CN113307269A - Method for preparing carbon dioxide after purification of liquid carbon dioxide - Google Patents

Method for preparing carbon dioxide after purification of liquid carbon dioxide Download PDF

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Publication number
CN113307269A
CN113307269A CN202110685720.6A CN202110685720A CN113307269A CN 113307269 A CN113307269 A CN 113307269A CN 202110685720 A CN202110685720 A CN 202110685720A CN 113307269 A CN113307269 A CN 113307269A
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carbon dioxide
purification
parts
liquid carbon
gas cylinder
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鲁侠
刘光继
邓小波
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Yunnan Anfeng Gas Co ltd
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Yunnan Anfeng Gas Co ltd
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    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00Carbon; Compounds thereof
    • C01B32/50Carbon dioxide

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  • Organic Chemistry (AREA)
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Abstract

The invention discloses a method for preparing carbon dioxide after purification of liquid carbon dioxide, which comprises the following steps of 1) conveying 99.5% of liquid carbon dioxide in a low-temperature liquid storage tank into a high-purity liquid carbon dioxide purification device for first purification, conveying the purified carbon dioxide into a vaporizer for gasification, and conveying the gasified carbon dioxide into a purifier for second purification; a breathable film is arranged in an air outlet pipe of the high-purity liquid carbon dioxide purification device; 2) purifying, detecting and testing the carbon dioxide treated by the purifier, sending the purified carbon dioxide into a diaphragm compressor after the carbon dioxide is qualified, pressurizing by 0-15 mpa, and filling into a vacuum gas cylinder; 3) testing the carbon dioxide filled in the vacuum gas cylinder, sending the carbon dioxide to a warehouse for storage after the carbon dioxide is qualified; the invention can meet the requirement of the market on carbon dioxide and can realize the requirement on the purity of the carbon dioxide, so that the purity of the carbon dioxide reaches 99.999 percent.

Description

Method for preparing carbon dioxide after purification of liquid carbon dioxide
Technical Field
The invention relates to the technical field of carbon dioxide processing, in particular to a method for preparing carbon dioxide after purifying liquid carbon dioxide.
Background
The liquid carbon dioxide has wide application, can be used as a refrigerant for preserving food, can be used for artificial rainfall, and is also an industrial raw material. Although liquid carbon dioxide is very versatile, its purity requirements are also very high.
At present, a common method of a carbon dioxide purification method is that a refrigerant cools compressed gas to about minus 25 ℃ to liquefy the compressed gas, and then rectification and purification are performed, so that noncondensable gases such as hydrogen, nitrogen, methane and the like in raw materials can be effectively removed by the method to obtain high-purity liquid carbon dioxide, but the purity of the carbon dioxide is usually 99.5%, but the carbon dioxide cannot be met and used in industries with high requirements for the purity of carbon dioxide, and a simple, convenient and rapid purification method is needed to further improve the purity of carbon dioxide.
Disclosure of Invention
The invention provides a method for preparing carbon dioxide after purifying liquid carbon dioxide.
The scheme of the invention is as follows:
a method for producing carbon dioxide after purification by liquid carbon dioxide, comprising the steps of:
1) conveying 99.5% of liquid carbon dioxide in the low-temperature liquid storage tank into a high-purity liquid carbon dioxide purification device for first purification, conveying the purified carbon dioxide into a vaporizer for gasification, and conveying the gasified carbon dioxide into a purifier for second purification; a breathable film is arranged in an air outlet pipe of the high-purity liquid carbon dioxide purification device, and comprises 50-70 parts of aromatic polyamide solution, 30-50 parts of melamine derivative, 1-2 parts of nano graphene and 3-5 parts of nano silver;
2) purifying, detecting and testing the carbon dioxide treated by the purifier, sending the purified carbon dioxide into a diaphragm compressor after the carbon dioxide is qualified, pressurizing by 0-15 mpa, and filling into a vacuum gas cylinder;
3) and testing the carbon dioxide filled in the vacuum gas cylinder, and sending the carbon dioxide to a warehouse for storage after the carbon dioxide is qualified.
