CN110980670A - Rectification method of high-purity nitrous oxide - Google Patents
Rectification method of high-purity nitrous oxide Download PDFInfo
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- CN110980670A CN110980670A CN201911030824.2A CN201911030824A CN110980670A CN 110980670 A CN110980670 A CN 110980670A CN 201911030824 A CN201911030824 A CN 201911030824A CN 110980670 A CN110980670 A CN 110980670A
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- nitrous oxide
- valve
- purity
- rectifying tower
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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
- C01B21/00—Nitrogen; Compounds thereof
- C01B21/20—Nitrogen oxides; Oxyacids of nitrogen; Salts thereof
- C01B21/22—Nitrous oxide (N2O)
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/14—Fractional distillation or use of a fractionation or rectification column
- B01D3/32—Other features of fractionating columns ; Constructional details of fractionating columns not provided for in groups B01D3/16 - B01D3/30
Abstract
The invention provides a rectification method of high-purity nitrous oxide, belonging to the technical field of chemical industry. It has solved prior art and has had the poor problem of stability. The rectification method of the high-purity nitrous oxide comprises the following steps: A. storing materials: storing nitrous oxide containing impurities in a storage tank; B. preparing for rectification: the rectifying tower is provided with an inlet, an exhaust port and an outlet which are communicated with the inner cavity of the rectifying tower, the inlet is connected with a first valve capable of being opened and closed, the exhaust port is connected with a second valve capable of being opened and closed, the first valve is opened and the second valve is closed in an initial state, and the outlet is communicated with the high-purity storage tank; C. and (3) rectification: inputting the nitrous oxide into a rectifying tower from an inlet, removing a small amount of nitrogen, oxygen and hydrogen contained in the nitrous oxide through the rectifying tower, and periodically opening a second valve in the operation process of the rectifying tower; D. and (4) storage tank. The rectification method of the high-purity nitrous oxide has high stability.
Description
Technical Field
The valve belongs to the technical field of chemical industry, and relates to a rectification method of high-purity nitrous oxide.
Background
The nitrous oxide is prepared into the nitrous oxide of normal gas, and when the nitrous oxide is used as electronic gas in semiconductor industry, the requirement on the purity of the nitrous oxide is higher.
The existing common gas nitrous oxide can be used as electronic gas after being filtered.
The existing nitrous oxide is generally purified and filtered directly through a rectifying tower. The nitrous oxide is gradually vaporized in the rectifying tower until the nitrous oxide reaches the liquefaction temperature and is converted into liquid. However, the existing rectification column still contains a small amount of gas in the output process of the liquid nitrous oxide, which affects the purity of the nitrous oxide.
Disclosure of Invention
The invention aims to provide a method for rectifying high-purity nitrous oxide with high stability, aiming at the problems in the prior art.
The purpose of the invention can be realized by the following technical scheme:
a method for rectifying high-purity nitrous oxide, comprising the following steps:
A. storing materials: storing the liquid nitrous oxide containing impurities in a storage tank;
B. preparing for rectification: the rectifying tower is provided with an inlet, an exhaust port and an outlet which are communicated with the inner cavity of the rectifying tower, the inlet is connected with a first valve capable of being opened and closed, the exhaust port is connected with a second valve capable of being opened and closed, the first valve is opened and the second valve is closed in an initial state, and the outlet is communicated with the high-purity storage tank;
C. and (3) rectification: inputting the nitrous oxide into a rectifying tower from an inlet, removing a small amount of nitrogen, oxygen and hydrogen contained in the nitrous oxide through the rectifying tower, and periodically opening a second valve in the operation process of the rectifying tower;
D. storage tank: inputting the rectified high-purity nitrous oxide into a high-purity storage tank for storage.
The ordinary gaseous nitrous oxide containing a small amount of impurities is stored in a storage tube. Because the valve is opened, nitrous oxide in the storage tank is stably and continuously input into the rectifying tower, and the nitrous oxide is liquefied in the rectifying tower. And the second valve is opened periodically to discharge the impurity gas in the rectifying tower.
The liquid nitrous oxide output from the outlet is stably stored in a high-purity storage tank.
In the above rectification method of high-purity nitrous oxide, when the rectification tower is first started in step B, the second valve is opened and the first valve is closed, and after the internal pressure of the rectification tower is stabilized, the second valve is closed and the first valve is opened.
