CN215756465U - Purification device of ultrapure carbon dioxide - Google Patents

Purification device of ultrapure carbon dioxide Download PDF

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Publication number
CN215756465U
CN215756465U CN202121413852.5U CN202121413852U CN215756465U CN 215756465 U CN215756465 U CN 215756465U CN 202121413852 U CN202121413852 U CN 202121413852U CN 215756465 U CN215756465 U CN 215756465U
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raw material
carbon dioxide
vaporizer
adsorption mechanism
adsorption
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黄加斗
宗立冬
刘川
蔡炎南
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CHONGQING TONGHUI GAS CO LTD
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CHONGQING TONGHUI GAS CO LTD
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Abstract

The utility model discloses a purification device of ultrapure carbon dioxide, and relates to the technical field of gas purification. The low-temperature liquid filling device comprises a raw material tank, a vaporizer, an adsorption mechanism, a filter system, a rectifying tower, a low-temperature liquid filling pump and a finished product tank, wherein the vaporizer is connected to one side of the raw material tank and used for vaporizing raw material gas in the raw material tank through the vaporizer, the adsorption mechanism is connected to one side of the vaporizer and used for adsorbing partial impurities in the raw material gas, and the filter system is connected to one side of the adsorption mechanism. The utility model prepares the ultrapure carbon dioxide by adsorption and rectification, the raw materials sequentially enter a vaporizer, an adsorption mechanism, a filter system, a rectifying tower, a low-temperature liquid filling pump and a finished product tank through a raw material tank, and finally the ultrapure carbon dioxide is obtained and can be used for preparing various substances.

