CN109224775B - Washing tower for preparing hydrogen fluoride - Google Patents
Washing tower for preparing hydrogen fluoride Download PDFInfo
- Publication number
- CN109224775B CN109224775B CN201811207321.3A CN201811207321A CN109224775B CN 109224775 B CN109224775 B CN 109224775B CN 201811207321 A CN201811207321 A CN 201811207321A CN 109224775 B CN109224775 B CN 109224775B
- Authority
- CN
- China
- Prior art keywords
- washing
- gas
- tower
- acid
- storage tank
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Images
Classifications
-
- 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
- B01D53/1456—Removing acid components
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B7/00—Halogens; Halogen acids
- C01B7/19—Fluorine; Hydrogen fluoride
- C01B7/191—Hydrogen fluoride
- C01B7/192—Preparation from fluorspar
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B7/00—Halogens; Halogen acids
- C01B7/19—Fluorine; Hydrogen fluoride
- C01B7/191—Hydrogen fluoride
- C01B7/195—Separation; Purification
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Analytical Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (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 tower for preparing hydrogen fluoride. The method is characterized in that: the device comprises a washing tower, a washing circulation storage tank, a washing acid pump assembly and a primary condenser, wherein the bottoms of the washing tower and the primary condenser are communicated with the washing circulation storage tank to form a U-shaped communicating vessel.
Description
Technical Field
The invention relates to the technical field of fluorine chemical industry, in particular to a washing tower for preparing hydrogen fluoride.
Background
Hydrogen fluoride has been widely used in the industries of electronics, chemical industry, petroleum and the like, and is mainly used for preparing villiaumite, fluorine-halogen alkane, fluorine refrigerant, corrosion glass, wood impregnation, electrolysis of elemental fluorine and the like. The Chinese invention patent (with the patent number of CN201310287202.4, the patent name is an anhydrous hydrogen fluoride production method) discloses an anhydrous hydrogen fluoride production method, which is characterized by comprising the following steps: feeding fluorite powder and sulfuric acid into a pre-reactor; in a pre-reactor, sulfuric acid and fluorite powder are fully mixed and react at the same time to generate crude hydrogen fluoride gas; removing impurities from the crude hydrogen fluoride gas through a pre-purification tower and a washing tower, then sequentially passing through two condensers, condensing most of the hydrogen fluoride gas by a freezing medium, refluxing condensate obtained in the first condenser to the pre-purification tower, and pumping crude acid condensate obtained in the second condenser to a rectifying tower through a second crude acid pump for refining; anhydrous hydrofluoric acid leaves the rectifying tower by means of the pressure of the tower and flows to an anhydrous hydrogen fluoride finished product storage tank through a finished product cooler; the non-condensable gas at the top of the rectifying tower and in the hydrogen fluoride condenser enters a sulfuric acid absorption tower; sulfuric acid flows downwards from the top of the tower and absorbs hydrogen fluoride in a gas phase; returning the sulfuric acid containing hydrogen fluoride to the scrubber with a pump; the gas leaving the top of the sulfuric acid absorption tower passes through a water washing tower to obtain a byproduct, namely fluosilicic acid; the sulfuric acid absorbed with hydrogen fluoride is returned to the pre-reactor through the washing tower. The Chinese invention patent (with the patent number of CN201210506779.5, the patent name is a preparation method of anhydrous hydrogen fluoride) discloses a preparation method of anhydrous hydrogen fluoride, which is characterized by comprising the following steps: a) respectively heating mixed sulfuric acid and fluorspar powder, mixing in a pre-reactor according to a certain feeding weight ratio, and carrying out pre-reaction to obtain a mixed material, wherein the mixed sulfuric acid is a mixture of concentrated sulfuric acid and fuming sulfuric acid, and the weight ratio of the sulfuric acid to the fuming sulfuric acid is 1: 1.40-1.50; the heating time of the mixed sulfuric acid is 7-8 minutes, and the heating temperature is 100-120 ℃; b) continuously feeding the mixed material into a converter reactor, reacting the mixed material at 550-650 ℃ and 700-800 ℃ for 50-70 minutes under the conditions that the rotating speed of the converter reactor is 1.0 r/min-2.0 r/min and the pressure in the converter is-0.55-0.45 KPa, so as to obtain crude hydrogen fluoride gas and solid material, feeding part of the obtained solid material into the converter reactor through a material returning device for secondary reaction, and feeding the rest solid material into a dihydrate gypsum production device; c) treating the crude hydrogen fluoride gas by a washing tower, a condenser, a rectifying tower and a degassing tower to obtain pure hydrogen fluoride gas and residual gas; d) recycling the residual gas by using sulfuric acid to absorb hydrogen fluoride gas; e) and residual gas which is not recycled is discharged from the top of the tail gas tower after being treated by a water washing tower and a tail gas tower.
