CN112707372A - Method for removing water in hydrogen chloride by using thionyl chloride - Google Patents
Method for removing water in hydrogen chloride by using thionyl chloride Download PDFInfo
- Publication number
- CN112707372A CN112707372A CN202011466961.3A CN202011466961A CN112707372A CN 112707372 A CN112707372 A CN 112707372A CN 202011466961 A CN202011466961 A CN 202011466961A CN 112707372 A CN112707372 A CN 112707372A
- Authority
- CN
- China
- Prior art keywords
- hydrogen chloride
- chloride
- rectifying
- thionyl chloride
- sulfur dioxide
- Prior art date
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- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 title claims abstract description 74
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 title claims abstract description 67
- 229910000041 hydrogen chloride Inorganic materials 0.000 title claims abstract description 67
- FYSNRJHAOHDILO-UHFFFAOYSA-N thionyl chloride Chemical compound ClS(Cl)=O FYSNRJHAOHDILO-UHFFFAOYSA-N 0.000 title claims abstract description 60
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 32
- 238000000034 method Methods 0.000 title claims abstract description 24
- RAHZWNYVWXNFOC-UHFFFAOYSA-N Sulphur dioxide Chemical compound O=S=O RAHZWNYVWXNFOC-UHFFFAOYSA-N 0.000 claims abstract description 52
- 239000007789 gas Substances 0.000 claims abstract description 22
- 238000006243 chemical reaction Methods 0.000 claims abstract description 21
- 238000003795 desorption Methods 0.000 claims description 18
- 239000007788 liquid Substances 0.000 claims description 12
- 238000010521 absorption reaction Methods 0.000 claims description 6
- 238000000926 separation method Methods 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 5
- 238000007599 discharging Methods 0.000 claims description 5
- 239000012535 impurity Substances 0.000 abstract description 5
- 230000007797 corrosion Effects 0.000 abstract description 3
- 238000005260 corrosion Methods 0.000 abstract description 3
- 230000000694 effects Effects 0.000 abstract description 3
- 229910052751 metal Inorganic materials 0.000 abstract description 3
- 239000002184 metal Substances 0.000 abstract description 3
- 238000003889 chemical engineering Methods 0.000 abstract description 2
- 239000012847 fine chemical Substances 0.000 abstract description 2
- 230000018044 dehydration Effects 0.000 description 8
- 238000006297 dehydration reaction Methods 0.000 description 8
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 7
- 229910052731 fluorine Inorganic materials 0.000 description 7
- 239000011737 fluorine Substances 0.000 description 7
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 5
- 238000001179 sorption measurement Methods 0.000 description 4
- 238000005530 etching Methods 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- SYNPRNNJJLRHTI-UHFFFAOYSA-N 2-(hydroxymethyl)butane-1,4-diol Chemical compound OCCC(CO)CO SYNPRNNJJLRHTI-UHFFFAOYSA-N 0.000 description 1
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 1
- 229910006124 SOCl2 Inorganic materials 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000003905 agrochemical Substances 0.000 description 1
- 238000005804 alkylation reaction Methods 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000003518 caustics Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 150000002221 fluorine Chemical class 0.000 description 1
- 150000002222 fluorine compounds Chemical class 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 229910000040 hydrogen fluoride Inorganic materials 0.000 description 1
- ORUIBWPALBXDOA-UHFFFAOYSA-L magnesium fluoride Chemical compound [F-].[F-].[Mg+2] ORUIBWPALBXDOA-UHFFFAOYSA-L 0.000 description 1
- 229910001635 magnesium fluoride Inorganic materials 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000002808 molecular sieve Substances 0.000 description 1
- 238000005554 pickling Methods 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 238000010926 purge Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000003507 refrigerant Substances 0.000 description 1
- 238000005057 refrigeration Methods 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 230000000717 retained effect Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 1
- 239000000126 substance 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
- C01B7/01—Chlorine; Hydrogen chloride
- C01B7/07—Purification ; Separation
- C01B7/0706—Purification ; Separation of hydrogen chloride
-
- 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
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The invention relates to a method for removing water in hydrogen chloride by using thionyl chloride, belonging to the technical field of fine chemical engineering. Adding thionyl chloride into hydrogen chloride enriched with water, reacting for 3-5 hours at-20-50 ℃ and-0.1-2 MPa to obtain a mixed gas of the hydrogen chloride and sulfur dioxide; and after the reaction is finished, rectifying the mixed gas to obtain dehydrated hydrogen chloride. The method has good water removal effect, impurities generated by the reaction are easy to separate, high-purity hydrogen chloride with the content of less than 0.5ppm can be obtained, and the influence of metal impurities caused by equipment corrosion is avoided.