Description

Purification device of ultrapure carbon dioxide
Technical Field
The utility model belongs to the technical field of gas purification, and particularly relates to a purification device for ultrapure carbon dioxide.
Background
Carbon dioxide (carbon dioxide) is a carbon oxide, a common compound in air, is colorless, odorless, non-combustion-supporting, non-flammable at normal pressure, and slightly dissolves in water to form carbonic acid, which is a weak acid.
The ultra-pure carbon dioxide is used for semiconductor cleaning equipment, under the coordination of a small amount of organic solvent, carbon dioxide superfluid without surface tension is taken as a cleaning medium and rinsing liquid, the ultra-pure carbon dioxide superfluid goes deep into tiny pores to obtain good cleaning and drying effects, the carbon dioxide supercritical fluid semiconductor cleaning equipment is utilized, the large consumption of pure water and the pollution caused by chemical agents are avoided, and the problems of structural deformation, particle adsorption and the like caused by the surface tension in the traditional process can be solved.
At present, the world has no available ultrapure carbon dioxide product, and is only limited to a high-purity carbon dioxide product, so that the method and the device for purifying the ultrapure carbon dioxide are developed to obtain the ultrapure carbon dioxide, and the method and the device have positive display significance.
SUMMERY OF THE UTILITY MODEL
The utility model aims to provide a device for purifying ultrapure carbon dioxide, which solves the existing problems: currently, the world has no available ultrapure carbon dioxide product, and is only limited to high-purity carbon dioxide products.
In order to solve the technical problems, the utility model is realized by the following technical scheme: a purification device of ultrapure carbon dioxide comprises a raw material tank, a vaporizer, an adsorption mechanism, a filter system, a rectifying tower, a low-temperature liquid filling pump and a finished product tank;
one side of the raw material tank is connected with a vaporizer for vaporizing the raw material gas in the raw material tank;
one side of the vaporizer is connected with an adsorption mechanism for adsorbing partial impurities in the raw material gas;
one side of the adsorption mechanism is connected with a filter system for removing particles of the raw material gas and residual dust carried by the raw material gas through the adsorption mechanism;
one side of the filter system is connected with a rectifying tower for removing residual impurities in the raw material gas;
one side of the rectifying tower is connected with a low-temperature liquid filling pump, and one side of the low-temperature liquid filling pump is connected with a finished product tank.
Further, the feedstock tank is configured to:
the raw material tank is a horizontal tank;
the inlet of the raw material tank is connected with the raw material vehicle;
and the outlet of the raw material tank is connected with the vaporizer.
Further, the vaporizer is an air-temperature vaporizer.
Further, the adsorption mechanism is configured to:
the adsorption mechanism is formed by connecting two groups of adsorption towers in parallel;
the two adsorption towers are formed by connecting two adsorption columns in series;
and the inside of the adsorption mechanism is also connected with a nitrogen regeneration system.
Further, the filter system is configured to:
the filter system is composed of two groups of filter mechanisms in parallel connection:
the filter mechanism consists of two filter columns;
the precision of the filter column is 0.01 um.
Further, the rectifying column comprises a condenser and a reboiler;
the top of the rectifying tower is connected with a condenser, and the bottom of the rectifying tower is connected with a reboiler;
the condenser and reboiler are arranged to:
the cold source of the condenser is provided by a Freon refrigerating unit and is used for refrigerating the interior of the condenser;
the heat source of the reboiler is provided by an internal electric heater for heating the interior of the reboiler.
Further, a discharge hole of the reboiler is connected with an inlet of the low-temperature liquid filling pump.
The utility model has the following beneficial effects:
1. the utility model prepares the ultrapure carbon dioxide by adsorption and rectification, the raw materials sequentially enter a vaporizer, an adsorption mechanism, a filter system, a rectifying tower, a low-temperature liquid filling pump and a finished product tank through a raw material tank, and finally the ultrapure carbon dioxide is obtained and can be used for preparing various substances.
2. The utility model utilizes special adsorbent in the adsorption mechanism for adsorbing impurities such as water, ethanol, ammonia, sulfur dioxide and the like, and removes main impurities through the rectifying tower, wherein the rectifying tower is used for high-pressure low-temperature rectifying operation, lower part feeding is adopted, tower bottom discharging is adopted, steam in a tower top condenser is directly discharged at high altitude, and the production cost is effectively controlled.
3. The utility model can be designed in parallel through the adsorption mechanism and the filter system, thereby ensuring the continuity of the purification process.
