CN210480875U - Carbonyl fluoride's purification device - Google Patents
Carbonyl fluoride's purification device Download PDFInfo
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- CN210480875U CN210480875U CN201921539237.1U CN201921539237U CN210480875U CN 210480875 U CN210480875 U CN 210480875U CN 201921539237 U CN201921539237 U CN 201921539237U CN 210480875 U CN210480875 U CN 210480875U
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Abstract
The utility model discloses a carbonyl fluoride's purification device, including the raw materials storage tank that is used for saving crude carbonyl fluoride and the product storage tank that is used for saving high-purity carbonyl fluoride, still including the cold trap equipment that is arranged in the export of preliminary desorption carbonyl fluoride high boiling point component, a adsorption system that is arranged in further desorption carbonyl fluoride high boiling point component export and the rectification system of low boiling point component export and is arranged in desorption carbonyl fluoride impurity, the exit linkage of raw materials storage tank is to the entry of cold trap equipment, the low boiling point component exit linkage of cold trap equipment is to the entry of rectification system, the exit linkage of rectification system is to adsorption system's entry, adsorption system's exit linkage is to the product storage tank. The utility model discloses a low temperature cold trap combines worker of rectification, absorptionSelecting proper technological parameters, adding HCl and CO2And COF2The effective separation is carried out, and the carbonyl fluoride purity is greatly improved.
Description
Technical Field
The utility model relates to a purification field, concretely relates to carbonyl fluoride's purification device.
Background
Carbonyl fluoride (COF)2) Also called carbon-based fluorine and fluorophosphates, is an irritant, non-flammable, colorless and toxic gas at normal temperature. In recent years, COF2Cleaning gas and etching gas for semiconductor manufacturing apparatus, fluorinated gas and raw material of organic compound, intermediate of organic synthesis, and fluorinating agent, and COF of high purity is required as cleaning gas for semiconductor manufacturing apparatus2Are receiving increasing attention.
However, in the crude carbonyl fluoride synthesized in the prior art, HCl, HF and COCl may be possibly2、CF4、CO2、CO、N2And O2Equal impurities, at normal pressure, COF2Has a boiling point of-84.57 deg.C, HCl has a boiling point of-85 deg.C, HF has a boiling point of 19.52 deg.C, and COCl2Has a boiling point of 7.56 ℃ and CF4Has a boiling point of-128.06 ℃ and CO2The boiling point of (A) is-78.45 ℃, the boiling point of CO is-191.45 ℃, and N is2Has a boiling point of-195.8 ℃ and O2The boiling point of (A) is-182.98 ℃; wherein, COF2With HCl, CO2Are less closely different in boiling point and therefore separation is more difficult, for COF2Purification and separation from HCl, and Chinese patent CN200980139487 introduces a separation COF2And HCl, will contain COF2Mixtures with HCl and with HCl azeotropes but with COF2Organic solvents not in azeotropic relationship are mixed and rectified to separate COF2. For COF2And CO2The purification and separation of (1) can be carried out by a conventional simple adsorption method because the boiling points of the two are very close to each other and the physicochemical properties and the molecular sizes of the two are relatively close to each other,The rectification method has great difficulty in purification and separation; in addition, due to COF2And CO2Both are easily reacted with alkaline substances, and thus separation of both by neutralization is also difficult.
Disclosure of Invention
The utility model aims at providing a carbonyl fluoride's purification device adopts cryotrap to combine rectification, absorbent technology, selects suitable technological parameter, with HCl and CO2And COF2The effective separation is carried out, and the carbonyl fluoride purity is greatly improved.
In order to achieve the above purpose, the utility model adopts the technical scheme that: a carbonyl fluoride purification device comprises a raw material storage tank for storing crude carbonyl fluoride and a product storage tank for storing high-purity carbonyl fluoride, and further comprises a cold trap device for preliminarily removing a high-boiling-point component outlet in carbonyl fluoride, a rectification system for further removing the high-boiling-point component outlet and a low-boiling-point component outlet in carbonyl fluoride and an adsorption system for removing impurities in carbonyl fluoride, wherein an outlet of the raw material storage tank is connected to an inlet of the cold trap device, a low-boiling-point component outlet of the cold trap device is connected to an inlet of the rectification system, an outlet of the rectification system is connected to an inlet of the adsorption system, and an outlet of the adsorption system is connected to the product storage tank.
