CN118183628A - Method for preparing high-purity halide wet electronic chemicals by using sub-boiling distillation method - Google Patents
Method for preparing high-purity halide wet electronic chemicals by using sub-boiling distillation method Download PDFInfo
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- CN118183628A CN118183628A CN202410506445.0A CN202410506445A CN118183628A CN 118183628 A CN118183628 A CN 118183628A CN 202410506445 A CN202410506445 A CN 202410506445A CN 118183628 A CN118183628 A CN 118183628A
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- 238000009835 boiling Methods 0.000 title claims abstract description 77
- 150000004820 halides Chemical class 0.000 title claims abstract description 32
- 238000000034 method Methods 0.000 title claims abstract description 30
- 238000004821 distillation Methods 0.000 title claims abstract description 25
- 239000000126 substance Substances 0.000 title claims abstract description 23
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 123
- 238000010521 absorption reaction Methods 0.000 claims abstract description 77
- 239000006096 absorbing agent Substances 0.000 claims abstract description 64
- 239000011552 falling film Substances 0.000 claims abstract description 60
- 229910000041 hydrogen chloride Inorganic materials 0.000 claims abstract description 52
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 claims abstract description 52
- 229910000039 hydrogen halide Inorganic materials 0.000 claims abstract description 52
- 239000012433 hydrogen halide Substances 0.000 claims abstract description 52
- 239000007788 liquid Substances 0.000 claims abstract description 43
- 239000007789 gas Substances 0.000 claims abstract description 38
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 15
- 238000010438 heat treatment Methods 0.000 claims abstract description 10
- 238000007599 discharging Methods 0.000 claims abstract description 3
- 239000000463 material Substances 0.000 claims abstract description 3
- 239000012535 impurity Substances 0.000 claims description 7
- 229910021645 metal ion Inorganic materials 0.000 claims description 5
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 4
- CPELXLSAUQHCOX-UHFFFAOYSA-N Hydrogen bromide Chemical compound Br CPELXLSAUQHCOX-UHFFFAOYSA-N 0.000 claims description 4
- 239000000498 cooling water Substances 0.000 claims description 3
- 229910000042 hydrogen bromide Inorganic materials 0.000 claims description 2
- 229910000040 hydrogen fluoride Inorganic materials 0.000 claims description 2
- 238000009834 vaporization Methods 0.000 claims description 2
- 230000008016 vaporization Effects 0.000 claims description 2
- 238000010533 azeotropic distillation Methods 0.000 claims 1
- 230000026030 halogenation Effects 0.000 abstract 1
- 238000005658 halogenation reaction Methods 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 18
- 238000011084 recovery Methods 0.000 description 9
- 229910021642 ultra pure water Inorganic materials 0.000 description 8
- 239000012498 ultrapure water Substances 0.000 description 8
- 239000000443 aerosol Substances 0.000 description 5
- 238000002309 gasification Methods 0.000 description 5
- 239000007791 liquid phase Substances 0.000 description 5
- 238000011049 filling Methods 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 238000002360 preparation method Methods 0.000 description 4
- 238000005265 energy consumption Methods 0.000 description 3
- 239000012071 phase Substances 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 238000007670 refining Methods 0.000 description 2
- 238000010992 reflux Methods 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- BMYNFMYTOJXKLE-UHFFFAOYSA-N 3-azaniumyl-2-hydroxypropanoate Chemical compound NCC(O)C(O)=O BMYNFMYTOJXKLE-UHFFFAOYSA-N 0.000 description 1
- 239000002250 absorbent Substances 0.000 description 1
- 230000002745 absorbent Effects 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000001174 ascending effect Effects 0.000 description 1
- 239000001110 calcium chloride Substances 0.000 description 1
- 229910001628 calcium chloride Inorganic materials 0.000 description 1
- 230000001143 conditioned effect Effects 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 230000006837 decompression Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000007770 graphite material Substances 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- -1 hydrogen halides Chemical class 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 230000009972 noncorrosive effect Effects 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Classifications
-
- 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
- C01B7/01—Chlorine; Hydrogen chloride
- C01B7/07—Purification ; Separation
- C01B7/0706—Purification ; Separation of hydrogen chloride
- C01B7/0712—Purification ; Separation of hydrogen chloride by distillation
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
Abstract
The invention discloses a method for preparing high-purity halide wet electronic chemicals by adopting a near-sub-boiling distillation method, which belongs to the technical field of wet electronic chemicals and comprises the following steps of: (1) Feeding industrial liquid hydrogen halide from the middle lower part of the sub-boiling distiller, and enabling circulating water to serve as a heat source to enter an external heating sleeve of the sub-boiling distiller; the industrial liquid hydrogen halide is in a sub-boiling state in the sub-boiling distiller, the liquid hydrogen halide does not rise along the wall, the hydrogen halide gas is discharged from the top of the sub-boiling distiller, and the liquid hydrogen halide enters the first-stage falling film absorber after being depressurized; discharging residual materials from the tower kettle of the sub-boiling distiller; (2) The hydrogen chloride gas which is not absorbed by the first-stage falling film absorber sequentially enters the second-stage falling film absorber and the absorption tower; the hydrogen halide solution discharged from the bottom of the first-stage falling film absorber enters a first-stage absorption tank, hydrogen halide in the absorption tank is taken as circulating absorption liquid, and enters the top of the first-stage falling film absorber through a first-stage circulating pump until the mass concentration of the hydrogen halide solution reaches the requirement of electronic-stage hydrogen halide, and the circulation is stopped to obtain electronic-stage halogenation.