4. The utility model has high gas purification efficiency through a series of designs, does not relate to chemical reagents, is easy to operate, has lower cost and is suitable for popularization and application.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings used in the description of the embodiments will be briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art that other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a schematic structural view of the present invention as a whole;
FIG. 2 is a schematic diagram of the filter system of the present invention.
In the drawings, the components represented by the respective reference numerals are listed below:
1. a raw material tank; 2. a vaporizer; 3. an adsorption mechanism; 31. an adsorption column; 4. a filter system; 41. a filtration column; 5. a rectifying tower; 51. a condenser; 52. a reboiler; 6. a cryogenic liquid charge pump; 7. and (5) a finished product can.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Referring to fig. 1-2, the present invention relates to a purification apparatus for ultrapure carbon dioxide, comprising a raw material tank 1, a vaporizer 2, an adsorption mechanism 3, a filter system 4, a rectifying tower 5, a cryogenic liquid charging pump 6, and a finished product tank 7;
one side of the raw material tank 1 is connected with a vaporizer 2 for vaporizing the raw material gas in the raw material tank 1;
one side of the vaporizer 2 is connected with an adsorption mechanism 3 for adsorbing partial impurities in the raw material gas;
one side of the adsorption mechanism 3 is connected with a filter system 4 for removing particles of the raw material gas and residual dust carried by the raw material gas through the adsorption mechanism 3;
one side of the filter system 4 is connected with a rectifying tower 5 for removing residual impurities in the raw material gas;
one side of the rectifying tower 5 is connected with a low-temperature liquid filling pump 6, and one side of the low-temperature liquid filling pump 6 is connected with a finished product tank 7;
the raw material tank 1 is configured to:
the inlet of the raw material tank 1 is connected with a raw material vehicle;
the outlet of the raw material tank 1 is connected to the vaporizer 2.
The raw material tank 1 and the finished product tank 7 are both horizontal tanks;
the vaporizer 2 is an air-temperature vaporizer.
The adsorption mechanism 3 is provided:
the adsorption mechanism 3 is formed by connecting two groups of adsorption towers in parallel;
the two adsorption towers are formed by connecting two adsorption columns 31 in series;
the interior of the adsorption mechanism 3 is also connected with a nitrogen regeneration system;
the adsorption mechanism 3 is an existing product, the core is an adsorption column 31, in the adsorption mechanism 3, the adsorption columns 31 are connected in parallel to form two groups, one group works, and the other group regenerates, so that the purification operation can be ensured to be uninterrupted; the adsorption column 31 adsorbs main impurities contained in the raw material, including: water, sulfur dioxide, ammonia gas, hydrocarbon compounds and the like, so as to ensure the purity of the ultrapure carbon dioxide product of the subsequent rectifying tower 5;
the filter system 4 is arranged to:
the filter system 4 consists of two sets of filter mechanisms in parallel:
the filter mechanism consists of two filter columns 41;
the accuracy of the filter column 41 is 0.01 um;
the filter system 4 is an existing product, the core is the filter columns 41, and in the filter system 4, the filter columns 41 are formed by connecting two groups in parallel, so that the purification operation can be ensured to be uninterrupted, the filter columns can also work simultaneously, and the filtering effect is improved; the precision of the filter column 41 is 0.01um, and particulate matters in the raw material gas are effectively removed.
The rectifying column 5 includes a condenser 51 and a reboiler 52;
the top of the rectifying tower 5 is connected with a condenser 51, and the bottom of the rectifying tower 5 is connected with a reboiler 52;
the condenser 51 and reboiler 52 are arranged:
the cold source of the condenser 51 is provided by a Freon refrigerating unit and is used for refrigerating the interior of the condenser 51;
the heat source of the reboiler 52 is provided by an internal electric heater for heating the interior of the reboiler 52.
The outlet of the reboiler 52 is connected to the inlet of the cryogenic liquid charge pump 6.
The rectifying tower 5 is used for high-pressure low-temperature rectifying operation, lower feeding is adopted, liquid discharging is carried out at the bottom, steam in a condenser 51 at the top of the rectifying tower 5 is directly discharged at high altitude, and heavy component impurities at the bottom of the rectifying tower 5 are discharged through a bottom liquid discharge valve.
The connection refers to air pipe connection and is used for gas transmission among all parts, and all parts are provided with gas inlets and outlets;
in the utility model, the adsorption mechanism 3 is used for adsorbing raw material gas and is used for adsorbing impurities such as water, ethanol, ammonia, sulfur dioxide and the like; the filter system 4 filters out solid particles in the adsorber to 0.01 um; the filtered gas enters a rectifying tower 5; the rectifying tower 5 is a high-pressure low-temperature rectifying process, the condenser 51 is provided by a Freon refrigerating unit, steam in the tower top of the rectifying tower 5 is directly discharged at high altitude, and residual heavy component impurities at the tower bottom are discharged through a liquid discharge valve.