The hydrogen fluoride separation impurity refining device in the prior art 1 and the prior art 2 is a pre-purification tower, a washing tower, a condenser, a rectifying tower and a degassing tower which are commonly used at present, wherein washing and condensing are one of the processes of refining anhydrous hydrogen fluoride generally, and the prior art mainly has the problems that washing acid coming out of the bottom of the washing tower enters a washing circulation storage tank, a washing acid pipeline is generally inserted into the washing circulation storage tank, the liquid level of the washing acid rises below 800mm, if too much gas is back-mixed with acid liquor, the liquid level of the washing acid in the washing tower rises, a gas guide pipe for conveying hydrofluoric acid gas is blocked and flows back to a reaction furnace, and corrosion is caused to a reaction furnace body.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a washing tower for preparing hydrogen fluoride, which is characterized in that: the device comprises a washing tower, a washing circulation storage tank, a washing acid pump assembly and a primary condenser, wherein the bottoms of the washing tower and the primary condenser are communicated with the washing circulation storage tank to form a U-shaped communicating vessel.
The washing tower comprises a washing acid outlet I, a washing tower body, an air duct, a tower tray, a liquid separating tray, a spraying assembly and an exhaust port, wherein the first-stage condenser comprises an air inlet, a first-stage condenser body, a condensing pipe plate assembly, a liquid remover, an air outlet and a washing acid outlet II.
Hydrofluoric acid gas finishes the condensation process through a gas guide pipe, a tower tray, a liquid separation disc, a spraying assembly, an exhaust port, a gas inlet, a condensation pipe plate assembly, a liquid remover and a gas outlet in sequence, condensed washing acid is separated from gas and is collected into a washing circulation storage tank through a washing acid outlet I and a washing acid outlet II, and washing acid in the washing circulation storage tank is returned to the spraying assembly by a washing acid pump assembly to wash the condensed hydrofluoric acid gas.
The inventors found that fluorite (CaF) for producing hydrogen fluoride2) And sulfuric acid (H)2SO4) The following main reactions occur: CaF2+2H2S04→2HF+CaSO4The product entering the next process stage has mainly a heavy fraction H2SO4、H2O, light component SO2、SiF4、CO2、H2S, by-products including CaSO4、Fe2(SO4)3、H2SiF6. According to the requirements of national standard GB 7746-2SO4、H2O、H2SiF6、SO2The content of the hydrofluoric acid is limited, and the anhydrous hydrogen fluoride is prepared by removing impurities by washing, condensing, rectifying and degassing processes by utilizing the difference of the boiling points of the components, specifically, hydrofluoric acid gas enters a washing tower from a reaction furnace for washing, after dust and water impurities are removed, the hydrofluoric acid gas enters a condensing system from the washing tower, and crude hydrofluoric acid liquid (the main component of which is a heavy component H) is formed by primary condensation through primary, secondary and tertiary condensation and primary condensation after primary condensation through primary condensation2SO4、H2O) returns to the washing tower to condense and wash hydrofluoric acid gas, and crude hydrofluoric acid liquid (the main component is hydrofluoric acid) condensed from the second and third stages is sent into a degassing tower and a rectifying tower by a rectifying pump to further remove light component SO2、SiF4、CO2、H2S and heavy component H2SO4、H2And O, obtaining the finished product of the anhydrous hydrogen fluoride. The prior art mainly has the problems that the washing acid coming out of the bottom of the washing tower enters a washing circulation storage tank, a washing acid pipeline is generally inserted below the liquid level of the washing circulation storage tank, if the gas back-mixed by the acid liquid is too much, the liquid level of the washing acid in the washing tower rises, and the hydrofluoric acid gas is conveyedThe gas-guide tube is blocked and flows back to the reaction furnace, thus causing corrosion to the reaction furnace body.