Description
Technical Field
The invention belongs to the technical field of wet electronic chemicals, and particularly relates to a method for preparing high-purity halide wet electronic chemicals by adopting a sub-boiling distillation method.
Background
The high-purity halide belongs to a common wet electronic chemical, generally comprises hydrobromic acid, hydrochloric acid and hydrofluoric acid, and is mainly used for cleaning links in integrated circuit manufacturing and used for cleaning various metals, organic matters and particulate matters. Integrated circuits have higher purity requirements for wet electronics, essentially centered at levels above G3, and 12 inch wafer fabrication generally requires levels above G4 as wafer sizes are larger. Thus, high purity halides of G4, G5 grade place higher demands on the preparation process.
The purification method of the high-purity halide commonly used at present is to separate out gaseous halide from the aqueous solution of the halide, then filter, dehydrate and dry the gaseous halide, and then absorb the gaseous halide by ultrapure water to prepare the high-purity halide. For example, 31% industrial grade hydrochloric acid is adopted for preparing the electronic chemical grade hydrochloric acid, the hydrochloric acid gas is resolved by countercurrent contact of water vapor and the hydrochloric acid, the concentration of the hydrochloric acid in the resolving liquid is about 20%, at the moment, the halide and the water form an azeotrope, the hydrochloric acid cannot be resolved continuously, but only 10% of the hydrochloric acid is resolved by the method, and the utilization rate is about 30%. In particular, 1.65 tons of steam is needed for resolving one ton of hydrochloric acid, the needed steam consumption is large, and the energy consumption is high. The hydrogen chloride is circularly absorbed by the conditioned enterprises by utilizing the resolved azeotropic acid, and the enterprises without the cyclic absorption generally adopt salt (such as calcium chloride) adding rectification for deep resolution. Although the recovery rate of hydrogen chloride is higher in a single time of salt distillation, the cost of concentrating the calcium chloride solution is higher. In addition, the hydrochloric acid resolving tower is made of all-graphite materials, resolved hydrogen chloride gas contains 100ppm of water, and the hydrochloric acid resolving tower also needs to be subjected to treatment processes such as filtration, sulfuric acid drying and the like, so that equipment investment is large. Therefore, the existing preparation method of the high-purity halide has the defects of low recovery rate, higher energy consumption and large equipment investment.
In addition, the distillation operation must be carried out in such a way that the liquid is in a very boiling state, and an aerosol (aerosol) is formed in the still, i.e. a gas containing suspended droplets of the distilled liquid, which aerosol enters the condenser or is absorbed by the water into the product. Since these droplets are not purified by gasification, they still contain a certain amount of various impurities, thereby contaminating the quality of the distillate and thus reducing the quality of the high purity halide.
Disclosure of Invention
In order to obtain the high purity halide wet electron chemical, the present application provides a novel method for preparing the high purity halide wet electron chemical.
