CN106276799B - A kind of preparation method and device of electronic grade high-purity chlorine - Google Patents
A kind of preparation method and device of electronic grade high-purity chlorine Download PDFInfo
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- CN106276799B CN106276799B CN201610615012.4A CN201610615012A CN106276799B CN 106276799 B CN106276799 B CN 106276799B CN 201610615012 A CN201610615012 A CN 201610615012A CN 106276799 B CN106276799 B CN 106276799B
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- silicon tetrachloride
- reboiler
- extraction mouth
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- 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
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Abstract
The present invention relates to a kind of preparation method and device of electronic grade high-purity chlorine.Chlorine feed enters from dehydrating tower bottom of towe, silicon tetrachloride is added at the top of dehydrating tower, water reaction in silicon tetrachloride and chlorine feed is so as to by moisture removal, dehydration column overhead produces a small amount of light component, because silicon tetrachloride and water reaction are exothermic reaction, therefore a dehydrating tower tower reactor extraction part is returned in the middle part of dehydrating tower after centre takes reheater condenser to cool down, and another part enters silicon tetrachloride tower as raw material；The extraction of silicon tetrachloride column overhead gas phase enters segregator, liquid-phase reflux, and gas phase enters lightness-removing column as raw material, and tower reactor produces unreacted silicon tetrachloride.The extraction of lightness-removing column top gaseous phase enters segregator, liquid-phase reflux, and gas phase produces as light impurity, and tower reactor extraction enters chlorine tower as raw material.Chlorine column overhead produces the chlorine of purity >=99.9999%.Device is simple, it is easy to accomplish, substantially increase the economic benefit and social benefit of enterprise.
Description
Technical field
It is more particularly to a kind of using electrolytic chlorine gas as raw material essence the present invention relates to a kind of technology of preparing of electronic grade high-purity chlorine
Evaporate the method and device that purification prepares electronic grade high-purity chlorine.
Background technology
Electronic gas is microelectronics, the indispensable raw material of photoelectron, is to ensure that the most basic link of development in Hi-Tech.
From research to industrialized development, high-purity chlorine as important electronic gas will be sent out for the semiconductor in China, optical fiber industry in recent years
Wave important effect.Electron level purity of chlorine gas feeding requirement at present is more than 99.999%, because metal ion influences on optical fiber quality
It is very big, and moisture has a great influence to optical fiber hydroxy radical content, therefore electron level chlorine requires high to moisture, metal impurities.And
And chlorine has Strong oxdiative, the chemical property of deep-etching, in addition to a small number of rare gas, almost chemical combination can be formed with all elements
Thing, thus it is very high to equipment and technological requirement in preparation process.
Patent CN201310345584.1 proposes a kind of side that electronic grade high-purity chlorine is prepared using industrial liquid chlorine as raw material
Method, by removing nitrogen, oxygen through multistage physical dryness, adsorbing and removing carbon dioxide, compression condensation, rectifying after industrial liquid chlorine vaporizing
More than 99.999% electronic grade high-purity chlorine is made Deng low-boiling point gas.Patent CN201310362571.5 proposes a kind of height
Pure chlorine rectification process and equipment, high-purity chlorine of purity 99.9999% is prepared.But these techniques can not all avoid
Contour cost, high energy consumption step are condensed using adsorption dewatering, compressor compresses.
A kind of preparation technology of electronic grade high-purity chlorine of the present invention, absorbs the water in electrolytic chlorine gas using silicon tetrachloride,
Silicon tetrachloride and water reaction production silica and hydrogen chloride gas.The high-purity chlorine moisture-free prepared by the technique, institute
So that the sulfuric acid drying process of traditional handicraft can be cancelled, and compressor need not be used.
Patent of the present invention absorbs the water in electrolytic chlorine gas using silicon tetrachloride, passes through four towers using electrolytic chlorine gas as raw material
Continuous rectification apparatus, high-purity chlorine of purity >=99.9999%, and yield >=95% is prepared, and device is simple, is easy to real
It is existing, substantially increase the economic benefit and social benefit of enterprise.
