CN211998836U - Preparation device of high-purity carbon dioxide - Google Patents
Preparation device of high-purity carbon dioxide Download PDFInfo
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- CN211998836U CN211998836U CN201922482663.2U CN201922482663U CN211998836U CN 211998836 U CN211998836 U CN 211998836U CN 201922482663 U CN201922482663 U CN 201922482663U CN 211998836 U CN211998836 U CN 211998836U
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Abstract
The utility model relates to a high-purity carbon dioxide's preparation facilities belongs to fine chemistry industry technical field. The apparatus comprises CO2The system comprises a reaction kettle, a precooler cooler, a cryogenic cooler, a cold trap I, a rectifying tower, a cold trap II and a storage tank; CO 22The reaction kettle is provided with a carbonate/bicarbonate feeding port, an acid liquor feeding port and an air outlet; the pre-cooling cooler and the cryogenic cooler are used for condensing water, the pre-cooling cooler is used for pre-dewatering, and the cryogenic cooler is used for deeply dewatering; the cold trap I and the cold trap II are respectively provided with an air inlet, an emptying port and a liquid outlet; and the cold trap I and the cold trap II are used for liquefying carbon dioxide gas. Device simple structure, the operation energy consumption is low, fortuneThe method has stable and safe operation process, can effectively remove water and air impurities in the crude carbon dioxide gas prepared by the reaction of carbonate/bicarbonate and acid liquor, is easy to obtain high-purity (more than 99.995%) carbon dioxide, and has good industrial application value.
Description
Technical Field
The utility model relates to a high-purity carbon dioxide's preparation facilities belongs to fine chemistry industry technical field.
Background
Carbon dioxide is called carbonic acid gas, carbonic anhydride and dry ice, and is a colorless and tasteless suffocating non-combustible gas. The high-purity carbon dioxide can be used for oxidation, diffusion, chemical vapor deposition, standard gas and supercritical cleaning gas in semiconductor manufacturing; the method is also widely applied to the aspects of food, medicine, laser, spaceflight, welding and the like.
The industrial production method of high-purity carbon dioxide mainly adopts limestone calcining method and recovers natural gas, fermentation gas, petroleum refining by-product gas and synthetic ammonia industrial by-product gas. At present, solvent absorption and physical adsorption methods are mostly adopted for separating and recovering carbon dioxide from carbon dioxide gas mixture. The separation and recovery of carbon dioxide by the physical adsorption method belongs to a simple adsorption-desorption physical process, and has the advantages of simple process, low energy consumption, no toxicity, no pollution to the environment and an air source, no solution preparation and solvent loss required by the absorption method and the like. However, the requirement of high purity is still not met.
SUMMERY OF THE UTILITY MODEL
In view of this, the utility model provides a preparation facilities of high-purity carbon dioxide, the device simple structure, the operation energy consumption is low, production technology is steady safe, can detach moisture and air impurity in the carbon dioxide crude gas effectively, obtains high-purity carbon dioxide, has fine industrial application and worth.
The purpose of the utility model is realized through the following technical scheme.
A device for preparing high purity carbon dioxide, the device comprising CO2The system comprises a reaction kettle, a precooler cooler, a cryogenic cooler, a cold trap I, a rectifying tower, a cold trap II and a storage tank;
CO2the reaction kettle is provided with a carbonate/bicarbonate feeding port, an acid liquor feeding port and an air outlet;
the pre-cooling cooler and the cryogenic cooler are used for condensing water, the pre-cooling cooler is used for pre-dewatering, and the cryogenic cooler is used for deeply dewatering;
the cold trap I and the cold trap II are respectively provided with an air inlet, an evacuation port and a liquid outlet and are respectively used for liquefying carbon dioxide gas;
CO2the gas outlet of the reaction kettle is connected with the gas inlet of the precooling cooler, the gas outlet of the precooling cooler is connected with the gas inlet of the cryocooler, the gas outlet of the cryocooler is connected with the gas inlet of the cold trap I, the liquid outlet of the cold trap I is connected with the feed inlet at the lower part of the rectifying tower, the gas outlet at the upper part of the rectifying tower is connected with the gas inlet of the cold trap II, and the liquid outlet of the cold trap II is connected with the storage tank.
