses a method for preparing electronic-grade hydrofluoric acid, which comprises the following steps: (1) gasification of technical grade anhydrous HF feedstock: gasifying industrial HF at 35 deg.c; (2) fluorine gas oxidation and light component removal, wherein gasified HF and fluorine gas are continuously introduced into a fluorine gas oxidation reactor, the fluorine gas oxidation reactor is provided with a cooling heat exchanger for adjusting the temperature of reaction materials and an absorption tower internally provided with fillers, HF is continuously injected into the top of the absorption tower through a circulating pump, and the unreacted fluorine gas is in countercurrent contact with circulating HF flowing down from the absorption tower; the dosage of fluorine gas is 1-2g/kgHF, the temperature of the oxidation reaction of the fluorine gas is controlled at 0-20 ℃, the pressure of the equipment is normal pressure, and the circulating amount of the pump is 10 times of the mass of the feed HF; (3) HF after the high-boiling rectification is oxidized at the upper part and light components are removed enters a high-boiling rectification tower, the temperature of the HF at the top of the high-boiling rectification tower is controlled at 20 ℃, and the reflux ratio of the high-boiling rectification tower is 1-3; (4) HF and fresh electronic-grade high-purity water which are subjected to high-boiling rectification in water washing rectification are respectively injected into a tower kettle of a water washing rectification tower, the water washing rectification tower is divided into two sections, the lower section is a washing section, and the upper section is a rectification section; in the washing section, under the action of a tower kettle heater, hydrofluoric acid is gasified, refluxed hydrofluoric acid and newly added high-purity water are uniformly distributed on a filler through a liquid distributor and are in countercurrent contact with hydrofluoric acid steam rising from a tower kettle to wash impurities in HF, the concentration of liquid led out from the tower kettle is controlled to be 70-80%, and the temperature of liquid in a constant-temperature reboiler at the bottom of a water-washing rectifying tower is 48-65 ℃; the washed hydrofluoric acid enters a rectifying section, is rectified and purified and then enters a tower top condenser, after condensation, partial reflux is carried out, the reflux ratio is controlled to be 2-4, the operating pressure of the tower is 110kPa, and a product extracted from the tower top is anhydrous HF meeting the quality requirement of an electronic grade product; wherein: the anhydrous HF is absorbed by water to prepare electronic grade hydrofluoric acid products with various concentrations. The Chinese invention patent (with the patent number of CN201310052553.7, the patent name is a preparation method of electronic-grade hydrofluoric acid) discloses a preparation method of electronic-grade hydrofluoric acid, which is characterized in that industrial anhydrous hydrogen fluoride liquid and pure water are introduced into a rectifying tower to form hydrofluoric acid with a first concentration; then adding hydrogen peroxide solution to oxidize arsenic and silicon impurities in the solution, and then rectifying the solution; condensing the hydrogen fluoride gas obtained by rectification into hydrogen fluoride liquid, carrying out first filtration, absorbing the hydrogen fluoride liquid into hydrofluoric acid with a second concentration by using pure water, and carrying out second filtration to obtain an electronic grade hydrofluoric acid product; absorbing the tail gas with pure water to prepare industrial hydrofluoric acid. The preparation method has the advantages of simple preparation process, no introduction of extra impurities, high yield and low cost, and the prepared electronic-grade hydrofluoric acid reaches the semiconductor equipment and material international standard SEMI-C7, and can be used for preparing both electronic-grade hydrofluoric acid and analytically pure hydrofluoric acid by one production process.
