CN111978146A - Purification system and purification method of octafluorocyclobutane - Google Patents
Purification system and purification method of octafluorocyclobutane Download PDFInfo
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- CN111978146A CN111978146A CN202010884681.8A CN202010884681A CN111978146A CN 111978146 A CN111978146 A CN 111978146A CN 202010884681 A CN202010884681 A CN 202010884681A CN 111978146 A CN111978146 A CN 111978146A
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Abstract
The invention provides a purifying system of octafluorocyclobutane, and belongs to the technical field of chemical industry. It has solved prior art and has had the poor problem of stability. The octafluorocyclobutane purification system comprises a rack, wherein a first drying absorber, a compressor, a condenser, a rectifying tower, a qualified product tank and a second drying absorber are sequentially connected in series on the rack, the first drying absorber is provided with an inlet communicated with a crude product, and the second drying absorber is provided with an outlet connected with a finished product storage position. This octafluorocyclobutane's purification system stability is high.
Description
Technical Field
The invention belongs to the technical field of chemical industry, and relates to a purification system of octafluorocyclobutane.
Background
The existing octafluorocyclobutane purification process mainly adopts an extractive distillation method or a single adsorption method for treatment.
The extractive distillation method has expensive equipment cost and complicated procedures, needs higher technical talents and is not suitable for large-scale production.
The single adsorption method is difficult to remove impurities with similar physical properties and structures, and octafluorocyclobutane produced by different processes has different impurities and is difficult to adapt to different crude products.
Disclosure of Invention
The first purpose of the present invention is to provide a purification system of octafluorocyclobutane with high stability and good purification effect, which addresses the above problems of the prior art.
The second purpose of the invention is to provide a purification method adopted by the purification system of the octafluorocyclobutane.
The first object of the present invention can be achieved by the following technical solutions:
the octafluorocyclobutane purification system comprises a rack and is characterized in that a first drying absorber, a compressor, a condenser, a rectifying tower, a qualified product tank and a second drying absorber are sequentially connected to the rack in series, wherein the first drying absorber is provided with an inlet communicated with a crude product, and the second drying absorber is provided with an outlet connected with a finished product storage position.
Introducing the crude product of octafluorocyclobutane into a dry adsorber, adsorbing by using a molecular sieve adsorbent to remove most of water and other impurities in the crude product to obtain a crude product, removing part of non-condensable gases (mainly comprising nitrogen, carbon monoxide, oxygen, carbon dioxide, part of halohydrocarbon compounds and the like and a small amount of octafluorocyclobutane) from the crude product by compression and condensation, pressurizing to about 0.5MPa, keeping the temperature at 0-25 ℃, introducing the liquefied octafluorocyclobutane into a rectifying tower, and detecting the properties of the halohydrocarbon compounds according to raw materials, by adjusting the pressure in the thermometer rectifying tower of the reboiler at the bottom of the tower and the condenser at the top of the tower, the temperature and the pressure of the solution in the rectifying tower are kept stable, impurities with similar boiling points can be removed, the solution enters a product dryer after being analyzed to be qualified, removing impurities such as water and carbon dioxide to obtain refined octafluorocyclobutane (not less than 99.999%).
In the above-described purification system for octafluorocyclobutane, the inlet is located at the lower part of the first dry adsorber.
In the above-mentioned purification system for octafluorocyclobutane, the outlet is located at the upper part of the second dry adsorber.
The second object of the present invention can be achieved by the following technical solutions:
a method for purifying octafluorocyclobutane, which comprises the following steps:
A. adsorption: inputting the gaseous octafluorocyclobutane crude product into a drying adsorber, and performing drying adsorption to obtain an octafluorocyclobutane crude product;
B. liquefaction: pressurizing and inputting the crude product of the octafluorocyclobutane to a condenser by a compressor, cooling the crude product of the octafluorocyclobutane by the condenser to obtain liquid octafluorocyclobutane, and removing part of non-condensable gas in the process;
C. canning: introducing liquefied octafluorocyclobutane into a rectifying tower, heating the rectifying tower, condensing the tower top, keeping the pressure, the temperature and the liquid level in the rectifying tower stable, ensuring the whole reflux time in the rectifying tower to be 4-6 hours, ensuring the temperature of a condenser to be-25-5 ℃, ensuring the temperature of a reboiler at the tower bottom of the rectifying tower to be 20-40 ℃, ensuring the pressure in the rectifying tower to be 0.2-0.5 MPa, slowly stopping supplying a cold and heat source after the reflux is finished, keeping the liquid level stable, removing gaseous impurities from a condenser at the tower top of the rectifying tower and collecting the gaseous impurities, and introducing a product at the tower bottom of the rectifying tower into a qualified product tank through an additional pressure pump after the product at the tower bottom is qualified;
D. and (3) purification: and (3) gasifying the medium in the qualified product tank, introducing the gasified medium into a drying adsorption tower, and removing impurities such as water, carbon dioxide, halohydrocarbon compounds and the like in the qualified product to obtain a finished product of the octafluorocyclobutane with the concentration of 99.999%.