Based on the above purpose, the invention adopts the following technical scheme:
A method for preparing high purity halide wet electron chemicals using near-sub-boiling distillation comprising the steps of:
(1) Feeding industrial liquid hydrogen halide (more than or equal to 5.5N) from the middle lower part of the sub-boiling distiller, and taking circulating water at 25 ℃ as a heat source to enter an external heating sleeve of the sub-boiling distiller; the industrial liquid hydrogen halide is in a sub-boiling state in the sub-boiling distiller, the liquid hydrogen halide does not rise along the wall, the hydrogen halide gas is discharged from the top of the sub-boiling distiller, and the liquid hydrogen halide enters the first-stage falling film absorber after being depressurized; discharging residual materials from the tower kettle of the sub-boiling distiller;
(2) The hydrogen chloride gas which is not absorbed by the first-stage falling film absorber sequentially enters the second-stage falling film absorber and the absorption tower; the hydrogen halide solution discharged from the bottom of the first-stage falling film absorber enters a first-stage absorption tank, and hydrogen halide in the absorption tank is taken as circulating absorption liquid to enter the top of the first-stage falling film absorber through a first-stage circulating pump until the mass concentration of the hydrogen halide solution reaches the requirement of electronic-stage hydrogen halide, and the circulation is stopped to obtain electronic-stage hydrogen halide;
wherein the temperature of each stage of circulating absorption liquid is lower than the vaporization temperature of liquid hydrogen halide.
Further, the liquid level in the sub-boiling distiller is 50% -80%, the pressure in the sub-boiling distiller is 38barG-39barG, and the updraft rate of hydrogen chloride gas in the sub-boiling distiller is 3-6m/h.
The gasification temperature of the halide is pressure dependent, for example 38barG hydrogen chloride has a gasification temperature of 17 ℃. The circulating water at 25 ℃ is used for heating in the jacket, and the flow rate of the circulating water is determined according to the yield, so that the updraft rate is ensured to be 3-6m/h.
Further, the liquid level in the sub-boiling distiller is 60%, the pressure in the sub-boiling distiller is 38barG, and the ascending gas flow rate of the hydrogen chloride gas in the sub-boiling distiller is 3m/h.
Further, the hydrogen chloride gas which is not absorbed in the secondary falling film absorber enters the absorption tower after being discharged, the hydrogen halide solution discharged from the bottom of the secondary falling film absorber enters the secondary absorption tank, and the hydrogen halide in the absorption tank enters the top of the secondary falling film absorber through the secondary circulating pump as circulating absorption liquid.
Further, the hydrogen halide solution discharged from the tower bottom of the absorption tower is taken as circulating absorption liquid and enters the top of the absorption tower through a three-stage circulating pump.
Preferably, the hydrogen halide is hydrogen chloride, hydrogen fluoride or hydrogen bromide.
Preferably, the hydrogen halide is hydrogen chloride, the mass concentration of the electronic grade hydrogen chloride solution is 37%, and the impurity metal ion content is not more than 10ppt.
Further, a part of the hydrogen halide solution in the secondary absorption tank enters the top of the secondary falling film absorber through the secondary circulating pump to be circularly absorbed, and when the concentration of the hydrogen halide solution is absorbed to 22-25%, a part of the hydrogen halide solution is transferred to the primary absorption tank.
Further, a part of the hydrogen halide solution discharged from the bottom of the absorption tower enters the top of the absorption tower through a three-stage circulating pump, and when the circulating absorption concentration reaches 14-17%, a part of the hydrogen halide solution is transferred to a second-stage absorption tank.
Further, the shell pass of the primary falling film absorber and the secondary falling film absorber is filled with cooling water at 7 ℃, and the absorption temperature of the primary falling film absorber and the secondary falling film absorber is lower than 20 ℃.
Further, a cooler is arranged behind the absorption tower circulating pump.
Compared with the prior art, the invention has the following advantages:
The application adopts high-pressure liquefied halide as raw material, and is prepared by purifying again in a way of near-sub-boiling distillation and absorbing with ultrapure water, and has the characteristics of remarkable recovery rate, low equipment investment, short flow and more stable quality. Purified halides, typically high pressure liquefied hydrogen halides, are used as starting materials, are anhydrous, and are non-corrosive to equipment.
Taking hydrogen chloride as an example, the single recovery rate of sub-boiling distillation is close to more than 80 percent. The sub-boiling distillation evaporates the high-pressure liquefied hydrogen chloride, and the heat capacity of the sub-boiling distillation is about 0.3 times of that of water, so that the energy consumption of the evaporation process is very low. As the boiling point of the hydrogen chloride is only about 20 ℃ at normal temperature, the circulating water at 25 ℃ can be used as a sub-boiling distillation heat medium. The circulating water at 25 ℃ is taken as a heat source to enter a heating sleeve outside the sub-boiling distiller, the halide is not in direct contact with the heat source in the sub-boiling distiller, and the heat conduction is carried out through the jacket wall of the sub-boiling distiller, so that the hydrogen halide gas is distilled out, the consumption of the required hot water is only 0.3 times that of the hydrochloric acid, the temperature of the heat source is low, the consumption is low, and the consumed energy is low. The internal temperature of the sub-boiling distiller is below the boiling point of liquefied hydrogen chloride. The liquid phase does not boil and does not produce aerosol which is produced during normal boiling. The distilled hydrogen chloride gas does not contain aerosol, and can prevent liquid-phase hydrogen chloride microdroplets from being carried into the gas phase without gasification.