Furthermore, the rectifying tower is a filler rectifying tower, and the filler is a stainless steel pall ring, a rectangular saddle ring, a Raschig ring or a theta ring.
Has the advantages that:
device simple structure, the operation energy consumption is low, the steady safety of operation process can effectively detach moisture and air impurity in carbonate bicarbonate and acidizing fluid emergence reaction preparation carbon dioxide crude gas moreover, obtain the carbon dioxide of high purity (more than 99.995%), have fine industrial application and worth.
Drawings
Fig. 1 is a schematic structural diagram of the device of the present invention.
Wherein, 1-CO2The system comprises a reaction kettle, a 2-precooling cooler, a 3-cryogenic cooler, a 4-cold trap I, a 5-rectifying tower and a 6-cold trap II, a 7-storage tank.
Detailed Description
The invention is further described with reference to the accompanying drawings and detailed description, wherein the process is conventional, unless otherwise specified, and the starting materials are commercially available from a public perspective.
The apparatus involved in the preparation of high purity carbon dioxide in the following examples includes CO2A reaction kettle 1, a precooler 2, a cryogenic cooler 3, a cold trap I4, a rectifying tower 5, a cold trap II 6 and a storage tank 7, as shown in figure 1;
CO2a carbonate/bicarbonate feeding port, an acid liquid feeding port and an air outlet are arranged on the reaction kettle 1; adding CO2The carbonate/bicarbonate in the reaction kettle 1 can be lithium carbonate, sodium carbonate, potassium carbonate, lithium bicarbonate, sodium bicarbonate or potassium bicarbonate with the purity reaching the electronic grade, and the acid solution can be trifluoromethanesulfonic acid, bis-trifluoromethanesulfonimide acid, bis-fluorosulfonyl imide acid or sulfuric acid;
the lower parts of the cold trap I4 and the cold trap II 6 are respectively provided with an air inlet and a liquid outlet, and the upper parts of the cold trap I4 and the cold trap II are respectively provided with a drain hole; the cold trap I4 and the cold trap II 6 are mainly used for liquefying CO2The temperature of the gas is respectively set to-60 ℃ to-75 DEG C
The pre-cooling cooler 2 is used for pre-removing water, and the temperature is set to be 0 ℃ to-20 ℃; the cryogenic cooler 3 is used for deep water removal, and the temperature is set to be-30 ℃ to-50 ℃; the lower parts of the pre-cooling cooler 2 and the cryogenic cooler 3 are respectively provided with an air inlet, and the upper parts are respectively provided with an air outlet;
the rectifying tower 5 is used for rectifying and purifying carbon dioxide, a feed inlet is arranged at the lower part of the rectifying tower 5, and an air outlet is arranged at the upper part of the rectifying tower; the material of the packing inside the rectifying tower 5 is stainless steel pall ring, intalox saddle ring, Raschig ring or theta ring; the technological parameters of the rectification are as follows: the temperature of the top of the rectifying tower 5 is-20 ℃ to-10 ℃, the temperature of the bottom of the rectifying tower is-10 ℃ to-0 ℃, the temperature difference between the top of the rectifying tower and the bottom of the rectifying tower is not less than 5 ℃, the pressure in the rectifying tower is 1MPa to 5MPa, and the reflux ratio is 3 to 15;
CO2the gas outlet of reaction kettle 1 is connected with the gas inlet of precooling cooler 2, the gas outlet of precooling cooler 2 is connected with the gas inlet of cryocooler 3, the gas outlet of cryocooler 3 is connected with the gas inlet of cold trap I4, the liquid outlet of cold trap I4 is connected with the feed inlet of rectifying column 5, the gas outlet of rectifying column 5 is connected with the gas inlet of cold trap II 6, and the liquid outlet of cold trap II 6 is connected with storage tank 7.