As a preferable technical scheme, the stirring paddle in the purification tank of the high-purity liquid carbon dioxide purification device is a magnetic stirring paddle.
Preferably, the purifier is a carbon dioxide purifying device.
As a preferable technical solution, the purification detection assay in step 2) is performed after the carbon dioxide processed by the purifier is left for 8 hours.
Preferably, the diaphragm compressor pressurizes 0-15 mpa within 6 hours.
Preferably, the step 2) is carried out after being put into a vacuum cylinder and standing for more than 8 hours until the step 3).
Preferably, the carbon dioxide loaded in the vacuum cylinder in the step 3) is assayed by using a carbon dioxide analyzer.
As a preferable technical scheme, the carbon dioxide filled in the vacuum gas cylinder is tested in the step 3) to reach the standard of 99.999%.
As a preferred embodiment, the aromatic polyamide solution comprises 50 mol% of 4,4Diaminodiphenyl ether, 25 mol% p-phenylenediamine, 25 mol% o-dianisidine, dehydrated N-methyl-2-pyrrolidone, 100 mol% isophthaloyl chloride and lithium carbonate.
As a preferable technical scheme, the melamine derivative comprises 58 parts of formaldehyde, 40 parts of melamine, 29 parts of ethylenediamine and a proper amount of pH regulator.
Due to the adoption of the technical scheme, the method for preparing the carbon dioxide after purifying the liquid carbon dioxide comprises the following steps: 1) conveying 99.5% of liquid carbon dioxide in the low-temperature liquid storage tank into a high-purity liquid carbon dioxide purification device for first purification, conveying the purified carbon dioxide into a vaporizer for gasification, and conveying the gasified carbon dioxide into a purifier for second purification; a breathable film is arranged in an air outlet pipe of the high-purity liquid carbon dioxide purification device, and comprises 50-70 parts of aromatic polyamide solution, 30-50 parts of melamine derivative, 1-2 parts of nano graphene and 3-5 parts of nano silver; 2) purifying, detecting and testing the carbon dioxide treated by the purifier, sending the purified carbon dioxide into a diaphragm compressor after the carbon dioxide is qualified, pressurizing by 0-15 mpa, and filling into a vacuum gas cylinder; 3) and testing the carbon dioxide filled in the vacuum gas cylinder, and sending the carbon dioxide to a warehouse for storage after the carbon dioxide is qualified.
The invention has the advantages that:
the method for producing carbon dioxide disclosed by the invention can meet the requirement of the market on carbon dioxide, and can realize the requirement on the purity of the carbon dioxide while ensuring the yield, so that the purity of the carbon dioxide reaches 99.999 percent. The invention fully considers various factors to realize the operation of simple, stable, high-efficiency and low energy consumption preparation steps for producing the high-purity carbon dioxide.
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FIG. 1 is a flow chart of an embodiment of the present invention.
Detailed Description
In order to remedy the above disadvantages, the present invention provides a method for preparing carbon dioxide by purifying liquid carbon dioxide to solve the above problems in the background art.
A method for producing carbon dioxide after purification by liquid carbon dioxide, comprising the steps of:
1) conveying 99.5% of liquid carbon dioxide in the low-temperature liquid storage tank into a high-purity liquid carbon dioxide purification device for first purification, conveying the purified carbon dioxide into a vaporizer for gasification, and conveying the gasified carbon dioxide into a purifier for second purification; a breathable film is arranged in an air outlet pipe of the high-purity liquid carbon dioxide purification device, and comprises 50-70 parts of aromatic polyamide solution, 30-50 parts of melamine derivative, 1-2 parts of nano graphene and 3-5 parts of nano silver;
2) purifying, detecting and testing the carbon dioxide treated by the purifier, sending the purified carbon dioxide into a diaphragm compressor after the carbon dioxide is qualified, pressurizing by 0-15 mpa, and filling into a vacuum gas cylinder;
3) and testing the carbon dioxide filled in the vacuum gas cylinder, and sending the carbon dioxide to a warehouse for storage after the carbon dioxide is qualified.
