CN110040692B - Method and device for preparing high-purity sulfur dioxide gas - Google Patents
Method and device for preparing high-purity sulfur dioxide gas Download PDFInfo
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- CN110040692B CN110040692B CN201910401685.3A CN201910401685A CN110040692B CN 110040692 B CN110040692 B CN 110040692B CN 201910401685 A CN201910401685 A CN 201910401685A CN 110040692 B CN110040692 B CN 110040692B
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- sulfur dioxide
- dioxide gas
- purity
- adsorption
- storage tank
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- RAHZWNYVWXNFOC-UHFFFAOYSA-N Sulphur dioxide Chemical compound O=S=O RAHZWNYVWXNFOC-UHFFFAOYSA-N 0.000 title claims abstract description 96
- 238000000034 method Methods 0.000 title claims abstract description 12
- 238000001179 sorption measurement Methods 0.000 claims abstract description 24
- 238000003860 storage Methods 0.000 claims abstract description 11
- 238000000746 purification Methods 0.000 claims abstract description 6
- 229910000831 Steel Inorganic materials 0.000 claims abstract description 5
- 239000003513 alkali Substances 0.000 claims abstract description 5
- 239000010959 steel Substances 0.000 claims abstract description 5
- 238000001914 filtration Methods 0.000 claims abstract description 4
- 238000009833 condensation Methods 0.000 claims abstract description 3
- 230000005494 condensation Effects 0.000 claims abstract description 3
- 238000001816 cooling Methods 0.000 claims abstract description 3
- 229910052680 mordenite Inorganic materials 0.000 claims description 7
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 4
- 239000003463 adsorbent Substances 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 claims description 4
- 238000010521 absorption reaction Methods 0.000 claims description 3
- 239000002245 particle Substances 0.000 claims description 3
- 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
- 238000009776 industrial production Methods 0.000 abstract description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- 239000012535 impurity Substances 0.000 description 4
- 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
- 238000001035 drying Methods 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 239000007844 bleaching agent Substances 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 239000002274 desiccant Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000011532 electronic conductor Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000011593 sulfur 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
- 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)
- Treating Waste Gases (AREA)
- Separation Of Gases By Adsorption (AREA)
Abstract
The invention provides a method and a device for preparing high-purity sulfur dioxide gas, which comprises the steps of sequentially pre-cooling, adsorbing, precisely filtering, liquefying and rectifying sulfur dioxide to finally prepare high-purity sulfur dioxide gas, and then feeding the high-purity sulfur dioxide gas into a product storage tank; the device comprises an industrial sulfur dioxide steel bottle, a precooler, an adsorption bed, a precise filter, a liquefier, a rectifying tower and a product storage tank which are connected in sequence, and is characterized in that: the adsorption bed has four and connects into the multiple adsorption bed group of mutual series connection or mutual parallel connection through pipeline and valve, and rectifying column upper portion is equipped with the heat exchanger, and the sulfur dioxide after the heat transfer condensation purification is equipped with the passageway that returns rectifying column middle part and the passageway that leads to the product storage tank, and the condenser top is equipped with the evacuation passageway, and the evacuation passageway other end meets with alkali lye absorbing device, connects between liquefier and the heat exchanger and has advantages such as simple technological operation, low cost, can realize 4N, 5N purity sulfur dioxide gas of industrial production.
Description
Technical Field
The invention relates to a method and a device for preparing high-purity sulfur dioxide gas.
Background
At present, sulfur dioxide gas plays an important role in industry raw materials and bleaching agent industry, and is also rapidly developed in electronics and semiconductor industry in recent years, and is mainly used for manufacturing kinescope and the like. At present, sulfur dioxide in the market is industrial grade sulfur dioxide, the purity is up to 99.97%, the control indexes are water and residues, and the requirements of the electronic and semiconductor industries on high-purity sulfur dioxide cannot be met. Chinese patent No. CN201310004486.1 teaches that sulfur dioxide containing moisture is introduced into the air inlet, under the action of the drying screw, dioxygenThe moisture in the sulfur is dried by the drying agent CaCl in the drying screw 2 Solid powder is absorbed, dry sulfur dioxide is discharged through an exhaust port, and CaCl with water is absorbed 2 The solid powder is heated and dehydrated to realize continuous recycling. However, the water content of the sulfur dioxide obtained by the method and the device can only reach 0.15wt percent, and the method and the device are not applicable to the production of high-purity sulfur dioxide.