Further, the low boiling point component outlet of the cold trap device is close to the upper end thereof, and the high boiling point component outlet of the cold trap device is close to the lower end thereof.
Further, the rectifying system comprises a first-stage rectifying tower, a second-stage rectifying tower, a third-stage rectifying tower and a fourth-stage rectifying tower, wherein the low-boiling component outlet of the cold trap device is connected to the material inlet of the first-stage rectifying tower, the high-boiling component outlet of the first-stage rectifying tower is connected to the material inlet of the second-stage rectifying tower, the low-boiling component outlet of the second-stage rectifying tower is connected to the material inlet of the third-stage rectifying tower, the low-boiling component outlet of the third-stage rectifying tower is connected to the material inlet of the first-stage rectifying tower, the high-boiling component outlet of the third-stage rectifying tower is connected to the material inlet of the fourth-stage rectifying tower, the high-boiling component outlet of the fourth-stage rectifying tower is connected to the material inlet of the second-stage rectifying tower, and the low-boiling component outlet of the fourth-rectifying tower is connected to the inlet of the adsorption system.
Furthermore, the material inlet of the first-stage rectifying tower and the material inlet of the third-stage rectifying tower are close to the respective upper ends thereof, and the material inlet of the second-stage rectifying tower and the material inlet of the fourth-stage rectifying tower are close to the respective lower ends thereof.
Further, the low boiling point component outlet of the rectifying tower is close to the upper end of the rectifying tower, and the high boiling point component outlet of the rectifying tower is close to the lower end of the rectifying tower.
Further, the adsorption system comprises an adsorption tower.
Further, the adsorption tower is a pressure swing adsorption tower.
Further, the inlet of the adsorption tower is close to the lower end of the adsorption tower, and the outlet of the adsorption tower is close to the upper end of the adsorption tower.
Because of the application of the technical scheme, compared with the prior art, the utility model has the following advantages:
1) the utility model discloses a carbonyl fluoride's purification device adopts cold trap equipment to carry out heavy processing of taking off to crude carbonyl fluoride, makes heavy ends impurity (fluorine-containing compound, carbon dioxide etc.) content greatly reduced, reduces the heat and the cold volume of follow-up rectification purification, reduces adsorbent desorption number of times, improves product yield and purity, and economic nature is good;
2) the utility model discloses a carbonyl fluoride's purification device, through control rectification parameter, utilize the light heavy component of rectification purifying column T03, T04 to flow back respectively and carry out further rectification purification in purifying column T01, T02, cold volume and heat in the rectification process have been reduced, impurity content has also further been reduced simultaneously, gaseous purity has been improved, enable impurity concentration after the purification and fall to below the standard, it is greater than 99.9% carbonyl fluoride to obtain purity.
Drawings
Fig. 1 is a schematic structural diagram of a carbonyl fluoride purification apparatus disclosed in the present invention.
Wherein, 10, a raw material storage tank; 20. a product storage tank; 30. a cold trap device; 41. a primary rectifying tower; 42. a secondary rectification column; 43. a third-stage rectifying tower; 44. a fourth-stage rectifying tower; 51. an adsorption tower.
Detailed Description
The invention will be further described with reference to the accompanying drawings and examples:
referring to fig. 1, as shown in the figure, a carbonyl fluoride purification device comprises a raw material storage tank 10 for storing crude carbonyl fluoride and a product storage tank 20 for storing high-purity carbonyl fluoride, and further comprises a cold trap device 30 for primarily removing a high-boiling-point component outlet in carbonyl fluoride, a rectification system for further removing the high-boiling-point component outlet and a low-boiling-point component outlet in carbonyl fluoride, and an adsorption system for removing impurities in carbonyl fluoride, wherein an outlet of the raw material storage tank 10 is connected to an inlet of the cold trap device 30, the low-boiling-point component outlet of the cold trap device 30 is connected to an inlet of the rectification system, an outlet of the rectification system is connected to an inlet of the adsorption system, and an outlet of the adsorption system is connected to the product storage tank 20.