Therefore, the inner part of the rectifying tower can quickly meet the set stable operation requirement during operation.
In the rectification method of high-purity nitrous oxide, in the step B, the valve two is closed at a constant speed and slowly.
In the above rectification method of high purity nitrous oxide, the input flow rate of nitrous oxide in the step B is 110 to 150L/hr.
In the above rectification method of high purity nitrous oxide, the second valve is periodically opened in the step C.
And the second valve is opened once every 24 hours, so that the impurity gas in the rectifying tower can be effectively discharged.
In the above rectification method of high-purity nitrous oxide, the temperature in the rectification column in the step C is-80 ℃ to-86 ℃.
In the above method for rectifying high-purity nitrous oxide, in the step D, the high-purity nitrous oxide in the high-purity storage tank is sampled.
Compared with the prior art, the rectification method of the high-purity nitrous oxide can ensure that the rectification tower can quickly enter the operation state, so the operation efficiency is high.
Meanwhile, the periodically opened valve II can further improve the purity of the nitrous oxide, and has higher stability and higher practical value.
Drawings
FIG. 1 is a schematic cross-sectional view of an inlet assembly in a rectification column for rectification of high purity nitrous oxide.
In the figure, 1, connecting pipe; 1a, blocking edges; 2. a sealing seat; 2a, a first through hole; 2b, a contact edge; 2c, a positioning part; 3. a spring; 4. a ball; 5. a plug; 5a and a second through hole.
Detailed Description
Example one
A method for rectifying high-purity nitrous oxide, comprising the following steps:
A. storing materials: storing the liquid nitrous oxide containing impurities in a storage tank;
B. preparing for rectification: the rectifying tower is provided with an inlet, an exhaust port and an outlet which are communicated with the inner cavity of the rectifying tower, the inlet is connected with a first valve capable of being opened and closed, the exhaust port is connected with a second valve capable of being opened and closed, the first valve is opened and the second valve is closed in an initial state, and the outlet is communicated with the high-purity storage tank;
C. and (3) rectification: inputting the nitrous oxide into a rectifying tower from an inlet, removing a small amount of nitrogen, oxygen and hydrogen contained in the nitrous oxide through the rectifying tower, and periodically opening a second valve in the operation process of the rectifying tower;
D. storage tank: inputting the rectified high-purity nitrous oxide into a high-purity storage tank for storage.
And B, when the rectifying tower is started for the first time in the step B, opening a second valve and closing the first valve, and after the internal pressure of the rectifying tower is stable, closing the second valve and opening the first valve.
And B, closing the second valve slowly at a constant speed in the step B.
The input flow rate of the nitrous oxide in the step B is 110L/h.
And C, periodically opening a second valve.
And C, controlling the temperature in the rectifying tower in the step C to be-80 ℃.
And D, performing spot inspection on the high-purity nitrous oxide in the high-purity storage tank.
The ordinary gaseous nitrous oxide containing a small amount of impurities is stored in a storage tube. Because the valve is opened, nitrous oxide in the storage tank is stably and continuously input into the rectifying tower, and the nitrous oxide is liquefied in the rectifying tower. And the second valve is opened periodically to discharge the impurity gas in the rectifying tower.
The liquid nitrous oxide output from the outlet is stably stored in a high-purity storage tank.
The nitrous oxide component content after spot inspection is as follows:
as shown in fig. 1, the inlet assembly for the rectification column for rectifying high-purity nitrous oxide comprises a tubular connecting pipe 1, wherein the inner end of the connecting pipe 1 is used for being fixedly connected with the rectification column, the connecting pipe 1 is communicated with the inner cavity of the rectification column, the inlet assembly further comprises a sealing seat 2, a spring 3, a ball 4 and a plug 5 which are positioned in the connecting pipe 1, the sealing seat 2 is connected to the outer end of the connecting pipe 1 and is provided with a first through hole 2a which penetrates through the sealing seat, the plug 5 is connected to the inner end of the connecting pipe 1 and is provided with a second through hole 5a which penetrates through the connecting pipe, the spring 3 and the ball 4 are positioned between the plug 5 and the sealing seat 2, and the ball 4 is abutted to the port of the first through hole 2a under the elastic force of the spring 3 and has.
The inlet assembly creatively positions the spring 3 and the ball 4 in the connecting pipe 1 stably through the plug 5 and the sealing seat 2, and the ball 4 has the tendency of plugging the through hole I2 a under the elastic force action of the spring 3.
