CN110526213A - A kind of hydrogen bromide purification process - Google Patents
A kind of hydrogen bromide purification process Download PDFInfo
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- CN110526213A CN110526213A CN201910971972.8A CN201910971972A CN110526213A CN 110526213 A CN110526213 A CN 110526213A CN 201910971972 A CN201910971972 A CN 201910971972A CN 110526213 A CN110526213 A CN 110526213A
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- hydrogen bromide
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- purification process
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- CPELXLSAUQHCOX-UHFFFAOYSA-N Hydrogen bromide Chemical compound Br CPELXLSAUQHCOX-UHFFFAOYSA-N 0.000 title claims abstract description 175
- 229910000042 hydrogen bromide Inorganic materials 0.000 title claims abstract description 87
- 238000000746 purification Methods 0.000 title claims abstract description 32
- 238000004821 distillation Methods 0.000 claims abstract description 32
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 30
- 239000001257 hydrogen Substances 0.000 claims abstract description 30
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 29
- 230000031709 bromination Effects 0.000 claims abstract description 28
- 238000005893 bromination reaction Methods 0.000 claims abstract description 28
- 238000004519 manufacturing process Methods 0.000 claims abstract description 22
- 239000000463 material Substances 0.000 claims abstract description 17
- 239000000470 constituent Substances 0.000 claims abstract description 14
- 229920000557 Nafion® Polymers 0.000 claims abstract description 10
- 230000008016 vaporization Effects 0.000 claims abstract description 8
- 238000003860 storage Methods 0.000 claims abstract description 7
- 238000009834 vaporization Methods 0.000 claims abstract description 6
- 229910000831 Steel Inorganic materials 0.000 claims description 36
- 239000010959 steel Substances 0.000 claims description 36
- 239000007789 gas Substances 0.000 claims description 22
- 238000009413 insulation Methods 0.000 claims description 21
- 230000005484 gravity Effects 0.000 claims description 9
- 239000007788 liquid Substances 0.000 claims description 9
- 239000003513 alkali Substances 0.000 claims description 7
- 238000004140 cleaning Methods 0.000 claims description 7
- 238000005406 washing Methods 0.000 claims description 6
- 238000007599 discharging Methods 0.000 claims description 5
- 239000012535 impurity Substances 0.000 claims description 5
- 238000005201 scrubbing Methods 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 18
- 230000008569 process Effects 0.000 abstract description 6
- 229910045601 alloy Inorganic materials 0.000 abstract description 5
- 239000000956 alloy Substances 0.000 abstract description 5
- 230000007246 mechanism Effects 0.000 description 9
- 239000000126 substance Substances 0.000 description 7
- 238000009835 boiling Methods 0.000 description 6
- 239000002994 raw material Substances 0.000 description 6
- 238000001816 cooling Methods 0.000 description 5
- 238000010438 heat treatment Methods 0.000 description 5
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 4
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 239000002585 base Substances 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 238000005530 etching Methods 0.000 description 3
- 239000007791 liquid phase Substances 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- WKBOTKDWSSQWDR-UHFFFAOYSA-N Bromine atom Chemical compound [Br] WKBOTKDWSSQWDR-UHFFFAOYSA-N 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 239000003463 adsorbent Substances 0.000 description 2
- GDTBXPJZTBHREO-UHFFFAOYSA-N bromine Substances BrBr GDTBXPJZTBHREO-UHFFFAOYSA-N 0.000 description 2
- 229910052794 bromium Inorganic materials 0.000 description 2
