CN110040692A - Prepare the method and device of high-purity sulfur dioxide gas - Google Patents
Prepare the method and device of high-purity sulfur dioxide gas Download PDFInfo
- Publication number
- CN110040692A CN110040692A CN201910401685.3A CN201910401685A CN110040692A CN 110040692 A CN110040692 A CN 110040692A CN 201910401685 A CN201910401685 A CN 201910401685A CN 110040692 A CN110040692 A CN 110040692A
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- China
- Prior art keywords
- sulfur dioxide
- dioxide gas
- channel
- storage tank
- purity
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- RAHZWNYVWXNFOC-UHFFFAOYSA-N Sulphur dioxide Chemical compound O=S=O RAHZWNYVWXNFOC-UHFFFAOYSA-N 0.000 title claims abstract description 84
- 238000000034 method Methods 0.000 title claims abstract description 10
- 239000003463 adsorbent Substances 0.000 claims abstract description 22
- 238000010521 absorption reaction Methods 0.000 claims abstract description 12
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000001816 cooling Methods 0.000 claims abstract description 6
- 229910000831 Steel Inorganic materials 0.000 claims abstract description 5
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims abstract description 5
- 239000005864 Sulphur Substances 0.000 claims abstract description 5
- 238000000746 purification Methods 0.000 claims abstract description 5
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 5
- 239000010959 steel Substances 0.000 claims abstract description 5
- 238000009833 condensation Methods 0.000 claims abstract description 3
- 230000005494 condensation Effects 0.000 claims abstract description 3
- 238000005554 pickling Methods 0.000 claims description 7
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 4
- 239000002808 molecular sieve Substances 0.000 claims 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 claims description 2
- 239000002253 acid Substances 0.000 claims 1
- 238000004140 cleaning Methods 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 239000012535 impurity Substances 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 229910002092 carbon dioxide Inorganic materials 0.000 description 3
- 238000005070 sampling Methods 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- 238000009835 boiling Methods 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 206010054949 Metaplasia Diseases 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000007844 bleaching agent Substances 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 230000001276 controlling effect Effects 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
- 238000005516 engineering process Methods 0.000 description 1
- 235000015110 jellies Nutrition 0.000 description 1
- 239000008274 jelly Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 230000015689 metaplastic ossification Effects 0.000 description 1
- 229910052680 mordenite Inorganic materials 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000012216 screening 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
- C01B17/00—Sulfur; Compounds thereof
- C01B17/48—Sulfur dioxide; Sulfurous acid
- C01B17/50—Preparation of sulfur dioxide
- C01B17/56—Separation; Purification
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Separation Of Gases By Adsorption (AREA)
- Treating Waste Gases (AREA)
Abstract
The present invention provides a kind of method and device for preparing high-purity sulfur dioxide gas, including successively by pre-cooling, absorption, secondary filter, liquefaction, rectifying, finally high-purity sulfur dioxide gas obtained enters product storage tank by sulfur dioxide；Device includes the commercial silica sulphur steel cylinder successively to connect, forecooler, adsorbent bed, accurate filter, liquefier, rectifying column, product storage tank, it is characterized by: there are four connect into the multiple adsorbent bed group for being connected in series with each other or being connected in parallel with each other by pipeline and valve with the adsorbent bed, rectifier is equipped with heat exchanger, sulfur dioxide after heat exchange condensation purification, which is equipped with, returns to the channel in the middle part of rectifying column and the channel towards product storage tank, condenser overhead is equipped with emptying channel, the emptying channel other end connects with lye absorption plant, it is simple with technological operation that refrigerator is connected between liquefier and heat exchanger, the advantages that low in cost, the 4N of industrialized production can be achieved, 5N purity sulfur dioxide gas.
Description
Technical field
The present invention relates to a kind of method and devices for preparing high-purity sulfur dioxide gas.