That is, the connection pipe 1 is in a closed state at the initial state. When external gas medium is input, the ball 4 is separated from the sealing seat 2 after overcoming the elasticity of the spring 3 under the action of air pressure, and the external gas medium smoothly enters the rectifying tower through the connecting pipe 1.
The port of the through hole I2 a of the sealing seat 2 is provided with a concave contact edge 2b, and the contact edge 2b is in surface contact with the ball 4.
The structure can effectively improve the sealing performance between the ball 4 and the sealing seat 2.
The outer end of the connecting pipe 1 is provided with a blocking edge 1a protruding inwards, the sealing seat 2 abuts against the blocking edge 1a, and the plug 5 is in threaded connection with the connecting pipe 1.
The upper end of the sealing seat 2 is provided with a concave positioning part 2c, the blocking edge 1a is matched with the positioning part 2c, and the blocking edge 1a is embedded in the positioning part 2 c.
The upper end of the sealing seat 2 is flush with the outer end of the connecting pipe 1.
The stable threaded connection of end cap 5 is in connecting pipe 1, and stable the supporting of seal receptacle 2 is kept off along 1a, and such structure enables whole import subassembly connection stability height.
Example two
A method for rectifying high-purity nitrous oxide, comprising the following steps:
A. storing materials: storing the liquid nitrous oxide containing impurities in a storage tank;
B. preparing for rectification: the rectifying tower is provided with an inlet, an exhaust port and an outlet which are communicated with the inner cavity of the rectifying tower, the inlet is connected with a first valve capable of being opened and closed, the exhaust port is connected with a second valve capable of being opened and closed, the first valve is opened and the second valve is closed in an initial state, and the outlet is communicated with the high-purity storage tank;
C. and (3) rectification: inputting the nitrous oxide into a rectifying tower from an inlet, removing a small amount of nitrogen, oxygen and hydrogen contained in the nitrous oxide through the rectifying tower, and periodically opening a second valve in the operation process of the rectifying tower;
D. storage tank: inputting the rectified high-purity nitrous oxide into a high-purity storage tank for storage.
And B, when the rectifying tower is started for the first time in the step B, opening a second valve and closing the first valve, and after the internal pressure of the rectifying tower is stable, closing the second valve and opening the first valve.
And B, closing the second valve slowly at a constant speed in the step B.
The input flow rate of the nitrous oxide in the step B is 150L/h.
And C, periodically opening a second valve.
And C, controlling the temperature in the rectifying tower in the step C to be-86 ℃.
And D, performing spot inspection on the high-purity nitrous oxide in the high-purity storage tank.
The ordinary gaseous nitrous oxide containing a small amount of impurities is stored in a storage tube. Because the valve is opened, nitrous oxide in the storage tank is stably and continuously input into the rectifying tower, and the nitrous oxide is liquefied in the rectifying tower. And the second valve is opened periodically to discharge the impurity gas in the rectifying tower.
The liquid nitrous oxide output from the outlet is stably stored in a high-purity storage tank.
The nitrous oxide component content after spot inspection is as follows:
EXAMPLE III
A method for rectifying high-purity nitrous oxide, comprising the following steps:
A. storing materials: storing the liquid nitrous oxide containing impurities in a storage tank;
B. preparing for rectification: the rectifying tower is provided with an inlet, an exhaust port and an outlet which are communicated with the inner cavity of the rectifying tower, the inlet is connected with a first valve capable of being opened and closed, the exhaust port is connected with a second valve capable of being opened and closed, the first valve is opened and the second valve is closed in an initial state, and the outlet is communicated with the high-purity storage tank;
C. and (3) rectification: inputting the nitrous oxide into a rectifying tower from an inlet, removing a small amount of nitrogen, oxygen and hydrogen contained in the nitrous oxide through the rectifying tower, and periodically opening a second valve in the operation process of the rectifying tower;
D. storage tank: inputting the rectified high-purity nitrous oxide into a high-purity storage tank for storage.
And B, when the rectifying tower is started for the first time in the step B, opening a second valve and closing the first valve, and after the internal pressure of the rectifying tower is stable, closing the second valve and opening the first valve.
And B, closing the second valve slowly at a constant speed in the step B.
The input flow rate of the nitrous oxide in the step B is 14L/h.