Prior art 1 uses fluorine gas as oxidant to oxidize impurities in hydrogen fluoride, and uses washing rectification method to respectively remove high-boiling-point substances such as HAsF6、MAsF6、H2SO4、H2O、H2SiF6、H3PO4Iso and volatile component SO2、SiF4、PF3、POF3、AsF5、SF6、PF5The problems to be solved are that firstly, fluorine gas has high toxicity, high chemical activity and strong oxidizing property, the existing conveying machinery such as a circulating pump is difficult to solve the sealing problem, and serious safety accidents are easy to occur when leakage occurs; secondly, rectification and washing are integrated in a rectifying tower to finish the process which does not meet the technical specifications; prior art 2 teaches that arsenic, an impurity in hydrogen fluoride, has a severe impact on the performance of electronic devices, arsenic removal is a key technology for hydrogen fluoride purification, and the prior art generally employs a method of oxidizing trivalent arsenic to trivalent arsenic using an oxidizing agentHigh boiling point pentavalent arsenic compound, reuse the technological method of distillation to remove it, oxidizing agent usually choose potassium permanganate, hydrogen peroxide, potassium dichromate, etc., the problem still to be solved has, first, introduce other impurity to increase difficulty and cost of subsequent treatment; secondly, the oxidation time is long, generally reaching 6 to 48 hours, and the energy consumption is high.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a washing and absorbing device for preparing electronic grade hydrogen fluoride, which is characterized in that: the device comprises a washing absorption tower, a circulating storage tank, a circulating pump assembly and a condensing tower, wherein the bottoms of the washing absorption tower and the condensing tower are communicated with the circulating storage tank to form a U-shaped communicating vessel.
The washing absorption tower comprises a liquid collecting pipe, a washing absorption tower body, an air inlet guide pipe, a filler, a liquid distribution grid plate, a spraying pipe fitting and an exhaust guide pipe, and the condensing tower comprises a tail gas inlet, a condensing tower body, a condensing pipe plate, a liquid removing device, a tail gas discharge port and a condensate outlet.
The tail gas finishes the condensation process through an air inlet guide pipe, a filler, a liquid distribution grid plate, a spraying pipe fitting, an exhaust guide pipe, a tail gas inlet, a condensation pipe plate, a liquid removing device and a tail gas discharge port in sequence, condensed hydrofluoric acid condensate is separated from gas and collected into a circulating storage tank through a liquid collecting pipe and a condensate outlet, and the circulating pump assembly returns the hydrofluoric acid condensate in the circulating storage tank to the spraying pipe fitting to wash and condense the tail gas.
The tail gas import and the condensation tower body of condensing tower adopt venturi principle design, and the purpose makes tail gas get into the great condensation tower body diffusion of diameter behind the less tail gas import compression of diameter, makes the liquid drop evenly distributed in tail gas to improve the condensation efficiency at the condensation tube sheet.
The inventor finds that international standard SEMI-C7 for ultra-clean high-purity reagent of international semiconductor equipment and materials organization requires less than 10ppb of metal impurities, and arsenic is a doping element for semiconductor manufacture, so that the requirement on the content of arsenic impurities in hydrofluoric acid standard is particularly strict. In the prior method for removing arsenic, an oxidant is usually adopted to oxidize volatile trivalent arsenic fluoride to generate metal salt or complex of high boiling point pentavalent arsenic, and then the metal salt or complex is usedAnd (3) removing by a rectification method. The fluorine gas is adopted to oxidize arsenic impurities in the hydrogen fluoride to generate high-boiling-point substance HAsF6、MAsF6(metal salt or complex of pentavalent arsenic), and reusing HAsF as high boiling substance6、MAsF6Compared with volatility difference of HF and other components, the method adopts multiple equilibrium processes to separate pure electronic grade hydrogen fluoride from a multi-component mixture. The rectification process flow adopts reflux liquid and ascending gas to form gas-liquid countercurrent contact in a distillation tower, the non-volatile components in the ascending gas are continuously condensed, and simultaneously the non-volatile components are continuously received from the reflux liquid flowing from top to bottom, so that the content of the volatile components is continuously improved in the ascending process, the volatile components with higher purity can be obtained from the top of the tower, and on the other hand, the volatile components in the reflux liquid are continuously gasified in the flowing process, and simultaneously the non-volatile components condensed in the ascending steam are continuously received, so that the content of the non-volatile components is continuously improved, and the non-volatile components with higher purity can be obtained at the bottom of the tower. The tail gas generated in the rectification of the hydrogen fluoride mainly comprises HF steam and volatile component SO2、SiF4、PF3、POF3、AsF5、SF6、PF5And the tail gas can be completely washed by pure water and condensed to prepare industrial hydrofluoric acid.