The content of the invention
The preparation method and device of a kind of electronic grade high-purity chlorine proposed by the present invention；Using electrolytic chlorine gas as raw material, use
Silicon tetrachloride absorbs the water in electrolytic chlorine gas, and by four tower continuous rectification devices, the height of purity >=99.9999% is prepared
Pure chlorine, and yield >=96.8%, and device is simple, it is easy to accomplish, substantially increase the economic benefit and social benefit of enterprise.
To achieve the above object, the present invention is adopted the following technical scheme that to realize.
The inventive system comprises, including dehydrating tower, silicon tetrachloride tower, dehydrogenation tower, chlorine tower.It is characterized in that：Dehydrating tower
T101 bottoms are provided with raw material chlorine inlet, top silicon tetrachloride import, top gaseous phase extraction mouth, tower reactor extraction mouth and centre and take heat
Return port；Wherein hot cooler E101 and silicon tetrachloride tower T102 charging apertures, middle heat collector are taken among the connection of tower reactor extraction mouth
Hot return port is taken among E101 connections；Silicon tetrachloride tower T102 be provided with charging aperture, top gaseous phase extraction mouth, phegma return port,
Tower reactor produces mouth and reboiler return port, wherein top gaseous phase extraction mouth connection segregator E201, segregator E201 connections backflow
Liquid return port and lightness-removing column T103 charging apertures, tower reactor extraction mouth connection reboiler E202 imports, reboiler E202 connection reboilers
Return port；Lightness-removing column T103 is provided with charging aperture, top gaseous phase extraction mouth, phegma return port, tower reactor extraction mouth and reboiler and returned
Answer back, wherein top gaseous phase extraction mouth connection segregator E301, segregator E301 connection phegma return ports and weight-removing column T104
Charging aperture, tower reactor extraction mouth connection reboiler E302 imports, reboiler E302 connection reboiler return ports；Weight-removing column T104 is provided with
Charging aperture, top gaseous phase extraction mouth, phegma return port, tower reactor extraction mouth and reboiler return port, wherein top gaseous phase produce
Mouth connection condenser E401, condenser E401 connection phegma return port, tower reactor extraction mouth connection reboiler E402 imports, then boil
Device E402 connection reboiler return ports.
A kind of process of preparing of electronic grade high-purity chlorine, including by dehydrating tower, silicon tetrachloride tower, dehydrogenation tower, chlorine
The distillation system of tower composition, it is characterized in that chlorine feed enters from dehydrating tower T101 bottom of towe, tetrachloro is added at the top of dehydrating tower T101
SiClx, water reaction in silicon tetrachloride and chlorine feed is so as to by moisture removal, a small amount of light component of dehydrating tower T101 overhead extractions,
Because silicon tetrachloride and water reaction are exothermic reaction, therefore a dehydrating tower T101 tower reactors extraction part takes reheater condenser through centre
Returned after E101 coolings in the middle part of dehydrating tower T101, another part enters silicon tetrachloride tower T102 as raw material.Silicon tetrachloride tower
The extraction of T102 top gaseous phases enters segregator E201, liquid-phase reflux, and gas phase enters lightness-removing column T103 as raw material, and tower reactor produces not
The silicon tetrachloride of reaction.The extraction of lightness-removing column T103 top gaseous phases enters segregator E301, liquid-phase reflux, and gas phase is adopted as light impurity
Go out, tower reactor extraction enters chlorine tower T104 as raw material.The chlorine of chlorine tower T104 overhead extraction purity >=99.9999%, tower
Kettle produces heavy seeds.
Described tower can be that packed tower can also be plate column.
The present invention process conditions be preferably：
Dehydrating tower T101 operating pressures are 0.15-1MPa.
Silicon tetrachloride tower T102 operating pressures are 0.2-1MPa.
Lightness-removing column T103 operating pressures are 0.2-1MPa.
Chlorine tower T104 operating pressures are 0.2-1MPa.
The present invention uses four tower continuous rectification devices, and high-purity chlorine of purity >=99.9999% is prepared.
Brief description of the drawings
Fig. 1 is the preparation facilities schematic diagram of electronic grade high-purity chlorine；
T101 dehydrating towers, T102 silicon tetrachlorides tower, T103 lightness-removing columns, T104 chlorine tower, take among E101 hot cooler,
E201 dephlegmator of top of the tower, E202 tower reactor reboilers, E301 dephlegmator of top of the tower, E302 tower reactor reboilers, E401 dephlegmator of top of the tower,
E402 tower reactor reboilers.