- 239000000356 contaminant Substances 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000007710 freezing Methods 0.000 description 2
- 230000008014 freezing Effects 0.000 description 2
- 238000011031 large-scale manufacturing process Methods 0.000 description 2
- AMXOYNBUYSYVKV-UHFFFAOYSA-M lithium bromide Chemical compound [Li+].[Br-] AMXOYNBUYSYVKV-UHFFFAOYSA-M 0.000 description 2
- 239000002808 molecular sieve Substances 0.000 description 2
- 229910052759 nickel Inorganic materials 0.000 description 2
- 239000013618 particulate matter Substances 0.000 description 2
- 229910021420 polycrystalline silicon Inorganic materials 0.000 description 2
- 229920005591 polysilicon Polymers 0.000 description 2
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 2
- 239000004810 polytetrafluoroethylene Substances 0.000 description 2
- 239000003507 refrigerant Substances 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 239000000741 silica gel Substances 0.000 description 2
- 229910002027 silica gel Inorganic materials 0.000 description 2
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- CPELXLSAUQHCOX-UHFFFAOYSA-M Bromide Chemical compound [Br-] CPELXLSAUQHCOX-UHFFFAOYSA-M 0.000 description 1
- PHSPJQZRQAJPPF-UHFFFAOYSA-N N-alpha-Methylhistamine Chemical compound CNCCC1=CN=CN1 PHSPJQZRQAJPPF-UHFFFAOYSA-N 0.000 description 1
- 239000004809 Teflon Substances 0.000 description 1
- 229920006362 Teflon® Polymers 0.000 description 1
- PRPAGESBURMWTI-UHFFFAOYSA-N [C].[F] Chemical compound [C].[F] PRPAGESBURMWTI-UHFFFAOYSA-N 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 230000003749 cleanliness Effects 0.000 description 1
- 229920001577 copolymer Polymers 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 239000002274 desiccant Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005429 filling process Methods 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 229910001509 metal bromide Inorganic materials 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 229910021421 monocrystalline silicon Inorganic materials 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 238000001020 plasma etching Methods 0.000 description 1
- -1 polytetrafluoroethylene Polymers 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 230000000452 restraining effect Effects 0.000 description 1
- AIFMYMZGQVTROK-UHFFFAOYSA-N silicon tetrabromide Chemical compound Br[Si](Br)(Br)Br AIFMYMZGQVTROK-UHFFFAOYSA-N 0.000 description 1
- 239000006200 vaporizer Substances 0.000 description 1
- 239000010457 zeolite Substances 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
- C01B7/09—Bromine; Hydrogen bromide
- C01B7/093—Hydrogen bromide
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Drying Of Gases (AREA)
Abstract
The invention discloses a kind of hydrogen bromide purification process, include the following steps: hydrogen bromide carrying out part vaporization；Hydrogen bromide after vaporization enters Nafion drier, and depth removes the moisture in hydrogen bromide；Bromination hydrogen after removing moisture removal enters de-light rectification column；The hydrogen bromide for removing light component enters de- heavy distillation column, removes the heavy constituent in hydrogen bromide；The hydrogen bromide for removing heavy constituent discharges from the tower top of de- heavy distillation column, into hydrogen bromide storage unit, obtains electron level bromination hydrogen production.The present invention while moisture removed in hydrogen bromide being simple and efficient, does not need to greatly reduce equipment investment using materials such as 316L using the precious materials process equipment such as nickel-base alloy under the use of novel drier.
Description
Technical field
The present invention relates to gas purification fields, and in particular to a kind of hydrogen bromide purification process.