Description
Technical Field
The invention relates to a method for removing water in hydrogen chloride by using thionyl chloride, belonging to the technical field of fine chemical engineering.
Background
Hydrogen chloride is a widely used chemical, and its main application fields are as follows: (1) the raw material for producing the fluorine compound is a fluorine source for producing a fluorine salt, a fluorine-containing refrigerant, a fluorine-containing plastic, a fluorine-containing rubber, a fluorine-containing resin, a fluorine-containing medicine, an agricultural chemical or the like; (2) as a strong acid corrosive agent, used for etching glass, pickling metal and etching the surface of a semiconductor; (3) as a catalyst for the alkylation reaction; (4) as an analytical reagent; (5) as a purge gas.
The removal of water in hydrogen chloride is the key of the purification process, and for the removal of water in hydrogen chloride, the existing methods comprise distillation water removal after fluorine gas contact reaction, activated carbon adsorption, carbon molecular sieve adsorption, carbonyl fluoride reaction water removal, activated carbon adsorption loaded with magnesium fluoride and the like. The existing technologies for removing water in hydrogen fluoride widely used at present comprise adsorption, refrigeration and the like, and have the defects of different degrees, including high operation risk, low water removal efficiency, incomplete water removal, corrosion to equipment caused by other impurities which are difficult to separate, water and incomplete purification.
Disclosure of Invention
In view of the above, the present invention is directed to a method for removing water from hydrogen chloride using thionyl chloride.
In order to achieve the purpose, the technical scheme of the invention is as follows:
a method for removing moisture from hydrogen chloride by using thionyl chloride, comprising the following steps:
(1) adding thionyl chloride into the hydrogen chloride enriched with water, reacting for 3-5 hours at-20-50 ℃ and-0.1-2 MPa to obtain a mixed gas of the hydrogen chloride and sulfur dioxide;
(2) and after the reaction is finished, rectifying the mixed gas to obtain dehydrated hydrogen chloride.
Preferably, the mass ratio of thionyl chloride to hydrogen chloride in the step (1) is 1: 50 to 100.
Preferably, the reaction temperature in the step (1) is 20-25 ℃.
Preferably, the reaction pressure in the step (1) is 0.1-0.2 MPa.
Preferably, the reaction temperature in the step (1) is 20-25 ℃, and the reaction pressure is 0.1-0.2 MPa.
Preferably, in the step (2), the mixed gas after the reaction is introduced into a rectifying device, the temperature of a condenser is reduced under 0.1-0.2 MPa, the temperature difference between a rectifying kettle and the condenser in the rectifying device is 10-20 ℃, the temperature difference is controlled and condensed to obtain liquid sulfur dioxide, hydrogen chloride is discharged from a tower working desorption top of the rectifying device, enters a subsequent absorption treatment device and is collected into a low-temperature storage device, the liquid sulfur dioxide is retained in the tower working desorption kettle of the rectifying device, the rectifying collection temperature in the tower working desorption kettle is ensured to be 50-60 ℃, the pressure difference of 0.1-0.2 MPa is maintained, and the separation of the hydrogen chloride and the sulfur dioxide is realized.
Advantageous effects
The method has good water removal effect, impurities generated by the reaction are easy to separate, high-purity hydrogen chloride with the content less than 0.5ppm can be obtained, and the influence of metal impurities caused by equipment corrosion is avoided.
Detailed Description
The present invention will be described in further detail with reference to specific examples.
Example 1
A method for removing moisture from hydrogen chloride by using thionyl chloride, comprising the following steps:
(1) according to the mass ratio of thionyl chloride to hydrogen chloride of 1: 50, adding thionyl chloride into the hydrogen chloride enriched with water, and reacting for 3 hours at 20 ℃ and 0.1MPa to obtain mixed gas of the hydrogen chloride and sulfur dioxide;
the reaction equation is as follows: SOCl2+H2O→SO2+2HCl；
(2) After the reaction is finished, rectifying the mixed gas to obtain dehydrated hydrogen chloride; specifically, the method comprises the following steps: introducing the reacted mixed gas into a rectifying device, cooling a condenser under 0.1MPa to ensure that the temperature difference between a rectifying kettle and the condenser in the rectifying device is 10 ℃, controlling the temperature difference and condensing to obtain liquid sulfur dioxide, discharging hydrogen chloride from a tower working desorption top of the rectifying device, allowing the hydrogen chloride to enter a subsequent absorption treatment device and then collecting the hydrogen chloride into a low-temperature storage device, keeping the liquid sulfur dioxide in the tower working desorption kettle of the rectifying device, ensuring that the rectifying collection temperature in the tower working desorption kettle is 50 ℃, and keeping the pressure difference of 0.1MPa to realize the separation of the hydrogen chloride and the sulfur dioxide.