Background technique
At present sulfur dioxide gas in addition to the raw material of industry, bleaching agent industry relaying is continuous play a significant role other than, in recent years
It is also to grow rapidly in electronics, semicon industry, is mainly used for kinescope manufacture etc..Sulfur dioxide is work currently on the market
Industry grade sulfur dioxide, purity are up to 99.97%, and Con trolling index is water and residue, are unable to satisfy electronics, semicon industry to height
The demand of pure sulfur dioxide.China Patent No. CN201310004486.1 is pointed out, the sulfur dioxide containing moisture is introduced air inlet
Mouthful, under the action of dry screw rod, desiccant CaCl that the moisture in sulfur dioxide is dried in screw rod2Solid powder absorbs,
Dry sulfur dioxide is discharged by exhaust outlet, the CaCl of water suction2Solid powder is continuously recycled by thermal dehydration realization.
But the moisture content of sulfur dioxide obtained by the patented method and device can only achieve 0.15wt%, be not suitable for the life of high-purity sulfur dioxide
It produces.
Summary of the invention
The object of the present invention is to provide a kind of production method for being applicable in high-purity sulfur dioxide and devices.
The object of the invention technical solution are as follows: a method of prepare high-purity sulfur dioxide gas, it is characterised in that:
Including sulfur dioxide successively to be passed through to pre-cooling, absorption, secondary filter, liquefaction, rectifying finally high-purity sulfur dioxide gas obtained
Body enters product storage tank；
Pressure when the described sulfur dioxide gas gas absorption is 0.1~0.2MPa, and temperature is -5~0 DEG C；
The rectifying pressure is 0.3~0.4MPa, and rectification temperature is 20~25 DEG C.
The adsorbent of preferred absorption is partial size 3~4mm pickling modenite, the pickling modenite pickling
Journey are as follows: mordenite molecular sieve is passed through into 400 DEG C of vapor high-temperature roasting 4h, 1.0mol/L hydrochloric acid is immersed in after being cooled to room temperature
8h in solution activates dry 8h under the conditions of 300 DEG C.
A kind of device preparing high-purity sulfur dioxide gas, including successively connect commercial silica sulphur steel cylinder, pre-cooling
Device, adsorbent bed, accurate filter, liquefier, rectifying column, product storage tank, it is characterised in that:
There are four the adsorbent beds, and four adsorbent beds are connected by pipeline and valve to be connected in series with each other or company parallel with one another
The multiple adsorbent bed group connect；
The rectifier is equipped with heat exchanger, and the sulfur dioxide after heat exchange condensation purification is logical in the middle part of rectifying column equipped with returning
Road and channel towards product storage tank, condenser overhead are equipped with emptying channel, empty the channel other end and lye absorption plant phase
It connects；
Refrigerator is connected between the liquefier and heat exchanger；
The interface channel is equipped with flowmeter.
The pickling modenite that the adsorbent of preferred adsorbent bed is 3~4mm of partial size.
The present invention compared with the existing technology has the advantage that simple, low in cost, the achievable industrial metaplasia of technological operation
Produce 4N, 5N(99.999%) purity sulfur dioxide gas.
Detailed description of the invention
Fig. 1 is the schematic diagram of the embodiment of the present invention.
In figure: 1, commercial silica sulphur steel cylinder, 2, forecooler, 3, adsorbent bed, 4, accurate filter, 5, liquefier, 6, cold
Jelly machine, 7, rectifying column, 8, heat exchanger, 9, emptying channel, 10, product storage tank, 11, lye absorption plant, 12, sampling valve.
Specific embodiment
Illustrate embodiment with reference to the accompanying drawing:
Embodiment 1
Referring to Fig. 1: a kind of production method being applicable in high-purity sulfur dioxide and device, including connection commercial silica sulphur steel cylinder 1
Sulfur dioxide purifies channel, and 2, four adsorbent beds 3 of forecooler are successively passed through in carbon dioxide purification channel, and (four adsorbent beds pass through pipe
Road and valve connect into the multiple adsorbent bed group for being connected in series with each other or being connected in parallel with each other), accurate filter 4, liquefier 5,
7 bottom of rectifying column is finally connected, 7 top of rectifying column is equipped with the heat exchanger 8 that inside is connected with low temperature cold liquid, the output end of heat exchanger 8
Refrigerator is returned by liquefier 5, forecooler 2, heat exchanger 8.Emptying channel 9 is equipped at the top of rectifying column 8, emptying channel 9 is passed through
Lye absorption plant 11.7 bottom of rectifying column is equipped with electric heater, and 7 top of rectifying column is connected with discharge line, and discharge line is equipped with
Sampling valve 12.