Background technique
High-purity hydrogen bromide (HBr) is for the N-shaped polysilicon of semiconductor p-doped, the monocrystalline silicon of p-doped or two-dimensional semiconductor
Etching, is the first choice of fluorine carbon gas instead product.It can pass through using hydrogen bromide as the plasma etching technology of etching gas
The temperature for controlling the substance that is etched, which reaches, accurately controls the taper etch of vertical etch or the coning angle for having setting.Therefore, high
Pure electron level HBr is mainly used for the etching polysilicon in 8 cun and 12 cun of chip manufacturing process, is the core gas of chip advanced process
One of body.Furthermore hydrogen bromide is widely used due to having the ability as catalyst or reactant.It is pure in bromination hydrogen
The problem of being most difficult to during changing is how to remove moisture therein, and moisture content is high, extremely strong to metallic material corrosion, while also
Foreign gas is generated, product purity is influenced, this also becomes the most important restraining factors of high-purity bromination hydrogen preparation.Typically now
Purification or dry common method to hydrogen bromide have freezing separation method, physisorphtion and chemical de-moisture method.Freezing separation, but
Energy consumption is high, is difficult to control, industrial production has little significance.Physisorphtion, adsorbent include molecular sieve, silica gel, activated alumina
Deng.Such as Matheson TRI Gas, Inc patent WO00/20101 (using the method for the water in superheated zeolites removal gas), Pu Lai
Ke Si Technology Co., Ltd. patent WO2003/027581 (method and apparatus of purification hydrogen bromide), uses molecular sieve, silica gel, work
Property the adsorbents such as aluminium oxide purify hydrogen bromide, easily part reaction and heat release, when especially water content is higher, while causing part bromine
Change hydrogen loss, absorption method uses in the case that preferably moisture content is low in hydrogen bromide.Chemical de-moisture method, using to steam ten
Divide sensitive or is easily reacted with water electrode but do not pass through chemical reaction dehydration with the substance of reaction of hydrogen bromide.Such as the bright chemical research of middle sky
Co., Ltd, designing institute patent CN103318843 A (a kind of method of drying hydrogen bromide), these chemicals generally include
Silicon bromide, phosphorus tribromide, lithium bromide etc., these chemical attacks are active, are to be difficult to control in large-scale production process, there are larger
Security risk, be not suitable for so large-scale production.The production technology of hydrogen bromide has much room for improvement under industrial condition.
It essentially reacts, adsorb in existing hydrogen bromide purifying process, the way of purification such as rectifying.Teisan K.K. patent CN
1138314A prepares the method and apparatus of high purity hydrogen bromide, purifies the hydrogen bromide containing low boiling impurity, does not solve to remove
The scheme of weight boiling contaminants, especially water in hydrogen bromide.107352511 A (bromination of Lv Ling Electron Material Co., Ltd patent CN
Hydrogen purifying technique), hydrogen bromide is purified by the method for rectifying plus absorption and obtains electron level hydrogen bromide, but uses nickel in rectifier unit
Based alloy etc., equipment investment is excessive, while aqueous bromination hydrogen is also to have corrosion to nickel-base alloy, corrodes to pure nickel outstanding
Very, filling process is that heating pressurization fills, and the use of heating equipment, there are some potential safety problemss, propose more to safety
High requirement.
Summary of the invention
The object of the present invention is to provide a kind of hydrogen bromide purification process, under the use of novel drier, are being simple and efficient
Removal hydrogen bromide in moisture while, do not need to greatly reduce and set using the precious materials process equipment such as nickel-base alloy
Standby investment.
In order to achieve the above objectives, the technical solution adopted by the present invention is that: a kind of hydrogen bromide purification process, including walk as follows
It is rapid:
(1) hydrogen bromide is subjected to part vaporization, vapourizing temperature is controlled at 0 DEG C to 30 DEG C；
(2) hydrogen bromide after vaporizing enters Nafion drier, and depth removes the moisture in hydrogen bromide；
(3) the bromination hydrogen after removing moisture removal enters de-light rectification column from the middle and upper part of de-light rectification column, takes off light rectifying
At -18 DEG C to 10 DEG C, the voltage-controlled system of the tower of de-light rectification column removes in hydrogen bromide in 0.7MPa to 1.8MPa for the tower temperature control of tower
Light component；
(4) hydrogen bromide for removing light component discharges from the tower bottom of de-light rectification column, enters from the middle and lower part of de- heavy distillation column
De- heavy distillation column, the tower temperature for taking off heavy distillation column control taken off at -18 DEG C to 10 DEG C the voltage-controlled system of tower of heavy distillation column 0.65MPa extremely
1.75MPa removes the heavy constituent in hydrogen bromide；
(5) hydrogen bromide for removing heavy constituent discharges from the tower top of de- heavy distillation column, into hydrogen bromide storage unit, obtains electricity
Sub- grade bromination hydrogen production.
Further, in step (1), hydrogen bromide steel cylinder partially vaporizes after being heated.