In the above-mentioned purification method of octafluorocyclobutane, the purity of the crude octafluorocyclobutane in step A is 99%.
In the purification method of octafluorocyclobutane, in the step C, a reboiler at the bottom of the tower adopts water or heat-conducting oil as a heat source, the temperature is 40-100 ℃, the working pressure in the tower is 0.2-0.5 MPa, and the reflux time is 4-6 hours.
In the above-mentioned method for purifying octafluorocyclobutane, in the step C, the temperatures of the condenser at the top and the reboiler at the bottom of the rectifying column are adjusted, and the pressure in the column is adjusted according to the properties of the halocarbon compound detected as the raw material.
Compared with the prior art, the octafluorocyclobutane purification system has the advantages that the equipment cost of each part is relatively low, and the treatment requirement is relatively low, so that the stability is high, and the purification effect is good.
The method for purifying the octafluorocyclobutane adopts an intermittent rectification mode to purify the crude octafluorocyclobutane (99%) gas, has high phase separation efficiency and strong separation capacity of light components, can ensure that the purity of the purified octafluorocyclobutane is not less than 99.999 percent, can be used in the semiconductor industry or other related industries, and has high practical value.
Drawings
FIG. 1 is a schematic diagram showing the structure of a purification system for octafluorocyclobutane.
In the figure, 1, a first drying adsorber; 1a, an inlet; 2. a compressor; 3. a condenser; 4. a rectifying tower; 5. qualified product cans; 6. drying the second adsorber; 6a and an outlet.
Detailed Description
Example one
As shown in fig. 1, the octafluorocyclobutane purification system comprises a frame, wherein a first drying adsorber 1, a compressor 2, a condenser 3, a rectifying tower 4, a qualified product tank 5 and a second drying adsorber 6 are sequentially connected in series on the frame, the first drying adsorber 1 is provided with an inlet 1a for communicating with a crude product, and the second drying adsorber 6 is provided with an outlet 6a for connecting with a finished product storage place.
The inlet 1a is located at the lower part of the first drying adsorber 1.
The outlet 6a is located at the upper part of the second drying adsorber 6.
The purification method of octafluorocyclobutane comprises the following steps:
A. adsorption: inputting the gaseous octafluorocyclobutane crude product into a drying adsorber, and performing drying adsorption to obtain an octafluorocyclobutane crude product;
B. liquefaction: pressurizing and inputting the crude product of the octafluorocyclobutane to a condenser by a compressor, cooling the crude product of the octafluorocyclobutane by the condenser to obtain liquid octafluorocyclobutane, and removing part of non-condensable gas in the process;
C. canning: introducing liquefied octafluorocyclobutane into a rectifying tower, heating the rectifying tower, condensing the tower top, keeping the pressure, the temperature and the liquid level in the rectifying tower stable, ensuring the whole reflux time in the rectifying tower to be 4 hours, the temperature of a condenser to be-25 ℃, the temperature of a reboiler at the tower bottom of the rectifying tower to be 20 ℃, the pressure in the rectifying tower to be 0.2MPa, slowly stopping supplying cold and heat sources after the reflux is finished, keeping the liquid level stable, removing gaseous impurities from the condenser at the tower top of the rectifying tower and collecting the gaseous impurities, and introducing a product at the tower bottom of the rectifying tower into a qualified product tank by adding a pressure pump after the product at the tower bottom of the rectifying tower is qualified;
D. and (3) purification: and (3) gasifying the medium in the qualified product tank, introducing the gasified medium into a drying adsorption tower, and removing impurities such as water, carbon dioxide, halohydrocarbon compounds and the like in the qualified product to obtain a finished product of the octafluorocyclobutane with the concentration of 99.999%.
The purity of the crude octafluorocyclobutane in the step A is 99%.
And C, a reboiler at the bottom of the tower in the step C adopts water or heat conducting oil as a heat source, the temperature is 40 ℃, the working pressure in the tower is 0.2MPa, and the reflux time is 4 hours.