Embodiment
Implementation is further described below in conjunction with accompanying drawing dehydrating tower T101 bottoms provided with chlorine feed import, on
Portion's silicon tetrachloride import, top gaseous phase extraction mouth, tower reactor extraction mouth and centre take hot return port；Wherein in the connection of tower reactor extraction mouth
Between take hot cooler E101 and silicon tetrachloride tower T102 charging apertures, takes hot return port among middle heat collector E101 connections；Tetrachloro
SiClx tower T102 is provided with charging aperture, top gaseous phase extraction mouth, phegma return port, tower reactor extraction mouth and reboiler return port, its
Middle top gaseous phase extraction mouth connection segregator E201, segregator E201 connection phegma return ports and lightness-removing column T103 charging apertures,
Tower reactor extraction mouth connection reboiler E202 imports, reboiler E202 connection reboiler return ports；Lightness-removing column T103 be provided with charging aperture,
Top gaseous phase extraction mouth, phegma return port, tower reactor extraction mouth and reboiler return port, wherein top gaseous phase extraction mouth connection point
Condenser E301, segregator E301 connection phegma return port and weight-removing column T104 charging apertures, tower reactor extraction mouth connection reboiler
E302 imports, reboiler E302 connection reboiler return ports；Weight-removing column T104 is provided with charging aperture, top gaseous phase extraction mouth, backflow
Liquid return port, tower reactor extraction mouth and reboiler return port, wherein top gaseous phase extraction mouth connection condenser E401, condenser E401
Connect phegma return port, tower reactor extraction mouth connection reboiler E402 imports, reboiler E402 connection reboiler return ports.
Chlorine feed enters from dehydrating tower T101 bottom of towe, and silicon tetrachloride, silicon tetrachloride and chlorine are added at the top of dehydrating tower T101
Water reaction in gas raw material is so as to by moisture removal, a small amount of light component of dehydrating tower T101 overhead extractions, due to silicon tetrachloride and water
React for exothermic reaction, therefore a dehydrating tower T101 tower reactors extraction part returns to dehydration after centre takes reheater condenser E101 to cool down
In the middle part of tower T101, another part enters silicon tetrachloride tower T102 as raw material.The extraction of silicon tetrachloride tower T102 top gaseous phases enters
Segregator E201, liquid-phase reflux, gas phase enter lightness-removing column T103 as raw material, and tower reactor produces unreacted silicon tetrachloride.It is de- light
The extraction of tower T103 top gaseous phases enters segregator E301, liquid-phase reflux, and gas phase produces as light impurity, and tower reactor extraction is used as raw material
Into chlorine tower T104.The chlorine of chlorine tower T104 overhead extraction purity >=99.9999%, tower reactor extraction heavy seeds.
Embodiment 1
Chlorine feed enters from dehydrating tower T101 bottom of towe, and silicon tetrachloride, silicon tetrachloride and chlorine are added at the top of dehydrating tower T101
Water reaction in gas raw material is so as to by moisture removal, a small amount of light component of dehydrating tower T101 overhead extractions, due to silicon tetrachloride and water
React for exothermic reaction, therefore a dehydrating tower T101 tower reactors extraction part returns to dehydration after centre takes reheater condenser E101 to cool down
In the middle part of tower T101, another part enters silicon tetrachloride tower T102 as raw material.The extraction of silicon tetrachloride tower T102 top gaseous phases enters
Segregator E201, liquid-phase reflux, gas phase enter lightness-removing column T103 as raw material, and tower reactor produces unreacted silicon tetrachloride.It is de- light
The extraction of tower T103 top gaseous phases enters segregator E301, liquid-phase reflux, and gas phase produces as light impurity, and tower reactor extraction is used as raw material
Into chlorine tower T104.The chlorine of chlorine tower T104 overhead extraction purity >=99.9999%, tower reactor extraction heavy seeds.
The number of theoretical plate of each tower, operating pressure are as follows：
The number of theoretical plate of T101 dehydrating towers is 5, operating pressure 1MPa；T102 silicon tetrachloride towers number of theoretical plate is 10, operation
Pressure 1MPa；T103 lightness-removing columns number of theoretical plate is 32, operating pressure 1MPa；T104 chlorine towers number of theoretical plate is 32, operation pressure
Power is 1MPa.