Further, in step (2), the moisture in hydrogen bromide is reduced to 10ppb or less by Nafion drier.
Further, in step (3), -25 DEG C to -30 DEG C of the overhead condenser temperature of de-light rectification column is condensed out
Light component generates motive force through gravity and the temperature difference, receives steel cylinder into lighter component, the quality of light component be rectifying material 1/5 to
1/12, in step (4), the tower reactor of de- heavy distillation column, which produces motive force through pressure difference gravity and the temperature difference, stablizes the tower reactor of de- heavy distillation column
Discharging to heavy component receives steel cylinder, and the quality of heavy constituent is the 1/5 to 1/12 of rectifying material, in step (5), takes off heavy distillation column
Overhead condenser temperature is -25 DEG C to -30 DEG C, and the product condensed out generates motive force through gravity and the temperature difference, into hydrogen bromide
Storage unit, obtains electron level bromination hydrogen production, and the total impurities of electron level bromination hydrogen production are less than 5ppm.
Further, in step (3), light component receives steel cylinder and carries out cold insulation processing, -25 DEG C to -30 DEG C of cold insulation temperature, walks
Suddenly in (5), the progress cold insulation processing of bromination hydrogen production steel cylinder, -25 DEG C to -30 DEG C of cold insulation temperature.
Further, in step (3), the tower top on-condensible gas of de-light rectification column enters alkali liquid washing tower, after cleaning of off-gas
It is vented, in step (5), the tower top on-condensible gas of de- heavy distillation column enters alkali liquid washing tower, is vented after cleaning of off-gas.
Further, in step (3), the quality of light component is the 1/7 to 1/10 of rectifying material, in step (4), heavy constituent
Quality be rectifying material 1/7 to 1/10.
Further, all pipelines use EP grades of clean pipes.
Further, the tower pressure of de-light rectification column is higher than the tower pressure of de- heavy distillation column.
Further, hydrogen bromide storage unit is hydrogen bromide steel cylinder.
Due to the above technical solutions, the present invention has the following advantages over the prior art:
1) hydrogen bromide purification process disclosed by the invention, under the use of novel drier, in the removal bromine being simple and efficient
While changing the moisture in hydrogen, do not need using the precious materials process equipment such as nickel-base alloy, using materials such as 316L, greatly
Equipment investment is reduced greatly；
2) hydrogen bromide purification process disclosed by the invention, is filled by low temperature, improves the safety filled；
3) hydrogen bromide purification process disclosed by the invention, it is contemplated that the cleanliness of electron level hydrogen bromide, pipeline use EP grades
Cleaning pipe, it is ensured that product quality.
4) hydrogen bromide purification process disclosed by the invention carries out de-light rectification column by pressure difference and feeds to de- heavy distillation column,
Without also subtracting on the basis of reducing equipment simultaneously using dynamic equipment such as pump or compressors in the purification system of entire hydrogen bromide
The low contaminated probability of hydrogen bromide, improves the operability and stability of technique；
5) hydrogen bromide purification process disclosed by the invention, is applied in combination by de-light rectification column and de- heavy distillation column, is taken off light
Tower removes H2、N2、CO、Ar、O2、CH4、C2H6、HCl、CO2Equal low boiling impurities, weight-removing column remove H2S、HI、H2The heavy components such as O,
Also metal bromide, solid particulate matter etc. are removed simultaneously, weight-removing column tower top obtains bromination hydrogen production；
6) hydrogen bromide purification process disclosed by the invention, select -25 to -30 degrees Celsius between refrigerant, avoid using at
The refrigerants such as this higher liquid nitrogen, also lower the requirement to equipment material, reduce the cost；
7) hydrogen bromide purification process disclosed by the invention produces the hydrogen bromide of a small amount of production capacity, directly hydrogen bromide original
Expect that steel cylinder is used when head tank, reduces equipment investment；Such as the device of the larger demand of production capacity, vaporizer is installed additional after device.
Detailed description of the invention
Fig. 1 is the composition schematic diagram of bromination hydrogen purification devices disclosed by the invention.