The work flow of the purification device of the ultrapure carbon dioxide comprises the following steps:
s1, the raw material of the raw material tank 1 comes from a raw material vehicle;
s2, vaporizing the mixture into gas by the vaporizer 2 and then entering the adsorption mechanism 3;
s3, the adsorption mechanism 3 is composed of two groups of adsorption towers which are connected in parallel, each group of adsorption towers is composed of two adsorption columns 31 which are connected in series, an adsorbent treated by a special process is used as an adsorbent in the adsorption columns 31, and the adsorption mechanism 3 is accompanied with an online regeneration system, so that online regeneration treatment can be realized, and the continuity of the process is ensured;
s4, enabling the product out of the adsorption mechanism 3 to enter a filter system 4, wherein the filter system 4 is the existing product, the core is a filter column 41, and in the filter system 4, two groups of filter columns 41 are preferably connected in parallel to form the filter system, so that the purification operation can be ensured to be uninterrupted, and the filter system can also work simultaneously, and the filtering effect is improved;
s5, feeding the filtered gas into a rectifying tower 5, wherein a feed inlet of the rectifying tower 5 is the lower part of the rectifying tower 5; wherein, the rectifying tower 5 adopts stainless steel wire net structured packing as the packing;
s6, connecting the top end of the rectifying tower 5 with a condenser 51, cooling the low-boiling-point component into liquid, refluxing the liquid to the rectifying tower 5, discharging the light component impurities at the top of the tower at high altitude, and providing a cold source of the condenser 51 by a Freon refrigerating unit;
s7, connecting the lower part of the rectifying tower 5 with a reboiler 52, heating the high-boiling-point components by an electric heater, evaporating and rising, collecting the low-boiling-point heavy component impurities at the bottom of the tower, and discharging the low-boiling-point heavy component impurities by a liquid discharging method, wherein a heat source of the reboiler 52 is provided for the built-in electric heater;
s8, the purity of the product is ensured by online analysis of gas components, specifically, the product is connected to an analytical instrument through an analysis pipeline on the reboiler 52, and the moisture components in the reboiler 52 are analyzed; the tower top analysis pipeline is connected to the chromatographic analysis heavy component index; analyzing the metal ion indexes by ICP-MS through product sampling;
and S9, the bottom of the reboiler 52 is a product discharge port, the product is in a liquid state, and enters a finished product tank 7 through a low-temperature liquid filling pump 6.
This practical raw materials gas volume component that can handle is: CO2 is more than or equal to 99.9 percent, NO2 is less than 0.1ppm, NO is less than 0.1ppm, CO is less than or equal to 0.01ppm, SO2 is less than or equal to 0.05ppm, NH3 is less than 1ppm, CH3OH is less than 0.1ppm, acetaldehyde is less than 0.1ppm, chloroethylene is less than 0.1ppm, grease is less than 1mg/kg, total hydrocarbon is less than 10ppm, total sulfur (except SO 2) is less than 0.025ppm, and H2O is less than 5 ppm.
The product gas volume component of the utility model is: CO2 is more than or equal to 99.99999 percent, H2 is less than 0.01ppm, O2 is less than 0.01ppm, Ar is less than 0.01ppm, N2 is less than 0.01ppm, NO2 is less than 0.01ppm, CO is less than 0.01ppm, SO2 is less than 0.01ppm, NH3 is less than 0.01ppm, CH4 is less than 0, 01ppm, total hydrocarbon is less than 0.01ppm, total sulfur (except SO 2) is less than 0.01ppm, H2O is less than 0.01ppm, and particles are less than 25000 particles/m 3.
The heating temperature of the reboiler 52 is 120 ℃; the cooling temperature of the condenser 51 was-25 ℃.
The working pressure of the rectifying tower 5 is 2.0 Mpa.
The precision of the inner surfaces of the adsorption column 31, the rectifying tower 5, the finished product and other pressure containers is less than or equal to 0.3 um.
The finished product group analysis scheme is that a cavity ring-down moisture analyzer is used for water, a trace sulfur analyzer is used for sulfide, a granularity instrument is used for granularity, DID helium ion chromatography is used for analyzing H2, O2, Ar, N2, CH4, CO, NH3 and the like, and ICP-MC is used for analyzing metal ions (if required).
In the drawing, arrows indicate the direction of travel of the purification gas, i.e., the purification from the feed gas to ultrapure carbon dioxide.
In the description herein, references to the description of "one embodiment," "an example," "a specific example" or the like are intended to mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the utility model. In this specification, the schematic representations of the terms used above do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The preferred embodiments of the utility model disclosed above are intended to be illustrative only. The preferred embodiments are not intended to be exhaustive or to limit the utility model to the precise embodiments disclosed. Obviously, many modifications and variations are possible in light of the above teaching. The embodiments were chosen and described in order to best explain the principles of the utility model and the practical application, to thereby enable others skilled in the art to best utilize the utility model. The utility model is limited only by the claims and their full scope and equivalents.