And C, periodically opening a second valve.
And C, controlling the temperature in the rectifying tower in the step C to be-82 ℃.
And D, performing spot inspection on the high-purity nitrous oxide in the high-purity storage tank.
The ordinary gaseous nitrous oxide containing a small amount of impurities is stored in a storage tube. Because the valve is opened, nitrous oxide in the storage tank is stably and continuously input into the rectifying tower, and the nitrous oxide is liquefied in the rectifying tower. And the second valve is opened periodically to discharge the impurity gas in the rectifying tower.
The liquid nitrous oxide output from the outlet is stably stored in a high-purity storage tank.
The nitrous oxide component content after spot inspection is as follows:
Claims (7)
1. a method for rectifying high-purity nitrous oxide, comprising the following steps:
A. storing materials: storing nitrous oxide containing impurities in a storage tank;
B. preparing for rectification: the rectifying tower is provided with an inlet, an exhaust port and an outlet which are communicated with the inner cavity of the rectifying tower, the inlet is connected with a first valve capable of being opened and closed, the exhaust port is connected with a second valve capable of being opened and closed, the first valve is opened and the second valve is closed in an initial state, and the outlet is communicated with the high-purity storage tank;
C. and (3) rectification: inputting the nitrous oxide into a rectifying tower from an inlet, removing a small amount of nitrogen, oxygen and hydrogen contained in the nitrous oxide through the rectifying tower, and periodically opening a second valve in the operation process of the rectifying tower;
D. storage tank: inputting the rectified high-purity nitrous oxide into a high-purity storage tank for storage.
2. The method for rectifying high-purity nitrous oxide according to claim 1, wherein when the rectifying tower is first started in step B, the second valve is opened and the first valve is closed, and after the internal pressure of the rectifying tower is stabilized, the second valve is closed and the first valve is opened.
3. The method for rectifying high-purity nitrous oxide according to claim 2, wherein in the step B, a second valve is closed at a constant speed and slowly.
4. The method for rectifying high purity nitrous oxide according to claim 3, wherein an input flow rate of nitrous oxide in said step B is 110 to 150L/hr.
5. The method for rectifying high purity nitrous oxide according to claim 4, wherein a second valve is periodically opened in said step C.
6. The method for rectifying high-purity nitrous oxide according to claim 5, wherein a temperature in the rectifying tower in the step C is 80%OC—86OC。
7. The method for rectifying high purity nitrous oxide according to claim 6, wherein the high purity nitrous oxide in the high purity storage tank is sampled in the step D.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201911030824.2A CN110980670A (en) | 2019-10-28 | 2019-10-28 | Rectification method of high-purity nitrous oxide |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201911030824.2A CN110980670A (en) | 2019-10-28 | 2019-10-28 | Rectification method of high-purity nitrous oxide |
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| CN201911030824.2A Pending CN110980670A (en) | 2019-10-28 | 2019-10-28 | Rectification method of high-purity nitrous oxide |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0636576A1 (en) * | 1993-07-26 | 1995-02-01 | Teisan Kabushiki Kaisha | Ultra-high purity nitrous oxide producing method and unit |
| CN106335884A (en) * | 2016-03-17 | 2017-01-18 | 宁波工程学院 | Method for separating and preparing electronic grade nitrous oxide from medical grade nitrous oxide |
| CN107158733A (en) * | 2017-06-06 | 2017-09-15 | 淮阴工学院 | A kind of acetic acid rectifying column of good separating effect |
-
2019
- 2019-10-28 CN CN201911030824.2A patent/CN110980670A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0636576A1 (en) * | 1993-07-26 | 1995-02-01 | Teisan Kabushiki Kaisha | Ultra-high purity nitrous oxide producing method and unit |
| CN106335884A (en) * | 2016-03-17 | 2017-01-18 | 宁波工程学院 | Method for separating and preparing electronic grade nitrous oxide from medical grade nitrous oxide |
| CN107158733A (en) * | 2017-06-06 | 2017-09-15 | 淮阴工学院 | A kind of acetic acid rectifying column of good separating effect |
Non-Patent Citations (3)
| Title |
|---|
| 侯奎源: "《化工自动化基础》", 30 April 1994 * |
| 王建成等: "《化工原理实验》", 30 September 2007 * |
| 王银锁: "《过程控制系统应用与维护》", 30 April 2015 * |
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Application publication date: 20200410 |