Wherein, 11, hydrogen bromide raw material steel cylinder；12, heating blanket；21, Nafion drier；31, de-light rectification column；32, it takes off
Heavy distillation column；33, light component receives steel cylinder；34, the second cold insulation mechanism；35, heavy constituent receives steel cylinder；36, third cold insulation mechanism；
41, bromination hydrogen production steel cylinder；42, the first cold insulation mechanism.
Specific embodiment
In conjunction with accompanying drawings and embodiments, the invention will be further described:
Referring to Fig. 1, as shown in legend therein, a kind of bromination hydrogen purification devices, comprising:
Raw material feed unit comprising two hydrogen bromide raw material steel cylinders 11, the outside of every hydrogen bromide raw material steel cylinder 11 are set
There is heating blanket 12；
Drying unit comprising Nafion drier 21, the feed inlet and hydrogen bromide raw material steel cylinder of Nafion drier 21
11 outlet connection, desiccant use polytetrafluoroethylene (PTFE) (Teflon) and perfluor -3,6- diepoxy -4- methyl -7- decene-sulfuric acid
Copolymer；
Rectification cell comprising de-light rectification column 31 and de- heavy distillation column 32, the middle and upper part feed inlet of de-light rectification column 31
It is connect with the discharge port of Nafion drier 21, the middle and lower part feed inlet of de- heavy distillation column 32 and the tower bottom of de-light rectification column 31 go out
Material mouth connection, the liquid-phase outlet of the overhead condenser of de-light rectification column 31 receive steel cylinder 33 with light component and connect, and light component receives
The outside of steel cylinder 33 is equipped with the second cold insulation mechanism 34, and the second cold insulation mechanism 34 includes surrounding light component to receive the second cold of steel cylinder 33
But pipe and the second muff on the outside of the second cooling tube, the liquid-phase outlet and heavy constituent for taking off the tower reactor of heavy distillation column 32 receive
Steel cylinder 35 connects, and the outside that every heavy constituent receives steel cylinder 35 is equipped with third cold insulation mechanism 36, and third cold insulation mechanism 36 includes ring
The third cooling tube and the third muff on the outside of third cooling tube for receiving steel cylinder 35 around heavy constituent, de-light rectification column 31
The incoagulable gas of overhead condenser exports and the fixed gas gas vent of the overhead condenser of de- heavy distillation column 32 is separately connected
To the entrance of alkali liquid washing tower 37；
Product receiving unit, including two bromination hydrogen production steel cylinders 41, bromination hydrogen production steel cylinder 41 and de- heavy distillation column 32
Overhead condenser liquid-phase outlet connection, the outside of every bromination hydrogen production steel cylinder 41 is equipped with the first cold insulation mechanism 42, first
Cold insulation mechanism 42 includes surrounding the first cooling tube of bromination hydrogen production steel cylinder 41 and the first heat preservation on the outside of the first cooling tube
Set.
Preferred embodiment in this implementation, all pipelines use EP grades of clean pipes.