And C, in the step C, the temperatures of a condenser at the top of the rectifying tower and a reboiler at the bottom of the rectifying tower are adjusted, and the pressure in the rectifying tower is adjusted according to the properties of the halohydrocarbon compounds detected by the raw materials.
Introducing the crude product of octafluorocyclobutane into a dry adsorber, adsorbing by using a molecular sieve adsorbent to remove most of water and other impurities in the crude product to obtain a crude product, removing part of non-condensable gases (mainly comprising nitrogen, carbon monoxide, oxygen, carbon dioxide, part of halohydrocarbon compounds and the like and a small amount of octafluorocyclobutane) from the crude product by compression and condensation, pressurizing to about 0.5MPa, keeping the temperature at 0-25 ℃, introducing the liquefied octafluorocyclobutane into a rectifying tower, and detecting the properties of the halohydrocarbon compounds according to raw materials, by adjusting the pressure in the thermometer rectifying tower of the reboiler at the bottom of the tower and the condenser at the top of the tower, the temperature and the pressure of the solution in the rectifying tower are kept stable, impurities with similar boiling points can be removed, the solution enters a product dryer after being analyzed to be qualified, removing impurities such as water and carbon dioxide to obtain refined octafluorocyclobutane (not less than 99.999%).
Example two
As shown in fig. 1, the octafluorocyclobutane purification system comprises a frame, wherein a first drying adsorber 1, a compressor 2, a condenser 3, a rectifying tower 4, a qualified product tank 5 and a second drying adsorber 6 are sequentially connected in series on the frame, the first drying adsorber 1 is provided with an inlet 1a for communicating with a crude product, and the second drying adsorber 6 is provided with an outlet 6a for connecting with a finished product storage place.
The inlet 1a is located at the lower part of the first drying adsorber 1.
The outlet 6a is located at the upper part of the second drying adsorber 6.
The purification method of octafluorocyclobutane comprises the following steps:
A. adsorption: inputting the gaseous octafluorocyclobutane crude product into a drying adsorber, and performing drying adsorption to obtain an octafluorocyclobutane crude product;
B. liquefaction: pressurizing and inputting the crude product of the octafluorocyclobutane to a condenser by a compressor, cooling the crude product of the octafluorocyclobutane by the condenser to obtain liquid octafluorocyclobutane, and removing part of non-condensable gas in the process;
C. canning: introducing liquefied octafluorocyclobutane into a rectifying tower, heating the rectifying tower, condensing the tower top, keeping the pressure, the temperature and the liquid level in the rectifying tower stable, ensuring the whole reflux time in the rectifying tower to be 6 hours, the temperature of a condenser to be minus 5 ℃, the temperature of a reboiler at the tower bottom of the rectifying tower to be 40 ℃, the pressure in the rectifying tower to be 0.5MPa, slowly stopping supplying cold and heat sources after the reflux is finished, keeping the liquid level stable, removing gaseous impurities from the condenser at the tower top of the rectifying tower and collecting the gaseous impurities, and introducing a product at the tower bottom of the rectifying tower into a qualified product tank by adding a pressure pump after the product at the tower bottom of the rectifying tower is qualified;
D. and (3) purification: and (3) gasifying the medium in the qualified product tank, introducing the gasified medium into a drying adsorption tower, and removing impurities such as water, carbon dioxide, halohydrocarbon compounds and the like in the qualified product to obtain a finished product of the octafluorocyclobutane with the concentration of 99.999%.
The purity of the crude octafluorocyclobutane in the step A is 99%.
And C, a reboiler at the bottom of the tower in the step C adopts water or heat conducting oil as a heat source, the temperature is 100 ℃, the working pressure in the tower is 0.5MPa, and the reflux time is 6 hours.
And C, in the step C, the temperatures of a condenser at the top of the rectifying tower and a reboiler at the bottom of the rectifying tower are adjusted, and the pressure in the rectifying tower is adjusted according to the properties of the halohydrocarbon compounds detected by the raw materials.