Wherein, sulfur dioxide purification again passes by four adsorbent beds 3 after forecooler 2, finally connects rectifying column 7.
50.0kg sulfur dioxide first passes through forecooler 2 and is cooled to -5~0 DEG C in advance, charging rate 0.22kg/min；
Absorption: passing through four adsorbent beds 3, impurity gradually adsorbed, then passes through 4 impurity screening of accurate filter；
Liquefier 5, which cools down the sulfur dioxide gas Jing Guo suction-operated, to liquefy, and finally flows into 7 kettle of rectifying column；
The heater of 7 bottom of rectifying column, which heats sulfur dioxide, to be risen and condenses in heat exchanger 8, and the lower impurity of boiling point is then with gas
State is discharged at the top of rectifying column.Control tower press 0.35~0.40MPa, 22~25 DEG C of temperature.
Sampling valve 12 on 7 top discharge line of rectifying column detects sulfur dioxide purity, such as meets the requirements, then opens discharge
Valve on pipeline connects product storage tank 10.
The gas being collected into analyzes water content 2.3ppm by Moisture Meter, passes through chromatographic N2Content
3.1ppm, O2Content 3.7ppm, CO2Content 0.3ppm, CO content 0.1ppm analyzes residue content 0.2ppm.
Embodiment 2
30.0kg sulfur dioxide is cooled to -5~0 DEG C, charging rate 0.2kg/min in advance by first passing through forecooler 2, inhales by four
Attached bed 3, accurate filter 4, liquefier 5 enter 7 kettle of rectifying column of pre-cooling；
The heater of 7 bottom of rectifying column, which heats sulfur dioxide, to be risen and condenses in heat exchanger 8, and the lower impurity of boiling point is then with gas
State is discharged at the top of rectifying column.Control tower press 0.30~0.35MPa, 20~22 DEG C of temperature.
The gas being collected into analyzes water content 2.0ppm by Moisture Meter, passes through chromatographic N2Content
2.1ppm, O2Content 3.1ppm, CO2Content 0.2ppm, CO content 0.1ppm, residue analysis content 0.1ppm.
Claims (4)
1. a kind of method for preparing high-purity sulfur dioxide gas, it is characterised in that: including by sulfur dioxide successively by pre-cooling,
Finally high-purity sulfur dioxide gas obtained enters product storage tank for absorption, secondary filter, liquefaction, rectifying；
Pressure when the described sulfur dioxide gas gas absorption is 0.1~0.2MPa, and temperature is -5~0 DEG C；
The rectifying pressure is 0.3~0.4MPa, and rectification temperature is 20~25 DEG C.
2. a kind of device for preparing high-purity sulfur dioxide gas, including successively connect commercial silica sulphur steel cylinder (1), pre-cooling
Device (2), adsorbent bed (3), accurate filter (4), liquefier (5), rectifying column (7), product storage tank (10), it is characterised in that:
There are four the adsorbent beds (3), and four adsorbent beds (3) are connected by pipeline and valve to be connected in series with each other or mutually
The multiple adsorbent bed group being connected in parallel；
Rectifying column (7) top is equipped with heat exchanger (8), and the sulfur dioxide after heat exchange condensation purification, which is equipped with, returns to rectifying column
(7) channel in the middle part of and the channel towards product storage tank, heat exchanger (8) top are equipped with emptying channel (9), and emptying channel (9) is another
One end connects with lye absorption plant (11)；
Refrigerator (6) are connected between the liquefier (5) and heat exchanger (8)；
The interface channel is equipped with flowmeter.