The reflux tank of the raw material high-purity hydrogen chloride refining tower enters a sub-boiling distiller, 80% hydrogen chloride is decompressed by a decompression valve and enters the lower end of a primary falling film absorber, and is in countercurrent contact with dilute hydrochloric acid from a secondary falling film absorber. Unabsorbed hydrogen chloride enters the lower end of the secondary absorber and is in countercurrent contact with dilute hydrochloric acid from the absorber. The hydrogen chloride which is not absorbed yet enters the bottom of the absorption tower from the top of the secondary falling film absorber, is absorbed by ultrapure water from the outside, and the noncondensable gas enters the tail gas treatment unit. And 20% of hydrogen chloride in the tower kettle enters an industrial grade hydrogen chloride filling unit, and the single hydrogen chloride recovery rate of the device is 80%.
Drawings
Fig. 1 is a process flow diagram of example 1.
In the figure, 1, a sub-boiling distiller; 2. a first stage falling film absorber; 3. a primary absorption tank; 4. a primary circulation pump; 5. a secondary falling film absorber; 6. a secondary absorption tank; 7. a secondary circulation pump; 8. an absorption tower; 9. a three-stage circulating pump; 10. a cooler; 11. an exhaust gas treatment device.
Detailed Description
Example 1
Taking the preparation of high-purity hydrochloric acid as an example, a wet electronic chemical hydrochloric acid solution is prepared by using a device shown in fig. 1, and the device adopts a sub-boiling distiller to realize the extraction of hydrogen chloride gas. The device comprises a sub-boiling distiller 1, wherein a top outlet of the sub-boiling distiller 1 is sequentially connected with a first-stage falling film absorber 2, a first-stage absorption tank 3 and a first-stage circulating pump 4; the top gas outlet of the first-stage falling film absorber 2 is sequentially connected with a second-stage falling film absorber 5, a second-stage absorption tank 6 and a second-stage circulating pump 7; the top gas outlet of the second-stage falling film absorber 5 is connected to an absorption tower 8, and a third-stage circulating pump 9 is arranged outside the absorption tower 8. Wherein the shell passes of the primary falling film absorber 2 and the secondary falling film absorber 5 are filled with cooling water at 7 ℃, and the absorption temperature of the primary falling film absorber 2 and the secondary falling film absorber 5 is lower than 20 ℃.
The sub-boiling distiller 1 comprises a tower main body, wherein a heating jacket is arranged at the middle lower part outside the tower main body, circulating water at 25 ℃ is used as a heat source to enter the heating jacket outside the sub-boiling distiller 1, liquefied hydrogen chloride in the tower main body is heated to be in a sub-boiling state, and hydrogen chloride gas without liquid droplets is absorbed by ultrapure water after being steamed out to form high-purity hydrochloric acid.
Specifically, the method comprises the following steps:
(1) Taking high-purity hydrochloric acid as an example, feeding purified liquefied hydrogen chloride below the liquid level of a sub-boiling distiller, controlling the liquid level in the sub-boiling distiller to be 50% -80%, preferably 60%, and feeding circulating water at 25 ℃ into an external heating sleeve of the sub-boiling distiller 1 as a heat source, wherein the pressure in the sub-boiling distiller is 38barG; the heating rate in the sub-boiling distiller 1 ensures that the gas phase gas speed in the tower is 3m/S, the temperature in the tower is 18-19 ℃, liquefied hydrogen chloride is in a sub-boiling state in the sub-boiling distiller 1, and hydrogen chloride gas without liquid phase droplets is discharged from the top of the sub-boiling distiller 1 and enters the first-stage falling film absorber 2 after being decompressed; the rest hydrochloric acid aqueous solution with the mass concentration of 20% is discharged from the tower kettle of the sub-boiling distiller 1 and then enters an industrial grade hydrogen chloride filling unit.