The water content in the hydrogen chloride before dehydration was 100ppm and after dehydration was 0.2 ppm.
Example 2
A method for removing moisture from hydrogen chloride by using thionyl chloride, comprising the following steps:
(1) according to the mass ratio of thionyl chloride to hydrogen chloride of 1: 70, adding thionyl chloride into the hydrogen chloride enriched with water, reacting for 5 hours at-20 ℃ and-0.1 MPa to obtain mixed gas of the hydrogen chloride and sulfur dioxide;
(2) after the reaction is finished, rectifying the mixed gas to obtain dehydrated hydrogen chloride; specifically, the method comprises the following steps: introducing the reacted mixed gas into a rectifying device, cooling a condenser under 0.2MPa to ensure that the temperature difference between a rectifying kettle and the condenser in the rectifying device is 20 ℃, controlling the temperature difference and condensing to obtain liquid sulfur dioxide, discharging hydrogen chloride from a tower working desorption top of the rectifying device, allowing the hydrogen chloride to enter a subsequent absorption treatment device and then collecting the hydrogen chloride into a low-temperature storage device, keeping the liquid sulfur dioxide in the tower working desorption kettle of the rectifying device, ensuring that the rectifying collection temperature in the tower working desorption kettle is 60 ℃, and keeping the pressure difference of 0.2MPa to realize the separation of the hydrogen chloride and the sulfur dioxide.
The water content in the hydrogen chloride before dehydration was 100ppm and after dehydration was 0.2 ppm.
Example 3
A method for removing moisture from hydrogen chloride by using thionyl chloride, comprising the following steps:
(1) according to the mass ratio of thionyl chloride to hydrogen chloride of 1: 50, adding thionyl chloride into the hydrogen chloride enriched with water, and reacting for 4 hours at 50 ℃ and 2MPa to obtain mixed gas of the hydrogen chloride and sulfur dioxide;
(2) after the reaction is finished, rectifying the mixed gas to obtain dehydrated hydrogen chloride; specifically, the method comprises the following steps: introducing the reacted mixed gas into a rectifying device, cooling a condenser under 0.15MPa to ensure that the temperature difference between a rectifying kettle and the condenser in the rectifying device is 15 ℃, controlling the temperature difference and condensing to obtain liquid sulfur dioxide, discharging hydrogen chloride from a tower working desorption top of the rectifying device, allowing the hydrogen chloride to enter a subsequent absorption treatment device and then collecting the hydrogen chloride into a low-temperature storage device, keeping the liquid sulfur dioxide in the tower working desorption kettle of the rectifying device, ensuring that the rectifying collection temperature in the tower working desorption kettle is 55 ℃, and keeping the pressure difference of 0.15MPa to realize the separation of the hydrogen chloride and the sulfur dioxide.
The water content in the hydrogen chloride before dehydration was 100ppm and after dehydration was 0.25 ppm.
Example 4
A method for removing moisture from hydrogen chloride by using thionyl chloride, comprising the following steps:
(1) according to the mass ratio of thionyl chloride to hydrogen chloride of 1: 100, adding thionyl chloride into the hydrogen chloride enriched with water, and reacting for 3.5 hours at 0 ℃ and 1MPa to obtain a mixed gas of the hydrogen chloride and sulfur dioxide;
(2) after the reaction is finished, rectifying the mixed gas to obtain dehydrated hydrogen chloride; specifically, the method comprises the following steps: introducing the reacted mixed gas into a rectifying device, cooling a condenser under 0.15MPa to ensure that the temperature difference between a rectifying kettle and the condenser in the rectifying device is 15 ℃, controlling the temperature difference and condensing to obtain liquid sulfur dioxide, discharging hydrogen chloride from a tower working desorption top of the rectifying device, allowing the hydrogen chloride to enter a subsequent absorption treatment device and then collecting the hydrogen chloride into a low-temperature storage device, keeping the liquid sulfur dioxide in the tower working desorption kettle of the rectifying device, ensuring that the rectifying collection temperature in the tower working desorption kettle is 55 ℃, and keeping the pressure difference of 0.15MPa to realize the separation of the hydrogen chloride and the sulfur dioxide.
The water content in the hydrogen chloride before dehydration was 100ppm and after dehydration was 0.25 ppm.
In summary, the invention includes but is not limited to the above embodiments, and any equivalent replacement or local modification made under the spirit and principle of the invention should be considered as being within the protection scope of the invention.
Claims (6)
1. A method for removing water in hydrogen chloride by using thionyl chloride is characterized by comprising the following steps: the method comprises the following steps:
(1) adding thionyl chloride into the hydrogen chloride enriched with water, reacting for 3-5 hours at-20-50 ℃ and-0.1-2 MPa to obtain a mixed gas of the hydrogen chloride and sulfur dioxide;
(2) and after the reaction is finished, rectifying the mixed gas to obtain dehydrated hydrogen chloride.