It is below hydrogen bromide purification process, hydrogen bromide raw material steel cylinder carries out heating and carries out part vaporization, controls vapourizing temperature
It is 10 degrees Celsius；Gas enters Nafion drier after vaporization, and depth removes moisture in hydrogen bromide；Bromination hydrogen after purification
It into de-light rectification column, is fed from the middle and upper part of tower, the control of tower temperature degree is at 10 degrees Celsius, and for the voltage-controlled system of tower in 1.73MPa, tower top is cold
- 25 to -30 degrees Celsius of condenser temperature, when de-light rectification column rectifying, removes H2、N2、CO、Ar、O2、CH4、C2H6、HCl、CO2Etc. low
Boiling contaminants, the quality of low boiling component are rectifying material 1/10, and the lighter component condensed out generates promotion through gravity and the temperature difference
Power receives steel cylinder into lighter component, and lighter component receives steel cylinder and carries out cold insulation processing, -25 degrees Celsius of cold insulation temperature.De-light rectification column
Tower top on-condensible gas enter alkali liquid washing tower, be vented after cleaning of off-gas.Heavy distillation column is taken off in the tower bottom discharging of de-light rectification column,
It is fed from the middle and lower part of tower, the control of tower temperature degree is at 0 degree Celsius, and for the voltage-controlled system of tower in 1.28MPa, overhead condenser temperature -25 is Celsius
Degree takes off hydrogen bromide liquid of the heavy distillation column tower reactor discharging containing heavy component, removes the heavy components such as H2S, HI, H2O, also remove gold simultaneously
Belong to bromide, solid particulate matter etc.；The quality of weight boiling point component is rectifying material 1/10, and tower reactor is generated through pressure difference gravity and the temperature difference
The discharging that motive force keeps the tower reactor of de- heavy distillation column stable to heavy component receives steel cylinder, -25 degrees Celsius of overhead condenser temperature, tower
It pushes up the product condensed out and generates motive force through gravity and the temperature difference, into bromination hydrogen production steel cylinder, obtain the production of electron level hydrogen bromide
Product, total impurities are less than 5ppm, and bromination hydrogen production steel cylinder carries out cold insulation processing, -25 degrees Celsius of cold insulation temperature.De- heavy distillation column
Tower top on-condensible gas enters alkali liquid washing tower, is vented after cleaning of off-gas.
The foregoing description of the disclosed embodiments enables those skilled in the art to implement or use the present invention.
Various modifications to these embodiments will be readily apparent to those skilled in the art, as defined herein
General Principle can be realized in other embodiments without departing from the spirit or scope of the present invention.Therefore, of the invention
It is not intended to be limited to the embodiments shown herein, and is to fit to and the principles and novel features disclosed herein phase one
The widest scope of cause.
Claims (10)
1. a kind of hydrogen bromide purification process, which comprises the steps of:
(1) hydrogen bromide is subjected to part vaporization, vapourizing temperature is controlled at 0 DEG C to 30 DEG C；
(2) hydrogen bromide after vaporizing enters Nafion drier, and depth removes the moisture in hydrogen bromide；
(3) the bromination hydrogen after removing moisture removal enters de-light rectification column from the middle and upper part of de-light rectification column, de-light rectification column
At -18 DEG C to 10 DEG C, the voltage-controlled system of the tower of de-light rectification column removes light group in hydrogen bromide in 0.7MPa to 1.8MPa for tower temperature control
Point；
(4) hydrogen bromide for removing light component discharges from the tower bottom of de-light rectification column, enters de- weight from the middle and lower part of de- heavy distillation column
Rectifying column, take off heavy distillation column tower temperature control at -18 DEG C to 10 DEG C, take off heavy distillation column tower it is voltage-controlled system 0.65MPa extremely
1.75MPa removes the heavy constituent in hydrogen bromide；
(5) hydrogen bromide for removing heavy constituent discharges from the tower top of de- heavy distillation column, into hydrogen bromide storage unit, obtains electron level
Bromination hydrogen production.
2. hydrogen bromide purification process as described in claim 1, which is characterized in that in step (1), hydrogen bromide steel cylinder is heated
Part vaporizes afterwards.
3. hydrogen bromide purification process as described in claim 1, which is characterized in that in step (2), Nafion drier is by bromination
Moisture in hydrogen is reduced to 10ppb or less.
4. hydrogen bromide purification process as described in claim 1, which is characterized in that in step (3), the tower top of de-light rectification column is cold
- 25 DEG C to -30 DEG C of condenser temperature, the light component condensed out generates motive force through gravity and the temperature difference, receives steel into lighter component
Bottle, the quality of light component are the 1/5 to 1/12 of rectifying material, in step (4), take off the tower reactor of heavy distillation column through pressure difference gravity and temperature
Difference, which produces motive force, makes the stable discharging of the tower reactor of de- heavy distillation column to heavy component receive steel cylinder, and the quality of heavy constituent is rectifying material
1/5 to 1/12, in step (5), the overhead condenser temperature for taking off heavy distillation column is -25 DEG C to -30 DEG C, and the product condensed out passes through
Gravity and the temperature difference generate motive force and obtain electron level bromination hydrogen production, electron level bromination hydrogen production into hydrogen bromide storage unit
Total impurities be less than 5ppm.