Example 1
The method for preparing high-purity carbon dioxide based on the device comprises the following steps:
electronic grade lithium carbonate and trifluoromethanesulfonic acid in stoichiometric ratio in CO2CO produced by reaction in reaction kettle 12The crude gas is first pre-cooled and dewatered in a pre-cooling cooler 2 at a temperature of minus 10 +/-2 ℃, and CO is discharged from the pre-cooling cooler 22The water content in the crude gas is reduced to 129.3ppm, and then the crude gas enters a stage cooler 3 with the temperature of minus 48 +/-2 ℃ for further cooling and water removal, and CO coming out of the cryogenic cooler 32The water content in the crude gas is reduced to 8.4ppm, the crude gas enters a cold trap I4 with the temperature of minus 70 +/-2 ℃ and is condensed into liquid, air and other gas impurities which are not liquefied are discharged from a vent port of the cold trap I4, the liquid discharged from the cold trap I4 enters a rectifying tower 5 for rectification, and CO discharged from an air outlet of the rectifying tower 52The gas is condensed into CO by a cold trap II 6 with the temperature of minus 70 +/-2 DEG C2Liquid and stored in the tank 7;
wherein, the rectifying tower 5 used in the embodiment has a tower height of 18m, a tower diameter of 500mm, an internal filler of stainless steel theta ring and a filler height of 5 m; the temperature at the top of the tower is-13.9 ℃, the temperature at the bottom of the tower is-5.5 ℃, the pressure in the tower is 2.9MPa, and the reflux ratio is 13.
CO collected in the storage tank 7 by gas chromatography detection2The purity of the product reaches more than 99.999 percent, and the specific impurity content is detailed in table 1.
TABLE 1
| Item | H2 | O2 | N2 | CO | Total hydrocarbons | Moisture content |
| Standard of merit | ≤0.5ppm | ≤1ppm | ≤3ppm | ≤0.5ppm | ≤2ppm | ≤3ppm |
| Measurement results | 0.09ppm | 0.33ppm | 0.98ppm | 0.27ppm | 0.83ppm | 0.77ppm |
Example 2
The method for preparing high-purity carbon dioxide based on the device comprises the following steps:
electronic grade lithium carbonate and trifluoromethanesulfonic acid in stoichiometric ratio in CO2Reaction kettle1, CO produced2The crude gas is first pre-cooled and dewatered in a pre-cooling cooler 2 at (-2 +/-2) deg.c, and CO is discharged from the pre-cooling cooler 22The water content in the crude gas is reduced to 866.3ppm, and then the crude gas enters a stage cooler 3 with the temperature of (-40 +/-2) DEG C for further cooling and water removal, and CO coming out of the cryogenic cooler 32The water content in the crude gas is reduced to 38.4ppm, the crude gas enters a cold trap I4 with the temperature of minus 65 +/-2 ℃ and is condensed into liquid, air and other gas impurities which are not liquefied are discharged from a vent port of the cold trap I4, the liquid discharged from the cold trap I4 enters a rectifying tower 5 for rectification, and CO discharged from an air outlet of the rectifying tower 52The gas is condensed into CO by a cold trap II 6 with the temperature of minus 70 +/-2 DEG C2Liquid and stored in the tank 7;
wherein, the rectifying tower 5 used in the embodiment has a tower height of 18m, a tower diameter of 500mm, an internal filler of stainless steel theta ring and a filler height of 5 m; the temperature at the top of the tower is-13.9 ℃, the temperature at the bottom of the tower is-5.5 ℃, the pressure in the tower is 2.9MPa, and the reflux ratio is 13.
CO collected in the storage tank 7 by gas chromatography detection2The purity of the product is more than 99.998%, and the specific impurity content is shown in table 2.