2. The method of claim 1 for removing water from hydrogen chloride using thionyl chloride, characterized in that: the mass ratio of the thionyl chloride to the hydrogen chloride in the step (1) is 1: 50 to 100.
3. The method of claim 1 for removing water from hydrogen chloride using thionyl chloride, characterized in that: the reaction temperature in the step (1) is 20-25 ℃.
4. The method of claim 1 for removing water from hydrogen chloride using thionyl chloride, characterized in that: the reaction pressure in the step (1) is 0.1-0.2 MPa.
5. The method of claim 1 for removing water from hydrogen chloride using thionyl chloride, characterized in that: in the step (1), the reaction temperature is 20-25 ℃, and the reaction pressure is 0.1-0.2 MPa.
6. The method of claim 1 for removing water from hydrogen chloride using thionyl chloride, characterized in that: in the step (2), introducing the reacted mixed gas into a rectifying device, cooling a condenser under 0.1-0.2 MPa, enabling the temperature difference between a rectifying kettle and the condenser in the rectifying device to be 10-20 ℃, controlling the temperature difference and condensing to obtain liquid sulfur dioxide, discharging hydrogen chloride from a tower working desorption top of the rectifying device, enabling the hydrogen chloride to enter a subsequent absorption treatment device and then collecting the hydrogen chloride into a low-temperature storage device, reserving the liquid sulfur dioxide in the tower working desorption kettle of the rectifying device, ensuring that the rectifying collection temperature in the tower working desorption kettle is 50-60 ℃, and keeping the pressure difference of 0.1-0.2 MPa to realize the separation of the hydrogen chloride and the sulfur dioxide.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011466961.3A CN112707372A (en) | 2020-12-14 | 2020-12-14 | Method for removing water in hydrogen chloride by using thionyl chloride |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011466961.3A CN112707372A (en) | 2020-12-14 | 2020-12-14 | Method for removing water in hydrogen chloride by using thionyl chloride |
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| CN112707372A true CN112707372A (en) | 2021-04-27 |
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| CN202011466961.3A Pending CN112707372A (en) | 2020-12-14 | 2020-12-14 | Method for removing water in hydrogen chloride by using thionyl chloride |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1063483A (en) * | 1991-01-25 | 1992-08-12 | 北京农业大学 | A new process for preparing anhydrous formic acid |
| US20080249253A1 (en) * | 2007-04-03 | 2008-10-09 | Royce Elton Ennis | Partially neutralized chlorosulfonated polyolefin elastomers |
| CN111115579A (en) * | 2020-01-12 | 2020-05-08 | 浙江博瑞电子科技有限公司 | Reactive ultrasonic rectification purification method for HCL electronic gas |
| CN111807325A (en) * | 2020-01-22 | 2020-10-23 | 浙江凯圣氟化学有限公司 | Reactive ultrasonic rectification purification method for HF electronic gas |
| CN112010268A (en) * | 2020-09-26 | 2020-12-01 | 安徽金禾实业股份有限公司 | Medium-pressure rectification separation method for sucralose chlorination tail gas |
-
2020
- 2020-12-14 CN CN202011466961.3A patent/CN112707372A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1063483A (en) * | 1991-01-25 | 1992-08-12 | 北京农业大学 | A new process for preparing anhydrous formic acid |
| US20080249253A1 (en) * | 2007-04-03 | 2008-10-09 | Royce Elton Ennis | Partially neutralized chlorosulfonated polyolefin elastomers |
| CN111115579A (en) * | 2020-01-12 | 2020-05-08 | 浙江博瑞电子科技有限公司 | Reactive ultrasonic rectification purification method for HCL electronic gas |
| CN111807325A (en) * | 2020-01-22 | 2020-10-23 | 浙江凯圣氟化学有限公司 | Reactive ultrasonic rectification purification method for HF electronic gas |
| CN112010268A (en) * | 2020-09-26 | 2020-12-01 | 安徽金禾实业股份有限公司 | Medium-pressure rectification separation method for sucralose chlorination tail gas |
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| CB02 | Change of applicant information |
Address after: 057550 No. five Weir Road, chemical industry gathering area, Feixiang District, Handan, Hebei, 1 Applicant after: China shipbuilding (Handan) Perry Special Gas Co.,Ltd. Address before: No.1 Weiwu Road, chemical industry gathering area, Feixiang County, Handan City, Hebei Province Applicant before: PERIC SPECIAL GASES Co.,Ltd. |
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Application publication date: 20210427 |
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