5. hydrogen bromide purification process as claimed in claim 4, which is characterized in that in step (3), light component receives steel cylinder and carries out
Cold insulation processing, -25 DEG C to -30 DEG C of cold insulation temperature, in step (5), the progress cold insulation processing of bromination hydrogen production steel cylinder, cold insulation temperature -
25 DEG C to -30 DEG C.
6. hydrogen bromide purification process as claimed in claim 4, which is characterized in that in step (3), the tower top of de-light rectification column is not
Solidifying gas enters alkali liquid washing tower, is vented after cleaning of off-gas, and in step (5), the tower top on-condensible gas of de- heavy distillation column enters alkali
Liquid scrubbing tower is vented after cleaning of off-gas.
7. hydrogen bromide purification process as claimed in claim 4, which is characterized in that in step (3), the quality of light component is rectifying
The 1/7 to 1/10 of material, in step (4), the quality of heavy constituent is the 1/7 to 1/10 of rectifying material.
8. hydrogen bromide purification process as described in claim 1, which is characterized in that all pipelines use EP grades of clean pipes.
9. hydrogen bromide purification process as described in claim 1, which is characterized in that the tower pressure of de-light rectification column is higher than de- rectifying again
The tower pressure of tower.
10. hydrogen bromide purification process as described in claim 1, which is characterized in that hydrogen bromide storage unit is hydrogen bromide steel cylinder.
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| CN201910971972.8A CN110526213A (en) | 2019-10-14 | 2019-10-14 | A kind of hydrogen bromide purification process |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110980648A (en) * | 2019-12-31 | 2020-04-10 | 中船重工（邯郸）派瑞特种气体有限公司 | Hydrogen bromide purification device and method |
| CN112661114A (en) * | 2020-12-22 | 2021-04-16 | 福建久策气体股份有限公司 | Electronic grade hydrogen bromide rectifying and purifying method |
| CN112938899A (en) * | 2021-02-26 | 2021-06-11 | 绿菱电子材料（天津）有限公司 | Purification method of high-purity electronic grade hydrogen bromide |
| CN113247863A (en) * | 2021-06-11 | 2021-08-13 | 浙江陶特容器科技股份有限公司 | Preparation method of electronic grade hydrogen bromide gas and application of electronic grade hydrogen bromide gas in etching of polycrystalline silicon grid |
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| CN118480204A (en) * | 2024-04-18 | 2024-08-13 | 浙江陶特容器科技股份有限公司 | Hydrogen bromide deep water removal material and preparation method thereof |
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| CN110980648A (en) * | 2019-12-31 | 2020-04-10 | 中船重工（邯郸）派瑞特种气体有限公司 | Hydrogen bromide purification device and method |
| CN112661114A (en) * | 2020-12-22 | 2021-04-16 | 福建久策气体股份有限公司 | Electronic grade hydrogen bromide rectifying and purifying method |
| CN112938899A (en) * | 2021-02-26 | 2021-06-11 | 绿菱电子材料（天津）有限公司 | Purification method of high-purity electronic grade hydrogen bromide |
| CN113247863A (en) * | 2021-06-11 | 2021-08-13 | 浙江陶特容器科技股份有限公司 | Preparation method of electronic grade hydrogen bromide gas and application of electronic grade hydrogen bromide gas in etching of polycrystalline silicon grid |
| CN114195098A (en) * | 2022-01-06 | 2022-03-18 | 新地能源工程技术有限公司 | Electronic grade hydrogen bromide preparation device and process |
| CN118480204A (en) * | 2024-04-18 | 2024-08-13 | 浙江陶特容器科技股份有限公司 | Hydrogen bromide deep water removal material and preparation method thereof |
| CN118480204B (en) * | 2024-04-18 | 2024-10-25 | 浙江陶特容器科技股份有限公司 | Hydrogen bromide deep water removal material and preparation method thereof |
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