The inventor finds that the problem of blockage and backflow of a hydrofluoric acid gas guide tube to a reaction furnace is caused by the fact that a washing tower and a condenser cannot be effectively communicated to achieve gas-liquid two-phase balance, the gas-liquid two phases in the washing tower and the condenser are in a severe mass and heat transfer working state, the temperature and the pressure of the gas-liquid two phases are in extremely complex changes, and the requirement of balancing the gas-liquid two phases is difficult to achieve on any working surface in a working environment, so that the effective communication between the washing tower and the condenser is undoubtedly a good method under the condition that process conditions are allowed. The specific implementation mode is that the bottoms of the washing tower and the first-stage condenser are communicated with a washing circulation storage tank to form a U-shaped communicating vessel, washing acids of the washing tower and the first-stage condenser are collected in the washing circulation storage tank, and the surface of the washing acid liquid is more than 1000mm away from the gas guide pipe and the gas outlet, so that liquid seal is formed at the bottoms of the washing tower and the first-stage condenser, even if the washing acid in the washing circulation storage tank is continuously conveyed into a reaction furnace to react or returns to the washing tower to condense and wash hydrofluoric acid gas in work, the liquid level can be effectively balanced due to the mutual communication, and the liquid seal is always kept. Hydrofluoric acid gas finishes the condensation process through air duct, tower tray, liquid separation dish, spray set, gas vent, air inlet, condensation tube plate subassembly, liquid trap, gas outlet in proper order, and the scrubbing acid that condenses is separated with gas and is collected in the washing circulation storage tank through scrubbing acid export I and scrubbing acid export II, because the effect of liquid seal, hydrofluoric acid gas can't the cross flow take place back mixing phenomenon in the washing circulation storage tank, just can not take place to carry the problem that the air duct of hydrofluoric acid gas blocks up or even flows back to the reacting furnace.
Compared with the prior art, the invention at least has the following advantages: firstly, the bottoms of the washing tower and the first-stage condenser are communicated with a washing circulation storage tank to form a U-shaped communicating vessel, washing acids of the washing tower and the first-stage condenser are collected in the washing circulation storage tank, and the surface distance between the washing acid liquid and the gas guide pipe and the gas outlet is more than 1000mm, so that liquid seal is formed at the bottoms of the washing tower and the first-stage condenser, even if the washing acids in the washing circulation storage tank are continuously conveyed into a reaction furnace to react or return to the washing tower to condense and wash hydrofluoric acid gas in work, the liquid levels can be effectively balanced due to the mutual communication, and the liquid seal always keeps an effective working; secondly, due to the action of liquid seal, hydrofluoric acid gas can not flow into the washing circulation storage tank to cause back mixing, and the problem that the gas guide pipe for conveying the hydrofluoric acid gas is blocked and even flows back to the reaction furnace can not occur.
Drawings
FIG. 1 is a schematic diagram of a main view of a scrubber for preparing hydrogen fluoride according to the present invention.
FIG. 2 is a schematic top view of a scrubber for producing hydrogen fluoride according to the present invention.
FIG. 3 is a schematic diagram of the arrangement of the section A-A of a scrubber for preparing hydrogen fluoride according to the present invention.
1-washing tower 2-washing circulation storage tank 3-washing acid pump assembly 4-first-stage condenser
5-washing acid outlet I6-washing tower body 7-gas guide tube 8-tower tray 9-liquid separation disc
10-spraying component 11-exhaust port 12-air inlet 13-primary condenser body
14-a condensing tube plate assembly 15-a liquid remover 16-a gas outlet 17-a washing acid outlet II.