The inventor finds that HF steam and normal-temperature non-condensable gas SO in tail gas2、SiF4、PF3、POF3、AsF5、SF6、PF5The method can be recycled by using a pure water washing condensation absorption method, the problem that the liquid level of condensate rises to block an air inlet conduit and reflux is often caused in the implementation process of the combination of a washing absorption tower and a condensation tower because the washing absorption tower and the condensation tower cannot be effectively communicated to realize gas-liquid two-phase balance, the gas-liquid two phases in the washing absorption tower and the condensation tower are in a violent mass and heat transfer working state, the temperature and the pressure of the gas-liquid two phases are in extremely complex changes, the requirement of balancing the gas-liquid two phases is difficult to realize on any working surface in a working environment, for example, the gas in a circulating storage tank is more, and the washing absorption tower conveys the gas-liquid twoThe gas seal phenomenon can occur in the pipeline of the ring storage tank, so that the stored liquid at the bottom of the washing absorption tower cannot be conveyed, the liquid level is raised, the gas inlet guide pipe is submerged and reflows, and therefore the effective communication between the washing absorption tower and the condensing tower is definitely a good method under the condition that the process conditions allow. The specific implementation mode is that the bottoms of the washing absorption tower and the condensing tower are communicated with a circulating storage tank to form a U-shaped communicating vessel, hydrofluoric acid condensate of the washing absorption tower and the condensing tower is converged in the circulating storage tank, and the liquid level of the hydrofluoric acid condensate is more than 1000mm away from an air inlet guide pipe and a tail gas discharge port, so that liquid seal is formed at the bottoms of the washing absorption tower and the condensing tower, and even if the hydrofluoric acid condensate in the circulating storage tank is continuously prepared or returns to the washing absorption tower to condense and wash tail gas in work, the liquid level can be effectively balanced due to the mutual communication, and the liquid seal is always kept in an effective working state. Tail gas passes through air inlet pipe, filler, cloth liquid grid plate, spraying pipe fitting, exhaust pipe, tail gas import, condenser pipe board, liquid removal device, tail gas discharge port in proper order and accomplishes the condensation process, and the hydrofluoric acid condensate that condenses off collects the circulation storage tank through collector tube and condensate outlet with gaseous separation, because the effect of liquid seal, the unable drunkenness of tail gas takes place the back mixing phenomenon in reaching the circulation storage tank, just can not take place to carry the problem that the air inlet pipe of tail gas blockked up even backward flow.
The inventor finds that the tail gas inlet and the condensation tower body of the condensation tower are designed by adopting the venturi tube principle, and aims to enable tail gas to enter the condensation tower body with a larger diameter for diffusion after being compressed by the tail gas inlet with a smaller diameter, so that liquid drops are uniformly distributed in the tail gas, and the condensation efficiency of the condensation tower in a condensation pipe plate is improved.
The inventor finds that as the bottoms of the washing absorption tower and the condensing tower are communicated with the circulating storage tank, the washing liquid of the washing absorption tower and the condensate of the condensing tower are collected in the circulating storage tank, and the condensate is conveyed back to the washing absorption tower through the circulating pump assembly to continuously cool the washing tail gas, the concentration of hydrofluoric acid absorbed by pure water in the circulating storage tank is higher and higher, and industrial hydrofluoric acid with various concentrations can be obtained according to requirements.