The chlorine of chlorine tower T104 overhead extraction purity >=99.9999%, and chlorine yield >=95%.
Embodiment 2
Chlorine feed enters from dehydrating tower T101 bottom of towe, and silicon tetrachloride, silicon tetrachloride and chlorine are added at the top of dehydrating tower T101
Water reaction in gas raw material is so as to by moisture removal, a small amount of light component of dehydrating tower T101 overhead extractions, due to silicon tetrachloride and water
React for exothermic reaction, therefore a dehydrating tower T101 tower reactors extraction part returns to dehydration after centre takes reheater condenser E101 to cool down
In the middle part of tower T101, another part enters silicon tetrachloride tower T102 as raw material.The extraction of silicon tetrachloride tower T102 top gaseous phases enters
Segregator E201, liquid-phase reflux, gas phase enter lightness-removing column T103 as raw material, and tower reactor produces unreacted silicon tetrachloride.It is de- light
The extraction of tower T103 top gaseous phases enters segregator E301, liquid-phase reflux, and gas phase produces as light impurity, and tower reactor extraction is used as raw material
Into chlorine tower T104.The chlorine of chlorine tower T104 overhead extraction purity >=99.9999%, tower reactor extraction heavy seeds.
The number of theoretical plate of each tower, operating pressure are as follows：
The number of theoretical plate of T101 dehydrating towers is 5, operating pressure 0.15MPa；T102 silicon tetrachloride towers number of theoretical plate is 10, behaviour
Make pressure 0.2MPa；T103 lightness-removing columns number of theoretical plate is 32, operating pressure 0.2MPa；T104 chlorine towers number of theoretical plate is 32,
Operating pressure is 0.2MPa.
The chlorine of chlorine tower T104 overhead extraction purity >=99.9999%, and chlorine yield >=95%.
Embodiment 2
Chlorine feed enters from dehydrating tower T101 bottom of towe, and silicon tetrachloride, silicon tetrachloride and chlorine are added at the top of dehydrating tower T101
Water reaction in gas raw material is so as to by moisture removal, a small amount of light component of dehydrating tower T101 overhead extractions, due to silicon tetrachloride and water
React for exothermic reaction, therefore a dehydrating tower T101 tower reactors extraction part returns to dehydration after centre takes reheater condenser E101 to cool down
In the middle part of tower T101, another part enters silicon tetrachloride tower T102 as raw material.The extraction of silicon tetrachloride tower T102 top gaseous phases enters
Segregator E201, liquid-phase reflux, gas phase enter lightness-removing column T103 as raw material, and tower reactor produces unreacted silicon tetrachloride.It is de- light
The extraction of tower T103 top gaseous phases enters segregator E301, liquid-phase reflux, and gas phase produces as light impurity, and tower reactor extraction is used as raw material
Into chlorine tower T104.The chlorine of chlorine tower T104 overhead extraction purity >=99.9999%, tower reactor extraction heavy seeds.
The number of theoretical plate of each tower, operating pressure are as follows：
The number of theoretical plate of T101 dehydrating towers is 5, operating pressure 0.5MPa；T102 silicon tetrachloride towers number of theoretical plate is 10, behaviour
Make pressure 0.5MPa；T103 lightness-removing columns number of theoretical plate is 32, operating pressure 0.5MPa；T104 chlorine towers number of theoretical plate is 32,
Operating pressure is 0.5MPa.
The chlorine of chlorine tower T104 overhead extraction purity >=99.9999%, and chlorine yield >=95%.
Claims (8)
1. a kind of preparation facilities of electronic grade high-purity chlorine, including be made up of dehydrating tower, silicon tetrachloride tower, dehydrogenation tower, chlorine tower
Distillation system, it is characterized in that chlorine feed enters from dehydrating tower T101 bottom of towe, add silicon tetrachloride at the top of dehydrating tower T101, four
Water reaction in silicon chloride and chlorine feed is so as to by moisture removal, a small amount of light component of dehydrating tower T101 overhead extractions, due to four
Silicon chloride is exothermic reaction with water reaction, therefore a dehydrating tower T101 tower reactors extraction part takes reheater condenser E101 to cool down through centre
Return afterwards in the middle part of dehydrating tower T101, another part enters silicon tetrachloride tower T102 as raw material；Silicon tetrachloride tower T102 tower overhead gases
Mutually extraction enters segregator E201, liquid-phase reflux, and gas phase enters lightness-removing column T103 as raw material, and tower reactor produces unreacted tetrachloro
SiClx；The extraction of lightness-removing column T103 top gaseous phases enters segregator E301, liquid-phase reflux, and gas phase is produced as light impurity, and tower reactor is adopted
Go out and enter chlorine tower T104 as raw material；Chlorine tower T104 overhead extraction chlorine, tower reactor extraction heavy seeds.