Detailed Description
The invention is further described with reference to the following detailed description of embodiments and drawings.
As shown in fig. 1, 2 and 3, a scrubber for producing hydrogen fluoride is characterized in that: the device comprises a washing tower 1, a washing circulation storage tank 2, a washing acid pump assembly 3 and a primary condenser 4, wherein the bottoms of the washing tower 1 and the primary condenser 4 are communicated with the washing circulation storage tank 2 to form a U-shaped communicating vessel.
The washing tower 1 comprises a washing acid outlet I5, a washing tower body 6, an air duct 7, a tower tray 8, a liquid separating disc 9, a spraying assembly 10 and an exhaust port 11, wherein the first-stage condenser 4 comprises an air inlet 12, a first-stage condenser body 13, a condensing tube plate assembly 14, a liquid remover 15, an air outlet 16 and a washing acid outlet II 17.
Hydrofluoric acid gas finishes the condensation process through a gas guide pipe 7, a tower tray 8, a liquid separation disc 9, a spraying assembly 10, an exhaust port 11, a gas inlet 12, a condensation tube plate assembly 14, a liquid remover 15 and a gas outlet 16 in sequence, condensed washing acid and gas are separated and collected into a washing circulation storage tank 2 through a washing acid outlet I5 and a washing acid outlet II 17, and the washing acid in the washing circulation storage tank 2 is returned to the spraying assembly 10 by a washing acid pump assembly 3 to wash the condensed hydrofluoric acid gas.
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 (1)
1. A washing tower for preparing hydrogen fluoride is characterized in that: the washing tower and the bottom of the first-stage condenser are communicated with the washing circulating storage tank to form a U-shaped communicating vessel, washing acids of the washing tower and the first-stage condenser are converged in the washing circulating storage tank, and the height of a washing acid liquid surface is over 1000mm of a gas guide pipe and a gas outlet, so that liquid seals are formed at the bottoms of the washing tower and the first-stage condenser; the washing tower comprises a washing acid outlet I, a washing tower body, a gas guide pipe, a tower tray, a liquid separation tray, a spraying assembly and an exhaust port; the primary condenser comprises an air inlet, a primary condenser body, a condensing tube plate assembly, a liquid remover, an air outlet and a washing acid outlet II; hydrofluoric acid gas finishes the condensation process through a gas guide pipe, a tower tray, a liquid separation disc, a spraying assembly, an exhaust port, a gas inlet, a condensation pipe plate assembly, a liquid remover and a gas outlet in sequence, condensed washing acid and gas are separated and collected into a washing circulation storage tank through a washing acid outlet I and a washing acid outlet II, the hydrofluoric acid gas cannot flow into the washing circulation storage tank to generate a back mixing phenomenon due to the liquid seal effect, the problem that the gas guide pipe for conveying the hydrofluoric acid gas is blocked and even flows back to a reaction furnace is avoided, and the washing acid in the washing circulation storage tank is returned to the spraying assembly by a washing acid pump assembly to wash the condensed hydrofluoric acid gas.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811207321.3A CN109224775B (en) | 2018-10-17 | 2018-10-17 | Washing tower for preparing hydrogen fluoride |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811207321.3A CN109224775B (en) | 2018-10-17 | 2018-10-17 | Washing tower for preparing hydrogen fluoride |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN109224775A CN109224775A (en) | 2019-01-18 |
| CN109224775B true CN109224775B (en) | 2020-08-07 |
Family
ID=65052221
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201811207321.3A Active CN109224775B (en) | 2018-10-17 | 2018-10-17 | Washing tower for preparing hydrogen fluoride |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN109224775B (en) |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3840646A (en) * | 1972-05-17 | 1974-10-08 | Fuji Kasui Eng Co Ltd | Process for recovering nitric acid from waste pickle liquor solution |