Introducing the crude product of octafluorocyclobutane into a dry adsorber, adsorbing by using a molecular sieve adsorbent to remove most of water and other impurities in the crude product to obtain a crude product, removing part of non-condensable gases (mainly comprising nitrogen, carbon monoxide, oxygen, carbon dioxide, part of halohydrocarbon compounds and the like and a small amount of octafluorocyclobutane) from the crude product by compression and condensation, pressurizing to about 0.5MPa, keeping the temperature at 0-25 ℃, introducing the liquefied octafluorocyclobutane into a rectifying tower, and detecting the properties of the halohydrocarbon compounds according to raw materials, by adjusting the pressure in the thermometer rectifying tower of the reboiler at the bottom of the tower and the condenser at the top of the tower, the temperature and the pressure of the solution in the rectifying tower are kept stable, impurities with similar boiling points can be removed, the solution enters a product dryer after being analyzed to be qualified, removing impurities such as water and carbon dioxide to obtain refined octafluorocyclobutane (not less than 99.999%).
Example one
As shown in fig. 1, the octafluorocyclobutane purification system comprises a frame, wherein a first drying adsorber 1, a compressor 2, a condenser 3, a rectifying tower 4, a qualified product tank 5 and a second drying adsorber 6 are sequentially connected in series on the frame, the first drying adsorber 1 is provided with an inlet 1a for communicating with a crude product, and the second drying adsorber 6 is provided with an outlet 6a for connecting with a finished product storage place.
The inlet 1a is located at the lower part of the first drying adsorber 1.
The outlet 6a is located at the upper part of the second drying adsorber 6.
The purification method of octafluorocyclobutane comprises the following steps:
A. adsorption: inputting the gaseous octafluorocyclobutane crude product into a drying adsorber, and performing drying adsorption to obtain an octafluorocyclobutane crude product;
B. liquefaction: pressurizing and inputting the crude product of the octafluorocyclobutane to a condenser by a compressor, cooling the crude product of the octafluorocyclobutane by the condenser to obtain liquid octafluorocyclobutane, and removing part of non-condensable gas in the process;
C. canning: introducing liquefied octafluorocyclobutane into a rectifying tower, heating the rectifying tower, condensing the top of the tower, keeping the pressure, the temperature and the liquid level in the rectifying tower stable, ensuring the whole reflux time in the rectifying tower to be 5 hours, the temperature of a condenser to be-21 ℃, the temperature of a reboiler at the bottom of the rectifying tower to be 26 ℃, the pressure in the rectifying tower to be 0.4MPa, slowly stopping supplying cold and heat sources after the reflux is finished, keeping the liquid level stable, removing gaseous impurities from the condenser at the top of the rectifying tower and collecting the gaseous impurities, and introducing a product at the bottom of the rectifying tower into a qualified product tank by adding a pressure pump after the product at the bottom of the rectifying tower is qualified;
D. and (3) purification: and (3) gasifying the medium in the qualified product tank, introducing the gasified medium into a drying adsorption tower, and removing impurities such as water, carbon dioxide, halohydrocarbon compounds and the like in the qualified product to obtain a finished product of the octafluorocyclobutane with the concentration of 99.999%.
The purity of the crude octafluorocyclobutane in the step A is 99%.
And C, a reboiler at the bottom of the tower in the step C adopts water or heat conducting oil as a heat source, the temperature is 66 ℃, the working pressure in the tower is 0.3MPa, and the reflux time is 5 hours.
And C, in the step C, the temperatures of a condenser at the top of the rectifying tower and a reboiler at the bottom of the rectifying tower are adjusted, and the pressure in the rectifying tower is adjusted according to the properties of the halohydrocarbon compounds detected by the raw materials.
Introducing the crude product of octafluorocyclobutane into a dry adsorber, adsorbing by using a molecular sieve adsorbent to remove most of water and other impurities in the crude product to obtain a crude product, removing part of non-condensable gases (mainly comprising nitrogen, carbon monoxide, oxygen, carbon dioxide, part of halohydrocarbon compounds and the like and a small amount of octafluorocyclobutane) from the crude product by compression and condensation, pressurizing to about 0.5MPa, keeping the temperature at 0-25 ℃, introducing the liquefied octafluorocyclobutane into a rectifying tower, and detecting the properties of the halohydrocarbon compounds according to raw materials, by adjusting the pressure in the thermometer rectifying tower of the reboiler at the bottom of the tower and the condenser at the top of the tower, the temperature and the pressure of the solution in the rectifying tower are kept stable, impurities with similar boiling points can be removed, the solution enters a product dryer after being analyzed to be qualified, removing impurities such as water and carbon dioxide to obtain refined octafluorocyclobutane (not less than 99.999%).