In this embodiment, the low boiling point component outlet of the cold trap device 30 is near its upper end, and the high boiling point component outlet of the cold trap device 30 is near its lower end.
In this embodiment, the rectifying system includes a first-stage rectifying tower 41, a second-stage rectifying tower 42, a third-stage rectifying tower 43 and a fourth-stage rectifying tower 44, a low boiling point component outlet of the cold trap device 30 is connected to a material inlet of the first-stage rectifying tower 41, a high boiling point component outlet of the first-stage rectifying tower 41 is connected to a material inlet of the second-stage rectifying tower 42, a low boiling point component outlet of the second-stage rectifying tower 42 is connected to a material inlet of the third-stage rectifying tower 43, a low boiling point component outlet of the third-stage rectifying tower 43 is connected to a material inlet of the first-stage rectifying tower 41, a high boiling point component outlet of the third-stage rectifying tower 43 is connected to a material inlet of the fourth-stage rectifying tower 44, a high boiling point component outlet of the fourth-stage rectifying tower 44 is connected to a material inlet of the second-stage rectifying tower 42, and a low boiling point component outlet.
In this embodiment, the material inlet of the first-stage rectifying tower 41 and the material inlet of the third-stage rectifying tower 43 are close to their respective upper ends, and the material inlet of the second-stage rectifying tower 42 and the material inlet of the fourth-stage rectifying tower 44 are close to their respective lower ends.
In this embodiment, the outlet for the low boiling point component of the rectifying column is near its upper end, and the outlet for the high boiling point component of the rectifying column is near its lower end.
In this embodiment, the adsorption system includes an adsorption tower 51.
In this embodiment, the adsorption column 51 is a pressure swing adsorption column.
In this embodiment, the inlet of the adsorption tower 51 is near its lower end, and the outlet of the adsorption tower 51 is near its upper end.
The work flow of the present invention is described as follows:
1. the method comprises the following steps of firstly feeding a raw material crude product COF2 into a cold trap device with the temperature of about-81 ℃, heating at the heating rate of 0.01-0.1 ℃/min, carrying out weight removal treatment when the temperature is between-81 ℃ and-55 ℃, introducing treated carbonyl fluoride gas into a primary rectifying tower, stopping introducing the carbonyl fluoride gas into the primary rectifying tower when the temperature is more than-55 ℃, and removing high-boiling-point components in the cold trap device as heavy components;
2. the low boiling point component which is primarily subjected to the coarse product of the weight removal COF2 is subjected to light weight removal treatment in a primary rectifying tower, the temperature at the bottom of the tower is between 120 ℃ below zero and 90 ℃ below zero, the pressure is between 0.01 and 1MPa, the temperature at the top of the tower is 1 to 25 ℃ lower than that at the bottom of the tower, and the pressure is between 0.01 and 1MPa, the low boiling point material extracted from the top of the tower directly enters a low boiling point component impurity tank, and the material at the bottom of the tower enters a secondary rectifying;
3. the temperature of the bottom of the secondary rectifying tower is-81 ℃ to 90 ℃, the pressure is 0.01 to 1MPa, the temperature of the top is 1 to 25 ℃ lower than that of the bottom, high boiling point substances discharged from the bottom of the secondary rectifying tower directly enter a waste liquid tank, and a COF2 crude product subjected to primary rectification at the top of the secondary rectifying tower is introduced into a tertiary rectifying tower;
4. the tower low temperature of the third-stage rectifying tower is-130 ℃ to-85 ℃, the pressure is 0.01 to 1.2MPa, the top temperature is 0.5 to 45 ℃ lower than the bottom temperature, and the pressure is 0.01 to 1.2MPa, low boiling point substances extracted from the tower top directly enter a first-stage rectifying tower, and materials at the tower bottom enter a fourth-stage rectifying tower for weight removal treatment;
5. the bottom temperature of the four-stage rectifying tower is-82 deg.C to 70 deg.C, the pressure is 0.01 to 1.2MPa, and the top temperature is 0.5 to 45 deg.C lower than the bottom temperature0.01 to 1.2MPa, introducing the material at the bottom of the tower into a secondary rectifying tower, and obtaining a rectified COF at the top of the tower2Introducing into an adsorption tower;
6. performing pressure adsorption in an adsorption tower to obtain COF2Purifying the gas, wherein the adsorption pressure is 0.1 to 0.7MPa, the adsorption temperature is-30 ℃ to 40 ℃, the gas after adsorption is directly introduced into a product storage tank, and the purity of the gas after purification is more than 99.9 percent or even higher.