| 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 |
| CN107082407A (en) * | 2017-06-22 | 2017-08-22 | 多氟多化工股份有限公司 | A kind of method of purification of anhydrous hydrofluoric acid |
| CN207187454U (en) * | 2017-07-24 | 2018-04-06 | 广元金弘农林有限公司 | A kind of refrigeration compressed air dryer gas and water separator |
-
2018
- 2018-10-17 CN CN201811207321.3A patent/CN109224775B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3840646A (en) * | 1972-05-17 | 1974-10-08 | Fuji Kasui Eng Co Ltd | Process for recovering nitric acid from waste pickle liquor solution |
| 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 |
| CN107082407A (en) * | 2017-06-22 | 2017-08-22 | 多氟多化工股份有限公司 | A kind of method of purification of anhydrous hydrofluoric acid |
| CN207187454U (en) * | 2017-07-24 | 2018-04-06 | 广元金弘农林有限公司 | A kind of refrigeration compressed air dryer gas and water separator |
Also Published As
| Publication number | Publication date |
|---|---|
| CN109224775A (en) | 2019-01-18 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN109052326B (en) | Use method of process device for preparing electronic-grade hydrogen fluoride | |
| CN107082407B (en) | A kind of method of purification of anhydrous hydrofluoric acid | |
| CN108928804B (en) | Use method of washing tower for preparing hydrogen fluoride | |
| CN109224775B (en) | Washing tower for preparing hydrogen fluoride | |
| CN109200764B (en) | Use method for preparing electronic-grade hydrogen fluoride washing and absorbing device | |
| CN112661115B (en) | Separation and purification method for deep dehydration and impurity removal of FTrPSA refined by anhydrous HF produced by fluorite method | |
| CN108727160A (en) | A kind of alkyl esterification method production glyphosate hydrolyzing tail gas pressure control reclaimer and technique | |
| KR101306328B1 (en) | Method and apparatus for recovering hexafluorosilicic acid from manufacturing process of phosphoric acid | |
| CN217340094U (en) | Production device for preparing anhydrous hydrogen fluoride and coproducing hydrofluoric acid and hydrogen fluoride | |
| CN115518402B (en) | Toluene chlorination liquid post-treatment device and treatment method | |
| CN108946668B (en) | Preparation process of anhydrous hydrogen fluoride | |
| CN217808771U (en) | Refining system of anhydrous hydrogen fluoride | |
| CN208182895U (en) | A kind of tetrahydrofuran fractional order reaction separator | |
| CN109248642A (en) | A kind of application method preparing hydrogen fluoride stratum granulosum moving bed filter | |
| CN113233422B (en) | Method and system for separating SiF4 and HF mixed gas | |
| CN108996474B (en) | Process device for preparing electronic-grade hydrogen fluoride | |
| CN109052325B (en) | Preparation process of electronic grade hydrogen fluoride | |
| CN109200765B (en) | Preparation electronic level hydrogen fluoride washing absorbing device | |
| CN108892104B (en) | Application method of hydrogen fluoride preparation process device | |
| CN1201401A (en) | Method of recovering fluorine compounds from vapors exiting wet process phosphoric acid evaporators | |
| CN207187475U (en) | A kind of gas purifying device of chlorodifluoromethane | |
| CN109437108A (en) | A kind of waste acidity recovery 26%-28% hydrogen chloride new process | |
| CN114314539A (en) | Method for multi-effect sectional concentration and fractional flash defluorination of wet-process phosphoric acid | |
| CN108910827B (en) | Process device for preparing hydrogen fluoride | |
| CN111170873A (en) | Method for extracting N, N-dimethyl-1, 3-propane diamine from betaine wastewater |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| TA01 | Transfer of patent application right | ||
| TA01 | Transfer of patent application right |
Effective date of registration: 20200630 Address after: No.10, Tongshun Road, Nantong Economic and Technological Development Zone, Jiangsu Province, 226000 Applicant after: Houcheng new materials (Nantong) Co., Ltd Address before: 362000 Yuanyuan, 610 Xinmen Street, Licheng District, Quanzhou City, Fujian Province, and 32 buildings and 2 floors of 1916 Creative Industry Park Applicant before: Yang Song |
|
| GR01 | Patent grant | ||
| GR01 | Patent grant |