(2) The hydrogen chloride gas entering the first-stage falling film absorber 2 is partially absorbed by ultrapure water below 20 ℃, and enters the first-stage absorption tank 3 after forming an electronic-stage hydrochloric acid solution, and the unabsorbed hydrogen chloride gas enters the second-stage falling film absorber 5 after being discharged from the top; the hydrochloric acid solution in the primary absorption tank 3 is cooled and then enters the top of the primary falling film absorber 2 through the primary circulating pump 4 as circulating absorption liquid, until the hydrochloric acid solution in the primary absorption tank 3 reaches 36% -38%, the electronic grade hydrochloric acid in the primary absorption tank 3 is conveyed to a filling system, and the impurity content of the electronic grade hydrochloric acid is high-purity hydrochloric acid of G5 grade, and the impurity content of various metal ions is not more than 10ppt.
(3) The hydrogen chloride gas entering the second-stage falling film absorber 5 is partially absorbed by circulating absorption liquid below 20 ℃, hydrochloric acid solution is formed and then enters the second-stage absorption tank 6, and the unabsorbed hydrogen chloride gas is discharged from the top and then enters the bottom of the absorption tower 8; part of the hydrochloric acid solution in the secondary absorption tank 6 enters the top of the secondary falling film absorber 5 through the secondary circulating pump 7, and when the mass concentration of the hydrochloric acid solution reaches 20% -25%, part of the hydrochloric acid solution is circulated to the primary absorption tank 3 and is mixed with hydrochloric acid discharged from the bottom of the primary falling film absorber 2 to be used as circulating absorption liquid, and the circulating absorption liquid is circulated to the primary falling film absorber.
(4) The unabsorbed hydrogen chloride gas is continuously contacted with ultrapure water or circulating absorption liquid in the absorption tower 8 in a countercurrent way, and is continuously absorbed, low-concentration hydrochloric acid formed in the tower kettle is cooled by the cooler 10 and then is circulated to the top of the absorption tower as circulating absorption liquid, when the mass concentration of the low-concentration hydrochloric acid reaches 5% -10%, part of the circulating second-stage absorption tank 6 is mixed with hydrochloric acid discharged from the bottom of the second-stage falling film absorber 5 and then is used as circulating absorption liquid, and the circulating absorption liquid is circulated to the second-stage falling film absorber 6; the hydrogen chloride gas discharged from the top of the absorption tower 8 is sent to an alkaline washing step or an exhaust gas treatment device 11.
Meanwhile, the absorption liquid is recycled in the absorption tower, the secondary falling film absorber and the primary falling film absorber, so that the use of ultrapure water can be effectively reduced, the direct use amount of the absorbent is reduced, and the production cost is reduced.
In the process, the reflux tank of the raw material high-purity hydrogen chloride refining tower enters a sub-boiling distiller. In the sub-boiling distiller, 80% hydrogen chloride is gasified under reduced pressure after a pressure reducing valve and enters the lower end of a first-stage falling film absorber to be in countercurrent contact with dilute hydrochloric acid from a second-stage falling film absorber. Unabsorbed hydrogen chloride enters the lower end of the secondary absorber and is in countercurrent contact with dilute hydrochloric acid from the absorber. The hydrogen chloride which is not absorbed yet enters the bottom of the absorption tower from the top of the secondary falling film absorber, is absorbed by ultrapure water from the outside, and the noncondensable gas enters the tail gas treatment unit. Meanwhile, when 80% of hydrogen chloride is gasified under reduced pressure and enters the falling film absorber, 20% of high-pressure liquid-phase hydrogen chloride in the sub-boiling distiller enters the industrial-grade hydrogen chloride filling unit, and the recovery rate of the hydrogen chloride is 80% in the preparation process of the high-purity hydrochloric acid. As the gasification rate increases, the heavy components are enriched in the distiller liquid phase, so that the higher the recovery rate, the higher the heavy component content in the high-purity hydrochloric acid. Conversely, in order to control heavy components such as metal ion impurities, it is necessary to control the recovery rate within a reasonable range.
Example 2
A process for preparing wet electronics chemical hydrochloric acid using a sub-boiling distillation method, which differs from example 1 in that: the liquid level in the sub-boiling distiller and/or the pressure and/or the heating rate are different, and specific parameters are shown in table 1.
It can be seen from table 1 that the higher the liquid level in the sub-boiling still, the higher the gas phase gas velocity, the higher the recovery, and the higher the metal ion impurity content at the same operating pressure.