In steps 2,3 and 4, a step of mixing a mixture containing the carbonyl fluoride and the hydrogen chloride with an organic solvent that is azeotropic with hydrogen chloride but not azeotropic with carbonyl fluoride, and distilling the mixture to separate carbonyl fluoride. In step 5, the adsorbent in the adsorption tower is one or more of activated carbon, molecular sieve or carbon molecular sieve.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (8)
1. A carbonyl fluoride purification device comprises a raw material storage tank for storing crude carbonyl fluoride and a product storage tank for storing high-purity carbonyl fluoride, and is characterized by further comprising a cold trap device for preliminarily removing a high-boiling-point component outlet in carbonyl fluoride, a rectification system for further removing the high-boiling-point component outlet and a low-boiling-point component outlet in carbonyl fluoride and an adsorption system for removing impurities in carbonyl fluoride, wherein an outlet of the raw material storage tank is connected to an inlet of the cold trap device, the low-boiling-point component outlet of the cold trap device is connected to an inlet of the rectification system, an outlet of the rectification system is connected to an inlet of the adsorption system, and an outlet of the adsorption system is connected to the product storage tank.
2. The purification apparatus of claim 1, wherein the low boiling point component outlet of the cold trap device is near its upper end and the high boiling point component outlet of the cold trap device is near its lower end.
3. The purification apparatus of claim 1, wherein the rectification system comprises a first rectification column, a second rectification column, a third rectification column, and a fourth rectification column, the low boiling point component outlet of the cold trap device is connected to the material inlet of the first-stage rectifying tower, the high boiling point component outlet of the first-stage rectifying tower is connected to the material inlet of the second-stage rectifying tower, the low boiling point component outlet of the second-stage rectifying tower is connected to the material inlet of the third-stage rectifying tower, the low boiling point component outlet of the third-stage rectifying tower is connected to the material inlet of the first-stage rectifying tower, the high boiling point component outlet of the third-stage rectifying tower is connected to the material inlet of the fourth-stage rectifying tower, and a high-boiling-point component outlet of the fourth-stage rectifying tower is connected to a material inlet of the second-stage rectifying tower, and a low-boiling-point component outlet of the fourth-stage rectifying tower is connected to an inlet of the adsorption system.
4. The purification apparatus of claim 3, wherein the feed inlet of the first rectification column and the feed inlet of the third rectification column are proximate their respective upper ends, and the feed inlet of the second rectification column and the feed inlet of the fourth rectification column are proximate their respective lower ends.
5. The purification apparatus of claim 3, wherein the lower boiling component outlet of the rectification column is proximate its upper end and the higher boiling component outlet of the rectification column is proximate its lower end.
6. The purification apparatus of claim 1, wherein the adsorption system comprises an adsorption column.
7. The purification apparatus of claim 6, wherein the adsorption column is a pressure swing adsorption column.
8. The purification apparatus of claim 6, wherein the inlet of the adsorption column is near its lower end and the outlet of the adsorption column is near its upper end.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201921539237.1U CN210480875U (en) | 2019-09-17 | 2019-09-17 | Carbonyl fluoride's purification device |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201921539237.1U CN210480875U (en) | 2019-09-17 | 2019-09-17 | Carbonyl fluoride's purification device |
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| CN210480875U true CN210480875U (en) | 2020-05-08 |
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| CN201921539237.1U Active CN210480875U (en) | 2019-09-17 | 2019-09-17 | Carbonyl fluoride's purification device |
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Address after: 215152 Anmin Road, Panyang Industrial Park, Huangdai Town, Xiangcheng District, Suzhou City, Jiangsu Province Patentee after: Jinhong Gas Co.,Ltd. Address before: 215152 No. 6 Anmin Road, Panyang Industrial Park, Huangdi Town, Xiangcheng District, Suzhou City, Jiangsu Province Patentee before: SUZHOU JINHONG GAS Co.,Ltd. |
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