Claims (7)
1. The octafluorocyclobutane purification system comprises a rack and is characterized in that a first drying absorber, a compressor, a condenser, a rectifying tower, a qualified product tank and a second drying absorber are sequentially connected to the rack in series, wherein the first drying absorber is provided with an inlet communicated with a crude product, and the second drying absorber is provided with an outlet connected with a finished product storage position.
2. The octafluorocyclobutane purification system according to claim 1, wherein the inlet is located at the lower part of the first dry adsorber.
3. The octafluorocyclobutane purification system according to claim 1, wherein the outlet is located at the upper part of the second dry adsorber.
4. A method for purifying octafluorocyclobutane, which comprises the following steps:
A. adsorption: inputting the gaseous octafluorocyclobutane crude product into a drying adsorber, and performing drying adsorption to obtain an octafluorocyclobutane crude product;
B. liquefaction: pressurizing and inputting the crude product of the octafluorocyclobutane to a condenser by a compressor, cooling the crude product of the octafluorocyclobutane by the condenser to obtain liquid octafluorocyclobutane, and removing part of non-condensable gas in the process;
C. canning: introducing liquefied octafluorocyclobutane into a rectifying tower, heating the rectifying tower, condensing the tower top, keeping the pressure, the temperature and the liquid level in the rectifying tower stable, ensuring the whole reflux time in the rectifying tower to be 4-6 hours, ensuring the temperature of a condenser to be-25-5 ℃, ensuring the temperature of a reboiler at the tower bottom of the rectifying tower to be 20-40 ℃, ensuring the pressure in the rectifying tower to be 0.2-0.5 MPa, slowly stopping supplying a cold and heat source after the reflux is finished, keeping the liquid level stable, removing gaseous impurities from a condenser at the tower top of the rectifying tower and collecting the gaseous impurities, and introducing a product at the tower bottom of the rectifying tower into a qualified product tank through an additional pressure pump after the product at the tower bottom is qualified;
D. and (3) purification: and (3) gasifying the medium in the qualified product tank, introducing the gasified medium into a drying adsorption tower, and removing impurities such as water, carbon dioxide, halohydrocarbon compounds and the like in the qualified product to obtain a finished product of the octafluorocyclobutane with the concentration of 99.999%.
5. The method for purifying octafluorocyclobutane according to claim 4, wherein the purity of the crude octafluorocyclobutane in the step A is 99%.
6. The purification method of octafluorocyclobutane according to claim 5, wherein in step C, a reboiler at the bottom of the column uses water or heat transfer oil as a heat source, the temperature is 40-100 ℃, the working pressure in the column is 0.2-0.5 MPa, and the reflux time is 4-6 hours.
7. The method for purifying octafluorocyclobutane according to claim 6, wherein the temperatures of the condenser at the top and the reboiler at the bottom of the rectification column in step C are adjusted according to the properties of the halocarbon compound detected as the raw material.
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| CN114618429A (en) * | 2020-12-10 | 2022-06-14 | 浙江蓝天环保高科技股份有限公司 | Surface modification modified ZSM-5 molecular sieve and application thereof |
| CN115043702A (en) * | 2022-07-26 | 2022-09-13 | 浙江人行道化工有限公司 | Octafluorocyclobutane and purification method thereof |
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| CN105777483A (en) * | 2016-01-28 | 2016-07-20 | 广东华特气体股份有限公司 | High-purity octafluorocyclobutane purification method and system |
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| CN105777483A (en) * | 2016-01-28 | 2016-07-20 | 广东华特气体股份有限公司 | High-purity octafluorocyclobutane purification method and system |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114618429A (en) * | 2020-12-10 | 2022-06-14 | 浙江蓝天环保高科技股份有限公司 | Surface modification modified ZSM-5 molecular sieve and application thereof |
| CN114618429B (en) * | 2020-12-10 | 2024-04-16 | 浙江蓝天环保高科技股份有限公司 | Surface-modified ZSM-5 molecular sieve and application thereof |
| CN115043702A (en) * | 2022-07-26 | 2022-09-13 | 浙江人行道化工有限公司 | Octafluorocyclobutane and purification method thereof |
| CN115043702B (en) * | 2022-07-26 | 2023-12-22 | 浙江人行道化工有限公司 | Octafluorocyclobutane and purification method thereof |
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Denomination of invention: Purification system of octafluorocyclobutane and its purification method Effective date of registration: 20210928 Granted publication date: 20210608 Pledgee: Bank of Communications Co.,Ltd. Suzhou Branch Pledgor: Suzhou Yiwei New Material Co.,Ltd. Registration number: Y2021980010008 |
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