And the stirring paddle in the purification tank of the high-purity liquid carbon dioxide purification device is a magnetic stirring paddle.
The purifier is a carbon dioxide purification device.
And the purification detection assay in the step 2) is a purification detection assay performed after the carbon dioxide treated by the purifier is kept stand for 8 hours.
The diaphragm compressor is pressurized at 0-15 mpa for 6 hours.
Step 2) is filled into a vacuum gas cylinder and stands for more than 8 hours before the step 3) is carried out.
And 3) testing the carbon dioxide filled in the vacuum gas cylinder in the step 3) by using a carbon dioxide analyzer.
And 3) testing the carbon dioxide filled in the vacuum gas cylinder in the step 3) until the standard of 99.999 percent is reached.
The aromatic polyamide solution comprises 50 mol% of 4,4Diaminodiphenyl ether, 25 mol% p-phenylenediamine, 25 mol% o-dianisidine, dehydrated N-methyl-2-pyrrolidone, 100 mol% isophthaloyl chloride and lithium carbonate.
The melamine derivative comprises 58 parts of formaldehyde, 40 parts of melamine, 29 parts of ethylenediamine and a proper amount of pH regulator.
In order to make the technical means, the creation characteristics, the achievement purposes and the effects of the invention easy to understand, the invention is further described with the specific embodiments.
Example 1:
1) conveying 99.5% of liquid carbon dioxide in the low-temperature liquid storage tank into a high-purity liquid carbon dioxide purification device for first purification, conveying the purified carbon dioxide into a vaporizer for gasification, and conveying the gasified carbon dioxide into a purifier for second purification; a breathable film is arranged in an air outlet pipe of the high-purity liquid carbon dioxide purification device, and the breathable film comprises 50 parts by weight of aromatic polyamide solution, 30 parts by weight of melamine derivative, 1 part by weight of nano graphene and 3 parts by weight of nano silver;
2) purifying, detecting and testing the carbon dioxide treated by the purifier, sending the purified carbon dioxide into a diaphragm compressor after the carbon dioxide is qualified, pressurizing by 0-15 mpa, and filling into a vacuum gas cylinder;
3) and testing the carbon dioxide filled in the vacuum gas cylinder, and sending the carbon dioxide to a warehouse for storage after the carbon dioxide is qualified.
The preparation method of the breathable film comprises the following steps: stirring and mixing 50 parts by weight of aromatic polyamide solution, 30 parts by weight of melamine derivative, 1 part by weight of nano graphene and 3 parts by weight of nano silver to obtain film forming stock solution; and then coating the carrier plate by an applicator, drying the film-forming stock solution coated on the carrier plate at the hot air temperature of 120 ℃ to obtain a gel film, and stretching and forming by a stretcher to obtain the filtering film.
And the stirring paddle in the purification tank of the high-purity liquid carbon dioxide purification device is a magnetic stirring paddle.
The purifier is a carbon dioxide purification device, and the carbon dioxide purification device adopts an RZ-CO2-35 type carbon dioxide purification device of Razeg gas purification Hubei Limited company.
And the purification detection assay in the step 2) is a purification detection assay performed after the carbon dioxide treated by the purifier is kept stand for 8 hours.
The diaphragm compressor is pressurized at 0-15 mpa for 6 hours.
Step 2) is filled into a vacuum gas cylinder and stands for more than 8 hours before the step 3) is carried out.
And 3) testing the carbon dioxide filled in the vacuum gas cylinder in the step 3) by using a carbon dioxide analyzer.
And 3) testing the carbon dioxide filled in the vacuum gas cylinder in the step 3) until the standard of 99.999 percent is reached.