Disclosure of Invention
The invention aims to provide a production method and a device suitable for high-purity sulfur dioxide.
The technical proposal of the invention is as follows: a method for preparing high purity sulfur dioxide gas, characterized by: the method comprises the steps of sequentially pre-cooling, adsorbing, precisely filtering, liquefying and rectifying sulfur dioxide to obtain high-purity sulfur dioxide gas, and enabling the high-purity sulfur dioxide gas to enter a product storage tank;
the pressure of the sulfur dioxide gas during adsorption is 0.1-0.2 MPa, and the temperature is-5-0 ℃;
the rectification pressure is 0.3-0.4 MPa, and the rectification temperature is 20-25 ℃.
The preferred adsorbent for adsorption is acid-washed mordenite with a particle size of 3-4 mm, and the acid-washed mordenite is acid-washed by the following steps: the mordenite molecular sieve is baked for 4 hours at high temperature by 400 ℃ steam, cooled to room temperature, soaked in 1.0mol/L hydrochloric acid solution for 8 hours, activated and dried for 8 hours at 300 ℃.
The utility model provides a device of preparation high purity sulfur dioxide gas, includes industrial sulfur dioxide steel bottle, precooler, adsorption bed, precision filter, liquefier, rectifying column, the product storage tank that meets in proper order, its characterized in that:
the four adsorption beds are connected into a plurality of adsorption bed groups which are connected in series or in parallel through pipelines and valves;
the upper part of the rectifying tower is provided with a heat exchanger, the sulfur dioxide subjected to heat exchange, condensation and purification is provided with a channel returning to the middle part of the rectifying tower and a channel leading to a product storage tank, the top of the condenser is provided with an evacuation channel, and the other end of the evacuation channel is connected with an alkali liquor absorption device;
a refrigerator is connected between the liquefier and the heat exchanger;
and the connecting channel is provided with a flowmeter.
The adsorbent of the preferred adsorbent bed is acid-washed mordenite with a particle size of 3-4 mm.
Compared with the prior art, the invention has the following advantages: the process is simple to operate, the cost is low, and the industrial production of 4N and 5N (99.999%) pure sulfur dioxide gas can be realized.
Drawings
FIG. 1 is a schematic diagram of an embodiment of the present invention.
In the figure: 1. the industrial sulfur dioxide steel bottle, 2, precooler, 3, adsorption bed, 4, precision filter, 5, liquefier, 6, refrigerator, 7, rectifying tower, 8, heat exchanger, 9, evacuation channel, 10, product storage tank, 11, alkali liquor absorbing device, 12, sampling valve.
Detailed Description
The embodiments are described below with reference to the accompanying drawings:
example 1
See fig. 1: the utility model provides a method and device for producing suitable high-purity sulfur dioxide, including connecting the sulfur dioxide purification passageway of industry sulfur dioxide steel bottle 1, carbon dioxide purification passageway is through precooler 2, four adsorption beds 3 (four adsorption beds pass through pipeline and valve and connect into the multiple adsorption bed group of mutual series connection or mutual parallel connection), precision filter 4, liquefier 5, connect rectifying column 7 bottom at last, rectifying column 7 upper portion is equipped with the heat exchanger 8 that has the low temperature Leng Ye of leading to inside, the output of heat exchanger 8 passes through liquefier 5, precooler 2, heat exchanger 8 returns the refrigerator. An emptying channel 9 is arranged at the top of the rectifying tower 8, and the emptying channel 9 passes through an alkali liquor absorption device 11. An electric heater is arranged at the bottom of the rectifying tower 7, a discharge pipeline is connected to the upper part of the rectifying tower 7, and a sampling valve 12 is arranged on the discharge pipeline.
Wherein, the sulfur dioxide purification passes through four adsorption beds 3 again after passing through the precooler 2, and finally is connected with the rectifying tower 7.