3. a kind of method for preparing high-purity sulfur dioxide gas according to claim 1: it is characterized by: the suction
Attached adsorbent is partial size 3~4mm pickling modenite, the pickling modenite acid cleaning process are as follows: by modenite
Molecular sieve passes through 400 DEG C of vapor high-temperature roasting 4h, 8h in 1.0mol/L hydrochloric acid solution is immersed in after being cooled to room temperature, 300
Dry 8h is activated under the conditions of DEG C.
4. a kind of device for preparing high-purity sulfur dioxide gas according to claim 2, it is characterised in that: the suction
The adsorbent of attached bed (3) is the pickling modenite of 3~4mm of partial size.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910401685.3A CN110040692B (en) | 2019-05-15 | 2019-05-15 | Method and device for preparing high-purity sulfur dioxide gas |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910401685.3A CN110040692B (en) | 2019-05-15 | 2019-05-15 | Method and device for preparing high-purity sulfur dioxide gas |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN110040692A true CN110040692A (en) | 2019-07-23 |
| CN110040692B CN110040692B (en) | 2024-02-09 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201910401685.3A Active CN110040692B (en) | 2019-05-15 | 2019-05-15 | Method and device for preparing high-purity sulfur dioxide gas |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113562702A (en) * | 2021-08-25 | 2021-10-29 | 福建福豆新材料有限公司 | Method for purifying high-purity electronic-grade sulfur dioxide |
| CN114291795A (en) * | 2022-01-18 | 2022-04-08 | 中船(邯郸)派瑞特种气体股份有限公司 | Method for preparing high-purity sulfur dioxide |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH11228114A (en) * | 1998-02-05 | 1999-08-24 | Sumitomo Seika Chem Co Ltd | Purifying method of sulfur dioxide and device therefor |
| CN101254918A (en) * | 2008-03-31 | 2008-09-03 | 大连理工大学 | Device for purifying carbon dioxide by adsorption distillation technology |
| CN106276812A (en) * | 2016-09-14 | 2017-01-04 | 北京清新环境技术股份有限公司 | A kind of high temperature sulphur-containing exhaust gas prepares liquid sulfur dioxide device |
| CN109126358A (en) * | 2017-06-27 | 2019-01-04 | 清远先导材料有限公司 | The purifying technique and purifying plant of special gas |
| CN210366992U (en) * | 2019-05-15 | 2020-04-21 | 大连科利德光电子材料有限公司 | Device for preparing high-purity sulfur dioxide gas |
-
2019
- 2019-05-15 CN CN201910401685.3A patent/CN110040692B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH11228114A (en) * | 1998-02-05 | 1999-08-24 | Sumitomo Seika Chem Co Ltd | Purifying method of sulfur dioxide and device therefor |
| CN101254918A (en) * | 2008-03-31 | 2008-09-03 | 大连理工大学 | Device for purifying carbon dioxide by adsorption distillation technology |
| CN106276812A (en) * | 2016-09-14 | 2017-01-04 | 北京清新环境技术股份有限公司 | A kind of high temperature sulphur-containing exhaust gas prepares liquid sulfur dioxide device |
| CN109126358A (en) * | 2017-06-27 | 2019-01-04 | 清远先导材料有限公司 | The purifying technique and purifying plant of special gas |
| CN210366992U (en) * | 2019-05-15 | 2020-04-21 | 大连科利德光电子材料有限公司 | Device for preparing high-purity sulfur dioxide gas |
Non-Patent Citations (1)
| Title |
|---|
| 牟国培: "JMT型天然沸石干燥剂在酸性气体深度脱水中的应用", 化工设计, no. 01, pages 23 - 26 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113562702A (en) * | 2021-08-25 | 2021-10-29 | 福建福豆新材料有限公司 | Method for purifying high-purity electronic-grade sulfur dioxide |
| CN114291795A (en) * | 2022-01-18 | 2022-04-08 | 中船(邯郸)派瑞特种气体股份有限公司 | Method for preparing high-purity sulfur dioxide |
| CN114291795B (en) * | 2022-01-18 | 2023-04-18 | 中船(邯郸)派瑞特种气体股份有限公司 | Method for preparing high-purity sulfur dioxide |
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| Publication number | Publication date |
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| CN110040692B (en) | 2024-02-09 |
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