The aromatic polyamide solution comprises 50 mol% of 4,4Diaminodiphenyl ether, 25 mol% p-phenylenediamine, 25 mol% o-dianisidine, dehydrated N-methyl-2-pyrrolidone, 100 mol% isophthaloyl chloride and lithium carbonate; the preparation method of the aromatic polyamide solution comprises the following steps: 50 mol% of 4,4Diaminodiphenyl ether, 25 mol% of p-phenylenediamine, and 25 mol% of o-dianisidine were dissolved in dehydrated N-methyl-2-pyrrolidone, 100 mol% of isophthaloyl chloride was added thereto, and polymerization was carried out with stirring for 2 hours, followed by neutralization with lithium carbonate, to obtain an aromatic polyamide solution.
The melamine derivative comprises 58 parts by weight of formaldehyde, 40 parts by weight of melamine, 29 parts by weight of ethylenediamine and a proper amount of pH regulator, and the preparation method of the melamine derivative is provided; adding formaldehyde into melamine, adjusting pH to 9.5 with sodium hydroxide, stirring at 80 deg.C for 1h, adding ethylenediamine, adding acetic acid to adjust pH to 6.5, stirring at 90 deg.C for 1h, and removing impurities by short-path distillation to obtain melamine derivative.
Example 2:
1) conveying 99.5% of liquid carbon dioxide in the low-temperature liquid storage tank into a high-purity liquid carbon dioxide purification device for first purification, conveying the purified carbon dioxide into a vaporizer for gasification, and conveying the gasified carbon dioxide into a purifier for second purification; a breathable film is arranged in an air outlet pipe of the high-purity liquid carbon dioxide purification device, and the breathable film comprises 70 parts by weight of aromatic polyamide solution, 50 parts by weight of melamine derivative, 2 parts by weight of nano graphene and 5 parts by weight of nano silver;
2)2) purifying, detecting and testing the carbon dioxide treated by the purifier, sending the purified carbon dioxide into a diaphragm compressor after the carbon dioxide is qualified, pressurizing at 0-15 mpa, and filling into a vacuum gas cylinder;
3) and testing the carbon dioxide filled in the vacuum gas cylinder, and sending the carbon dioxide to a warehouse for storage after the carbon dioxide is qualified.
The preparation method of the breathable film comprises the following steps: stirring and mixing 70 parts by weight of aromatic polyamide solution, 50 parts by weight of melamine derivative, 2 parts by weight of nano graphene and 5 parts by weight of nano silver to obtain film forming stock solution; and then coating the carrier plate by an applicator, drying the film-forming stock solution coated on the carrier plate at the hot air temperature of 120 ℃ to obtain a gel film, and stretching and forming by a stretcher to obtain the filtering film.
And the stirring paddle in the purification tank of the high-purity liquid carbon dioxide purification device is a magnetic stirring paddle.
The purifier is a carbon dioxide purification device, and the carbon dioxide purification device adopts an RZ-CO2-35 type carbon dioxide purification device of Razeg gas purification Hubei Limited company.
And the purification detection assay in the step 2) is a purification detection assay performed after the carbon dioxide treated by the purifier is kept stand for 8 hours.
The diaphragm compressor is pressurized at 0-15 mpa for 6 hours.
Step 2) is filled into a vacuum gas cylinder and stands for more than 8 hours before the step 3) is carried out.
And 3) testing the carbon dioxide filled in the vacuum gas cylinder in the step 3) by using a carbon dioxide analyzer.
And 3) testing the carbon dioxide filled in the vacuum gas cylinder in the step 3) until the standard of 99.999 percent is reached.
The aromatic polyamide solution comprises 50 mol% of 4,4Diaminodiphenyl ether, 25 mol% p-phenylenediamine, 25 mol% o-dianisidine, dehydrated N-methyl-2-pyrrolidone, 100 mol% isophthaloyl chloride and lithium carbonate; the preparation method of the aromatic polyamide solution comprises the following steps: 50 mol% of 4,4Diaminodiphenyl ether, 25 mol% of p-phenylenediamine, and 25 mol% of o-dianisidine were dissolved in dehydrated N-methyl-2-pyrrolidone, 100 mol% of isophthaloyl chloride was added thereto, and polymerization was carried out with stirring for 2 hours, followed by neutralization with lithium carbonate, to obtain an aromatic polyamide solution.