2. a kind of preparation method of electronic grade high-purity chlorine, it is characterized in that：Dehydrating tower T101 bottoms be provided with raw material chlorine inlet, on
Portion's silicon tetrachloride import, top gaseous phase extraction mouth, tower reactor extraction mouth and centre take hot return port；Wherein in the connection of tower reactor extraction mouth
Between take hot cooler E101 and silicon tetrachloride tower T102 charging apertures, takes hot return port among middle heat collector E101 connections；Tetrachloro
SiClx tower T102 is provided with charging aperture, top gaseous phase extraction mouth, phegma return port, tower reactor extraction mouth and reboiler return port, its
Middle top gaseous phase extraction mouth connection segregator E201, segregator E201 connection phegma return ports and lightness-removing column T103 charging apertures,
Tower reactor extraction mouth connection reboiler E202 imports, reboiler E202 connection reboiler return ports；Lightness-removing column T103 be provided with charging aperture,
Top gaseous phase extraction mouth, phegma return port, tower reactor extraction mouth and reboiler return port, wherein top gaseous phase extraction mouth connection point
Condenser E301, segregator E301 connection phegma return port and weight-removing column T104 charging apertures, tower reactor extraction mouth connection reboiler
E302 imports, reboiler E302 connection reboiler return ports；Weight-removing column T104 is provided with charging aperture, top gaseous phase extraction mouth, backflow
Liquid return port, tower reactor extraction mouth and reboiler return port, wherein top gaseous phase extraction mouth connection condenser E401, condenser E401
Connect phegma return port, tower reactor extraction mouth connection reboiler E402 imports, reboiler E402 connection reboiler return ports.
3. method as claimed in claim 2, it is characterized in that dehydrating tower T101 operating pressures are 0.15-1MPa.
4. method as claimed in claim 2, it is characterized in that silicon tetrachloride tower T102 operating pressures are 0.2-1MPa.
5. method as claimed in claim 2, it is characterized in that lightness-removing column T103 operating pressures are 0.2-1MPa.
6. method as claimed in claim 2, it is characterized in that chlorine tower T104 operating pressures are 0.2-1MPa.
7. method as claimed in claim 2, it is characterized in that dehydrating tower, silicon tetrachloride tower, the tower of dehydrogenation tower or chlorine tower
It is packed tower or plate column.
8. method as claimed in claim 2, it is characterized in that purity >=99.9999% of high-purity chlorine is prepared.
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| CN201610615012.4A CN106276799B (en) | 2016-07-26 | 2016-07-26 | A kind of preparation method and device of electronic grade high-purity chlorine |
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| CN201610615012.4A CN106276799B (en) | 2016-07-26 | 2016-07-26 | A kind of preparation method and device of electronic grade high-purity chlorine |
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| CN106276799B true CN106276799B (en) | 2018-02-09 |
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| CN110683513B (en) * | 2019-11-12 | 2021-01-05 | 浙江博瑞电子科技有限公司 | Preparation method of high-purity chlorine |
| CN112777568B (en) * | 2021-02-22 | 2022-10-14 | 北京华宇同方化工科技开发有限公司 | System and method for jointly producing electronic chlorine and electronic hydrogen chloride |
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| CN103626129B (en) * | 2013-08-09 | 2016-03-02 | 杭州电化集团有限公司 | With industrial liquid chlorine for the method for electronic grade high-purity chlorine prepared by raw material |
| CN105510503A (en) * | 2015-12-31 | 2016-04-20 | 上海正帆科技股份有限公司 | Analysis device and method of electronic-grade chlorine gas |
| CN105731379A (en) * | 2015-12-31 | 2016-07-06 | 上海正帆科技股份有限公司 | Purifying method of electronic grade chlorine |
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