Claims (7)

1. A purification device of ultrapure carbon dioxide is characterized in that: comprises a raw material tank (1), a vaporizer (2), an adsorption mechanism (3), a filter system (4), a rectifying tower (5), a low-temperature liquid filling pump (6) and a finished product tank (7);
one side of the raw material tank (1) is connected with a vaporizer (2) for vaporizing the raw material gas in the raw material tank (1);
one side of the vaporizer (2) is connected with an adsorption mechanism (3) for adsorbing partial impurities in the raw material gas;
one side of the adsorption mechanism (3) is connected with a filter system (4) for removing particles of the raw material gas and residual dust carried by the raw material gas through the adsorption mechanism (3);
one side of the filter system (4) is connected with a rectifying tower (5) for removing residual impurities of the raw material gas;
one side of rectifying column (5) is connected with low temperature liquid filling pump (6), one side of low temperature liquid filling pump (6) is connected with finished product jar (7).
2. The apparatus for purifying ultrapure carbon dioxide as claimed in claim 1, wherein: the raw material tank (1) is configured to:
the raw material tank (1) is a horizontal tank;
the inlet of the raw material tank (1) is connected with a raw material vehicle;
the outlet of the raw material tank (1) is connected with the vaporizer (2).
3. The apparatus for purifying ultrapure carbon dioxide as claimed in claim 1, wherein: the vaporizer (2) is an air-temperature vaporizer.
4. The apparatus for purifying ultrapure carbon dioxide as claimed in claim 1, wherein: the adsorption mechanism (3) is configured to:
the adsorption mechanism (3) is formed by connecting two groups of adsorption towers in parallel;
the two adsorption towers are formed by connecting two adsorption columns (31) in series;
and a nitrogen regeneration system is also connected inside the adsorption mechanism (3).
5. The apparatus for purifying ultrapure carbon dioxide as claimed in claim 1, wherein: the filter system (4) is arranged to:
the filter system (4) is formed by connecting two groups of filter mechanisms in parallel:
the filter mechanism consists of two filter columns (41);
the precision of the filter column (41) is 0.01 um.
6. The apparatus for purifying ultrapure carbon dioxide as claimed in claim 1, wherein: the rectifying column (5) comprises a condenser (51) and a reboiler (52);
the top of the rectifying tower (5) is connected with a condenser (51), and the bottom of the rectifying tower (5) is connected with a reboiler (52);
the condenser (51) and reboiler (52) are arranged to:
the cold source of the condenser (51) is provided by a Freon refrigerating unit and is used for refrigerating the interior of the condenser (51);
the heat source of the reboiler (52) is provided by an internal electric heater for heating the interior of the reboiler (52).
7. The apparatus for purifying ultrapure carbon dioxide as claimed in claim 6, wherein: the discharge hole of the reboiler (52) is connected with the inlet of the low-temperature liquid filling pump (6).
CN202121413852.5U 2021-06-24 2021-06-24 Purification device of ultrapure carbon dioxide Active CN215756465U (en)

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Application Number Priority Date Filing Date Title
CN202121413852.5U CN215756465U (en) 2021-06-24 2021-06-24 Purification device of ultrapure carbon dioxide

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202121413852.5U CN215756465U (en) 2021-06-24 2021-06-24 Purification device of ultrapure carbon dioxide

Publications (1)

Publication Number Publication Date
CN215756465U true CN215756465U (en) 2022-02-08

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Application Number Title Priority Date Filing Date
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