Compared with the prior art, the invention at least has the following advantages: firstly, the bottoms of a washing absorption tower and a condensing tower are communicated with a circulating storage tank to form a U-shaped communicating vessel, hydrofluoric acid condensate of the washing absorption tower and the condensing tower is converged in the circulating storage tank, and the liquid level of the hydrofluoric acid condensate is more than 1000mm away from an air inlet guide pipe and a tail gas discharge port, so that liquid seal is formed at the bottoms of the washing absorption tower and the condensing tower, and even if the hydrofluoric acid condensate in the circulating storage tank continuously prepares products or returns to the washing absorption tower to condense and wash tail gas in work, the liquid level can be effectively balanced due to the mutual communication, and the liquid seal always keeps an effective working state; secondly, due to the effect of liquid seal, the tail gas can not flow into the circulating storage tank in a channeling way to generate a back mixing phenomenon, so that the problem that an air inlet duct for conveying the tail gas is blocked and even flows back can not occur.
Drawings
FIG. 1 is a schematic front view of an apparatus for preparing electronic grade hydrogen fluoride scrubbing and absorbing.
FIG. 2 is a schematic top view of an apparatus for preparing electronic grade HF scrubbing-absorbing material according to the present invention.
FIG. 3 is a schematic diagram of the arrangement of section A-A of an apparatus for preparing electronic grade hydrogen fluoride scrubbing-absorption unit according to the present invention.
1-washing absorption tower 2-circulating storage tank 3-circulating pump assembly 4-condensing tower
5-liquid collecting pipe 6-washing absorption tower body 7-air inlet guide pipe 8-filler 9-liquid distribution grid plate
10-spraying pipe fitting 11-exhaust conduit 12-tail gas inlet 13-condensation tower
14-condenser tube plate 15-liquid removing device 16-tail gas discharge port 17-condensate outlet.
Detailed Description
The invention is further described with reference to the following detailed description of embodiments and drawings.
As shown in fig. 1, fig. 2 and fig. 3, the device for preparing electronic grade hydrogen fluoride washing and absorbing is characterized in that: the device comprises a washing absorption tower 1, a circulating storage tank 2, a circulating pump assembly 3 and a condensing tower 4, wherein the bottoms of the washing absorption tower 1 and the condensing tower 4 are communicated with the circulating storage tank 2 to form a U-shaped communicating vessel.
The washing absorption tower 1 comprises a liquid collecting pipe 5, a washing absorption tower body 6, an air inlet guide pipe 7, a filler 8, a liquid distribution grid plate 9, a spraying pipe 10 and an exhaust guide pipe 11, and the condensing tower 4 comprises a tail gas inlet 12, a condensing tower body 13, a condensing pipe plate 14, a liquid removing device 15, a tail gas discharge port 16 and a condensate outlet 17.
Tail gas sequentially passes through the air inlet guide pipe 7, the filler 8, the liquid distribution grid plate 9, the spraying pipe fitting 10, the exhaust guide pipe 11, the tail gas inlet 12, the condensing pipe plate 14, the liquid removing device 15 and the tail gas discharge port 16 to complete the condensation process, condensed hydrofluoric acid condensate is separated from gas and collected into the circulating storage tank 2 through the liquid collecting pipe 5 and the condensate outlet 17, and the circulating pump assembly 3 returns the hydrofluoric acid condensate in the circulating storage tank 2 to the spraying pipe fitting 10 to wash and condense the tail gas.
The tail gas inlet 12 and the condensation tower body 13 of the condensation tower 4 are designed by adopting the venturi tube principle, and the purpose is to enable the tail gas to enter the condensation tower body 13 with a larger diameter for diffusion after being compressed by the tail gas inlet 12 with a smaller diameter, so that liquid drops are uniformly distributed in the tail gas, and the condensation efficiency of the condensation tube plate 14 is improved.