The melamine derivative comprises 58 parts by weight of formaldehyde, 40 parts by weight of melamine, 29 parts by weight of ethylenediamine and a proper amount of pH regulator, and the preparation method of the melamine derivative is provided; adding formaldehyde into melamine, adjusting pH to 9.5 with sodium hydroxide, stirring at 80 deg.C for 1h, adding ethylenediamine, adding acetic acid to adjust pH to 6.5, stirring at 90 deg.C for 1h, and removing impurities by short-path distillation to obtain melamine derivative.
Example 3:
1) conveying 99.5% of liquid carbon dioxide in the low-temperature liquid storage tank into a high-purity liquid carbon dioxide purification device for first purification, conveying the purified carbon dioxide into a vaporizer for gasification, and conveying the gasified carbon dioxide into a purifier for second purification; a breathable film is arranged in an air outlet pipe of the high-purity liquid carbon dioxide purification device, and the breathable film comprises 60 parts by weight of aromatic polyamide solution, 40 parts by weight of melamine derivative, 1 part by weight of nano graphene and 4 parts by weight of nano silver;
2) purifying, detecting and testing the carbon dioxide treated by the purifier, sending the purified carbon dioxide into a diaphragm compressor after the carbon dioxide is qualified, pressurizing by 0-15 mpa, and filling into a vacuum gas cylinder;
3) and testing the carbon dioxide filled in the vacuum gas cylinder, and sending the carbon dioxide to a warehouse for storage after the carbon dioxide is qualified.
The preparation method of the breathable film comprises the following steps: stirring and mixing 60 parts by weight of aromatic polyamide solution, 40 parts by weight of melamine derivative, 1 part by weight of nano graphene and 4 parts by weight of nano silver to obtain film forming stock solution; and then coating the carrier plate by an applicator, drying the film-forming stock solution coated on the carrier plate at the hot air temperature of 120 ℃ to obtain a gel film, and stretching and forming by a stretcher to obtain the filtering film.
And the stirring paddle in the purification tank of the high-purity liquid carbon dioxide purification device is a magnetic stirring paddle.
The purifier is a carbon dioxide purification device, and the carbon dioxide purification device adopts an RZ-CO2-35 type carbon dioxide purification device of Razeg gas purification Hubei Limited company.
And the purification detection assay in the step 2) is a purification detection assay performed after the carbon dioxide treated by the purifier is kept stand for 8 hours.
The diaphragm compressor is pressurized at 0-15 mpa for 6 hours.
Step 2) is filled into a vacuum gas cylinder and stands for more than 8 hours before the step 3) is carried out.
And 3) testing the carbon dioxide filled in the vacuum gas cylinder in the step 3) by using a carbon dioxide analyzer.
And 3) testing the carbon dioxide filled in the vacuum gas cylinder in the step 3) until the standard of 99.999 percent is reached.
The aromatic polyamide solution comprises 50 mol% of 4,4Diaminodiphenyl ether, 25 mol% p-phenylenediamine, 25 mol% o-dianisidine, dehydrated N-methyl-2-pyrrolidone100 mol% of isophthaloyl dichloride and lithium carbonate; the preparation method of the aromatic polyamide solution comprises the following steps: 50 mol% of 4,4Diaminodiphenyl ether, 25 mol% of p-phenylenediamine, and 25 mol% of o-dianisidine were dissolved in dehydrated N-methyl-2-pyrrolidone, 100 mol% of isophthaloyl chloride was added thereto, and polymerization was carried out with stirring for 2 hours, followed by neutralization with lithium carbonate, to obtain an aromatic polyamide solution.