TABLE 2
| Item | H2 | O2 | N2 | CO | Total hydrocarbons | Moisture content |
| Measurement results | 0.15ppm | 0.46ppm | 1.79ppm | 1.12ppm | 3.54ppm | 9.77ppm |
Example 3
The method for preparing high-purity carbon dioxide based on the device comprises the following steps:
electronic grade lithium carbonate and bis (trifluoromethanesulfonimide) acid in stoichiometric ratio in CO2CO produced by reaction in reaction kettle 12The crude gas is first pre-cooled and dewatered in a pre-cooling cooler 2 at a temperature of minus 10 +/-2 ℃, and CO is discharged from the pre-cooling cooler 22The water content in the crude gas is reduced to 133.7ppm, and then the crude gas enters a stage cooler 3 with the temperature of (-48 +/-2) DEG C for further cooling and water removal, and CO coming out of the cryogenic cooler 32The water content in the crude gas is reduced to 9.4ppm, the crude gas enters a cold trap I4 with the temperature of minus 70 +/-2 ℃ and is condensed into liquid, air and other gas impurities which are not liquefied are discharged from a vent port of the cold trap I4, the liquid discharged from the cold trap I4 enters a rectifying tower 5 for rectification, and CO discharged from an air outlet of the rectifying tower 52The gas is condensed into CO by a cold trap II 6 with the temperature of minus 70 +/-2 DEG C2Liquid and stored in the tank 7;
wherein, the rectifying tower 5 used in the embodiment has a tower height of 18m, a tower diameter of 500mm, an internal filler of stainless steel theta ring and a filler height of 5 m; the temperature at the top of the tower is-10 ℃, the temperature at the bottom of the tower is-4.5 ℃, the pressure in the tower is 3.4MPa, and the reflux ratio is 7.
CO collected in the storage tank 7 by gas chromatography detection2The purity of the product is more than 99.997%, and the specific impurity content is shown in table 3.
TABLE 3
| Item | H2 | O2 | N2 | CO | Total hydrocarbons | Moisture content |
| Measurement results | 0.35ppm | 2.33ppm | 7.54ppm | 4.25ppm | 5.35ppm | 3.83ppm |
In summary, the above is only a preferred embodiment of the present invention, and is not intended to limit the scope of the present invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (2)
1. A preparation facilities of high-purity carbon dioxide which characterized in that: the apparatus comprising CO2The system comprises a reaction kettle, a precooler cooler, a cryogenic cooler, a cold trap I, a rectifying tower, a cold trap II and a storage tank;
CO2the reaction kettle is provided with a carbonate/bicarbonate feeding port, an acid liquor feeding port and an air outlet;
the pre-cooling cooler and the cryogenic cooler are used for condensing water, the pre-cooling cooler is used for pre-dewatering, and the cryogenic cooler is used for deeply dewatering;
the cold trap I and the cold trap II are respectively provided with an air inlet, an emptying port and a liquid outlet; the cold trap I and the cold trap II are used for liquefying carbon dioxide gas;
CO2the gas outlet of the reaction kettle is connected with the gas inlet of the precooling cooler, the gas outlet of the precooling cooler is connected with the gas inlet of the cryocooler, the gas outlet of the cryocooler is connected with the gas inlet of the cold trap I, the liquid outlet of the cold trap I is connected with the feed inlet at the lower part of the rectifying tower, the gas outlet at the upper part of the rectifying tower is connected with the gas inlet of the cold trap II, and the liquid outlet of the cold trap II is connected with the storage tank.
2. The apparatus for producing high-purity carbon dioxide according to claim 1, characterized in that: the rectifying tower is a filler rectifying tower, and the filler is a stainless steel pall ring, a rectangular saddle ring, a Raschig ring or a theta ring.
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| CN110950339A (en) * | 2019-12-31 | 2020-04-03 | 中船重工（邯郸）派瑞特种气体有限公司 | Preparation method and preparation device of high-purity carbon dioxide |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110950339A (en) * | 2019-12-31 | 2020-04-03 | 中船重工（邯郸）派瑞特种气体有限公司 | Preparation method and preparation device of high-purity carbon dioxide |
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Address after: 057550 No. five Weir Road, chemical industry gathering area, Feixiang District, Handan, Hebei, 1 Patentee after: China shipbuilding (Handan) Perry Special Gas Co.,Ltd. Address before: No.1 Weiwu Road, chemical industry gathering area, Feixiang County, Handan City, Hebei Province Patentee before: PERIC SPECIAL GASES Co.,Ltd. |