Variations and modifications to the above-described embodiments may occur to those skilled in the art, which fall within the scope and spirit of the above description. Therefore, the present invention is not limited to the specific embodiments disclosed and described above, and some modifications and variations of the present invention should fall within the scope of the claims of the present invention. Furthermore, although specific terms are employed herein, they are used in a generic and descriptive sense only and not for purposes of limitation.

Claims (2)

1. A washing and absorbing device for preparing electronic-grade hydrogen fluoride is characterized in that: the device comprises a washing absorption tower, a circulating storage tank, a circulating pump assembly and a condensing tower, wherein the bottoms of the washing absorption tower and the condensing tower are communicated with the circulating storage tank to form a U-shaped communicating vessel; the washing absorption tower comprises a liquid collecting pipe, a washing absorption tower body, an air inlet guide pipe, a filler, a liquid distribution grid plate, a spraying pipe fitting and an exhaust guide pipe; the condensing tower comprises a tail gas inlet, a condensing tower body, a condensing tube plate, a liquid removing device, a tail gas discharge port and a condensate outlet; the hydrofluoric acid condensate of the circulating storage tank and the tail gas discharge port is converged in the circulating storage tank, the liquid level of the hydrofluoric acid condensate is 1000mm or more lower than that of the air inlet guide pipe and the tail gas discharge port, so that liquid seals are formed at the bottoms of the washing absorption tower and the condensing tower, the hydrofluoric acid condensate in the circulating storage tank in work can continuously prepare products or return to the washing absorption tower to condense and wash tail gas, the liquid levels can be effectively balanced due to the mutual communication, and the liquid seals are always in an effective working state; the tail gas finishes the condensation process through an air inlet guide pipe, a filler, a liquid distribution grid plate, a spraying pipe fitting, an exhaust guide pipe, a tail gas inlet, a condensation pipe plate, a liquid removing device and a tail gas discharge port in sequence, condensed hydrofluoric acid condensate is separated from gas and collected into a circulating storage tank through a liquid collecting pipe and a condensate outlet, and the circulating pump assembly returns the hydrofluoric acid condensate in the circulating storage tank to the spraying pipe fitting to wash and condense the tail gas.
2. The apparatus of claim 1, wherein the apparatus comprises: the tail gas import and the condensation tower body of condensing tower adopt venturi principle design, and the purpose makes tail gas get into the great condensation tower body diffusion of diameter behind the less tail gas import compression of diameter, makes the liquid drop evenly distributed in tail gas to improve the condensation efficiency at the condensation tube sheet.
CN201811207316.2A 2018-10-17 2018-10-17 Preparation electronic level hydrogen fluoride washing absorbing device Active CN109200765B (en)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN201031140Y (en) * 2007-01-08 2008-03-05 战玉柏 Device for producing ultra-clear and high-purity
CN203540322U (en) * 2013-10-28 2014-04-16 济南卡博唐生物科技有限公司 System for absorbing HCL gas in tail gas
CN105800559A (en) * 2014-12-30 2016-07-27 有研稀土新材料股份有限公司 Hydrofluoric acid recycling device and hydrofluoric acid recycling method
CN206168193U (en) * 2016-05-30 2017-05-17 李景致 Safety ring protects multi -functional chlorine absorbing device that lets out

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5064450A (en) * 1991-01-02 1991-11-12 Uop Gas absorber method and apparatus

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN201031140Y (en) * 2007-01-08 2008-03-05 战玉柏 Device for producing ultra-clear and high-purity
CN203540322U (en) * 2013-10-28 2014-04-16 济南卡博唐生物科技有限公司 System for absorbing HCL gas in tail gas
CN105800559A (en) * 2014-12-30 2016-07-27 有研稀土新材料股份有限公司 Hydrofluoric acid recycling device and hydrofluoric acid recycling method
CN206168193U (en) * 2016-05-30 2017-05-17 李景致 Safety ring protects multi -functional chlorine absorbing device that lets out

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