The melamine derivative comprises 58 parts by weight of formaldehyde, 40 parts by weight of melamine, 29 parts by weight of ethylenediamine and a proper amount of pH regulator, and the preparation method of the melamine derivative is provided; adding formaldehyde into melamine, adjusting pH to 9.5 with sodium hydroxide, stirring at 80 deg.C for 1h, adding ethylenediamine, adding acetic acid to adjust pH to 6.5, stirring at 90 deg.C for 1h, and removing impurities by short-path distillation to obtain melamine derivative.
The foregoing shows and describes the general principles, essential features, and advantages of the invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.

Claims (10)

1. A method for preparing carbon dioxide after purification of liquid carbon dioxide is characterized by comprising the following steps:
1) conveying 99.5% of liquid carbon dioxide in the low-temperature liquid storage tank into a high-purity liquid carbon dioxide purification device for first purification, conveying the purified carbon dioxide into a vaporizer for gasification, and conveying the gasified carbon dioxide into a purifier for second purification; a breathable film is arranged in an air outlet pipe of the high-purity liquid carbon dioxide purification device, and comprises 50-70 parts of aromatic polyamide solution, 30-50 parts of melamine derivative, 1-2 parts of nano graphene and 3-5 parts of nano silver;
2) purifying, detecting and testing the carbon dioxide treated by the purifier, sending the purified carbon dioxide into a diaphragm compressor after the carbon dioxide is qualified, pressurizing by 0-15 mpa, and filling into a vacuum gas cylinder;
3) and testing the carbon dioxide filled in the vacuum gas cylinder, and sending the carbon dioxide to a warehouse for storage after the carbon dioxide is qualified.
2. The method of claim 1 for producing carbon dioxide by purifying liquid carbon dioxide, wherein: and the stirring paddle in the purification tank of the high-purity liquid carbon dioxide purification device is a magnetic stirring paddle.
3. The method of claim 1 for producing carbon dioxide by purifying liquid carbon dioxide, wherein: the purifier is a carbon dioxide purification device.
4. The method of claim 1 for producing carbon dioxide by purifying liquid carbon dioxide, wherein: and the purification detection assay in the step 2) is a purification detection assay performed after the carbon dioxide treated by the purifier is kept stand for 8 hours.
5. The method of claim 1 for producing carbon dioxide by purifying liquid carbon dioxide, wherein: the diaphragm compressor is pressurized at 0-15 mpa for 6 hours.
6. The method of claim 1 for producing carbon dioxide by purifying liquid carbon dioxide, wherein: step 2) is filled into a vacuum gas cylinder and stands for more than 8 hours before the step 3) is carried out.
7. The method of claim 1 for producing carbon dioxide by purifying liquid carbon dioxide, wherein: and 3) testing the carbon dioxide filled in the vacuum gas cylinder in the step 3) by using a carbon dioxide analyzer.
8. The method of claim 1 for producing carbon dioxide by purifying liquid carbon dioxide, wherein: and 3) testing the carbon dioxide filled in the vacuum gas cylinder in the step 3) until the standard of 99.999 percent is reached.
9. The method of claim 1 for producing carbon dioxide by purifying liquid carbon dioxide, wherein: the aromatic polyamide solution comprises 50 mol% of 4, 4' -diaminodiphenyl ether, 25 mol% of p-phenylenediamine, 25 mol% of o-dianisidine, dehydrated N-methyl-2-pyrrolidone, 100 mol% of isophthaloyl dichloride and lithium carbonate.
10. The method of claim 1 for producing carbon dioxide by purifying liquid carbon dioxide, wherein: the melamine derivative comprises 58 parts of formaldehyde, 40 parts of melamine, 29 parts of ethylenediamine and a proper amount of pH regulator.
CN202110685720.6A 2021-06-21 2021-06-21 Method for preparing carbon dioxide after purification of liquid carbon dioxide Pending CN113307269A (en)

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Application publication date: 20210827