Claims (10)
1. A method for preparing high purity halide wet electron chemicals using near-azeotropic distillation comprising the steps of:
(1) Feeding industrial liquid hydrogen halide from the middle lower part of the sub-boiling distiller, and taking circulating water at 25 ℃ as a heat source to enter an external heating sleeve of the sub-boiling distiller; the industrial liquid hydrogen halide is in a sub-boiling state in the sub-boiling distiller, the liquid hydrogen halide does not rise along the wall, the hydrogen halide gas is discharged from the top of the sub-boiling distiller, and the liquid hydrogen halide enters the first-stage falling film absorber after being depressurized; discharging residual materials from the tower kettle of the sub-boiling distiller;
(2) The hydrogen chloride gas which is not absorbed by the first-stage falling film absorber sequentially enters the second-stage falling film absorber and the absorption tower; the hydrogen halide solution discharged from the bottom of the first-stage falling film absorber enters a first-stage absorption tank, and hydrogen halide in the absorption tank is taken as circulating absorption liquid to enter the top of the first-stage falling film absorber through a first-stage circulating pump until the mass concentration of the hydrogen halide solution reaches the requirement of electronic-stage hydrogen halide, and the circulation is stopped to obtain electronic-stage hydrogen halide;
wherein the temperature of each stage of circulating absorption liquid is lower than the vaporization temperature of liquid hydrogen halide.
2. The method for preparing high-purity halide wet electronic chemical by using the sub-boiling distillation method as claimed in claim 1, wherein the liquid level in the sub-boiling distillation apparatus is 50% -80%, the pressure in the sub-boiling distillation apparatus is 38barG-39barG, and the updraft rate of the hydrogen chloride gas in the sub-boiling distillation apparatus is 3-6m/h.
3. The method for preparing high-purity halide wet electronic chemicals by using a sub-boiling distillation method according to claim 2, wherein hydrogen chloride gas which is not absorbed in the secondary falling film absorber is discharged and then enters the absorption tower, the hydrogen halide solution discharged from the bottom of the secondary falling film absorber enters the secondary absorption tank, and hydrogen halide in the absorption tank enters the top of the secondary falling film absorber as circulating absorption liquid through the secondary circulating pump.
4. The method for preparing high-purity wet electronic chemicals of halide by using a sub-boiling distillation process as claimed in claim 3, wherein the hydrogen halide solution discharged from the bottom of the absorption tower is introduced into the top of the absorption tower as a circulating absorption liquid through a three-stage circulating pump.
5. The method for preparing high purity halide wet electron chemical by the sub-boiling distillation as claimed in claim 1, wherein the hydrogen halide is hydrogen chloride, hydrogen fluoride or hydrogen bromide.
6. The method for preparing high-purity wet electronic chemicals of halide by using a sub-boiling distillation process according to claim 5, wherein the hydrogen halide is hydrogen chloride, the mass concentration of the electronic grade hydrogen chloride solution is 37%, and the content of impurity metal ions is not more than 10pp.
7. The method for preparing high-purity wet electronic chemicals of halide by using a sub-boiling distillation process according to claim 4, wherein a part of the hydrogen halide solution in the secondary absorption tank is circularly absorbed by the top of the secondary falling film absorber through the secondary circulating pump, and a part of the hydrogen halide solution is transferred to the primary absorption tank when the concentration of the hydrogen halide solution reaches 22-25%.
8. The method for preparing high-purity wet electronic chemicals of halide by using a sub-boiling distillation process as claimed in claim 7, wherein a part of the hydrogen halide solution discharged from the bottom of the absorption tower is introduced into the top of the absorption tower by a three-stage circulation pump, and when the circulating absorption concentration reaches 14-17%, a part of the hydrogen halide solution is transferred into the second-stage absorption tank.
9. The method for preparing high-purity halide wet electronic chemicals by using a sub-boiling distillation process according to claim 1, wherein the shell pass of the primary falling film absorber and the secondary falling film absorber is filled with cooling water at 7 ℃, and the absorption temperature of the primary falling film absorber and the secondary falling film absorber is lower than 20 ℃.
10. The method for preparing high purity halide wet electronic chemicals by using a sub-boiling distillation process as claimed in claim 1, wherein a cooler is provided after the circulating pump of the absorption tower.
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| CN202410506445.0A CN118183628A (en) | 2024-04-25 | 2024-04-25 | Method for preparing high-purity halide wet electronic chemicals by using sub-boiling distillation method |
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| CN202410506445.0A CN118183628A (en) | 2024-04-25 | 2024-04-25 | Method for preparing high-purity halide wet electronic chemicals by using sub-boiling distillation method |
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