50.0kg of sulfur dioxide is pre-cooled to-5-0 ℃ by a pre-cooler 2, and the feeding speed is 0.22kg/min;
adsorption: gradually adsorbing impurities through four adsorption beds 3, and filtering the impurities through a precision filter 4;
the liquefier 5 cools and liquefies the sulfur dioxide gas subjected to adsorption, and finally flows into the rectifying tower 7 kettle;
the heater at the bottom of the rectifying tower 7 heats sulfur dioxide up and condenses in the heat exchanger 8, and impurities with lower boiling points are discharged from the top of the rectifying tower in a gaseous state. The tower pressure is controlled to be 0.35-0.40 MPa, and the temperature is controlled to be 22-25 ℃.
And if the sulfur dioxide purity is detected by a sampling valve 12 on a discharge pipeline at the upper part of the rectifying tower 7, opening the valve on the discharge pipeline and connecting a product storage tank 10.
The collected gas was analyzed for water content of 2.3ppm by a moisture meter, and N by a gas chromatograph 2 At a level of 3.1ppm, O 2 At a level of 3.7ppm, CO 2 0.3ppm, 0.1ppm CO and 0.2ppm analysis residue.
Example 2
30.0kg of sulfur dioxide is pre-cooled to-5-0 ℃ by a pre-cooler 2, the feeding speed is 0.2kg/min, and the sulfur dioxide enters a pre-cooled rectifying tower 7 kettle by four adsorption beds 3, a precise filter 4 and a liquefier 5;
the heater at the bottom of the rectifying tower 7 heats sulfur dioxide up and condenses in the heat exchanger 8, and impurities with lower boiling points are discharged from the top of the rectifying tower in a gaseous state. The tower pressure is controlled to be 0.30-0.35 MPa, and the temperature is controlled to be 20-22 ℃.
The collected gas was analyzed for water content of 2.0ppm by a moisture meter, and N by a gas chromatograph 2 At a level of 2.1ppm, O 2 At a level of 3.1ppm, CO 2 0.2ppm, 0.1ppm CO and 0.1ppm residue analysis.
Claims (2)
1. A method for preparing high purity sulfur dioxide gas, characterized by: the method comprises the steps of sequentially pre-cooling, adsorbing, precisely filtering, liquefying and rectifying sulfur dioxide to obtain high-purity sulfur dioxide gas, and enabling the high-purity sulfur dioxide gas to enter a product storage tank;
the precooling temperature is-5-0 ℃;
the sulfur dioxide gas passes through four adsorption beds during adsorption, the adsorption pressure is 0.1-0.2 MPa, and the temperature is-5-0 ℃;
the rectification pressure is 0.3-0.4 MPa, and the rectification temperature is 20-25 ℃;
the adsorbent for adsorption is acid-washed mordenite with the particle size of 3-4 mm, and the acid-washed mordenite is acid-washed by the following steps: the mordenite molecular sieve is baked for 4 hours at high temperature by 400 ℃ steam, cooled to room temperature, soaked in 1.0mol/L hydrochloric acid solution for 8 hours, activated and dried for 8 hours at 300 ℃.
2. The apparatus for the method for producing high-purity sulfur dioxide gas according to claim 1, comprising an industrial sulfur dioxide steel cylinder (1), a precooler (2), an adsorption bed (3), a precision filter (4), a liquefier (5), a rectifying tower (7) and a product storage tank (10) which are connected in sequence, wherein:
the four adsorption beds (3) are connected in series or are mutually connected through pipelines and valves
A plurality of adsorption bed groups connected in parallel;
the upper part of the rectifying tower (7) is provided with a heat exchanger (8), the sulfur dioxide subjected to heat exchange, condensation and purification is provided with a channel returning to the middle part of the rectifying tower (7) and a channel leading to a product storage tank, the top of the heat exchanger (8) is provided with an emptying channel (9), and the other end of the emptying channel (9) is connected with an alkali liquor absorption device (11);
a refrigerator (6) is connected between the liquefier (5) and the heat exchanger (8).
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 |
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| Publication Number | Publication Date |
|---|---|
| CN110040692A CN110040692A (en) | 2019-07-23 |
| CN110040692B true CN110040692B (en) | 2024-02-09 |
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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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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113562702B (en) * | 2021-08-25 | 2022-11-01 | 福建福豆新材料有限公司 | Method for purifying high-purity electronic-grade 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 |
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 |
|---|
| JMT型天然沸石干燥剂在酸性气体深度脱水中的应用;牟国培;化工设计(第01期);23-26 * |
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| CN110040692A (en) | 2019-07-23 |
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