CN111533129A - Carbon dioxide purification device - Google Patents
Carbon dioxide purification device Download PDFInfo
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- CN111533129A CN111533129A CN202010251583.0A CN202010251583A CN111533129A CN 111533129 A CN111533129 A CN 111533129A CN 202010251583 A CN202010251583 A CN 202010251583A CN 111533129 A CN111533129 A CN 111533129A
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Abstract
The invention relates to a carbon dioxide purification device, which comprises a first adsorption tower (1), a catalytic tower (2) and a second adsorption tower (16), wherein silica gel is filled in the first adsorption tower (1), activated carbon is filled in the second adsorption tower (3), magnesium perchlorate is carried on the activated carbon, the first adsorption tower (1) is provided with an air inlet pipe (13) and an inert gas pipe (5), the inert gas pipe (5) is communicated with the air inlet end of the first adsorption tower (1) through a stainless steel electromagnetic valve (14) and a flow stabilizing valve (11) in sequence, the air outlet end of the first adsorption tower (1) is connected with the catalytic tower (2), the air outlet pipeline of the catalytic tower (2) is connected with the second adsorption tower (16) through a corrugated pipe (7) and a metal filter (9) in sequence, and the second adsorption tower (16) is provided with a pure gas pipeline (6). The scheme purifies the original impurities in the carbon dioxide by combining catalytic conversion and adsorption of the catalyst, and ensures that CO is purified2The content of impurities in the gas is less than 1PPm, thereby obtaining high-purity CO2。
Description
Technical Field
The invention relates to the field of carbon dioxide purification, in particular to a carbon dioxide purification device.
Background
Carbon dioxide (English name: Carbon dioxide) is a common compound in air and has the molecular formula of CO2From two oxygensThe atom is linked to a carbon atom by a covalent bond. The air contains a trace amount of carbon dioxide, which accounts for about 0.03% of the total volume of the air. Carbon dioxide is soluble in water to form carbonic acid, a weak acid. Since the air contains carbon dioxide, the rainwater has a pH of 5.6 or higher and CO is generally contained2It is nontoxic, but when CO is in the air2When the content exceeds the normal content, the harmful effect on the human body is produced. High purity carbon dioxide is used in artificial diamond, carbon dioxide laser, optical fiber production, etching in the electronics industry, gas for analytical equipment, nonpolar and nonionic low molecular weight detergents in supercritical state. Carbon dioxide has CO and H in the manufacturing process2The carbon dioxide producer can also purify the medium in the production flow by harmful impurities such as O, hydrocarbons, O2 and the like, but the production of ultra-pure carbon dioxide with the impurity content of less than 1PPm is very difficult due to the restriction of large-scale chemical production, process and process flow.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a carbon dioxide purification device which purifies the original impurities in carbon dioxide by combining the catalytic conversion and adsorption of a catalyst to ensure that CO is purified2The content of impurities in the gas is less than 1PPm, thereby obtaining high-purity CO2。
The purpose of the invention is realized by the following technical scheme:
a carbon dioxide purification device comprises a first adsorption tower, a catalytic tower and a second adsorption tower;
silica gel is filled in the first adsorption tower, activated carbon is filled in the second adsorption tower, and magnesium perchlorate is carried on the activated carbon;
the first adsorption tower is provided with an air inlet pipe and an inert gas pipe;
the inert gas pipe is communicated with the gas inlet end of the first adsorption tower through a stainless steel electromagnetic valve and a flow stabilizing valve in sequence, and the gas outlet end of the first adsorption tower is connected with the catalytic tower;
the gas outlet pipeline of the catalytic tower is connected with the second adsorption tower sequentially through a corrugated pipe and a metal filter, and the second adsorption tower is provided with a pure gas pipeline.
The advantage of this solution is that CO is introduced2The purification operation is realized through three parts of treatment in sequence.
The first part is pretreatment, and silica gel is adopted in the first adsorption tower to remove CO2H in (1)2Removal of O, CO2Is stable in chemical property but is stable with H2O generates carbonic acid and is highly corrosive to metal materials and adsorbents. We prefer to use silica gel as the pre-treatment adsorbent filler, which is more stable than 3A molecular sieves under carbonic acid conditions. The regeneration temperature of silica gel only needs 150 ℃, the 3A molecular sieve needs high temperature of more than 300 ℃, the corrosivity of carbonic acid to materials can be further enhanced under the high temperature condition, and an anti-corrosion electromagnetic valve and a polytetrafluoroethylene pipeline are preferably adopted for transmission and control.
The second part is a catalytic part, dried CO2The catalyst in the catalytic tower is used for catalytic conversion, and the catalyst with active carbon as a carrier can be used for CO2Middle O2The catalytic conversion of (3) can convert methane, carbon monoxide, hydrocarbons, oxygen, and the like in carbon dioxide into carbon dioxide and water by using an activated carbon catalyst carrying a nano-level material such as nickel, palladium, platinum, and the like.
The third part is deep purification, and the carbon dioxide from the second part only contains trace impurity H2And O. In the second adsorption tower we preferably use the adsorbent loaded with anhydrous magnesium perchlorate, also can use 3A molecular sieve to carry out deep dehydration. The high-purity carbon dioxide is obtained by adopting a chemical adsorption method and a physical adsorption method.
As a preferable scheme, the first adsorption tower and the second adsorption tower are respectively provided with a first standby tower and a second standby tower;
and switch valves are respectively arranged between the first adsorption tower and the first standby tower and between the second adsorption tower and the second standby tower and used for controlling the use states of the first adsorption tower, the second adsorption tower, the first standby tower and the second standby tower.
As a preferable scheme, the gas inlet pipe and the inert gas pipe are respectively communicated with the first standby tower, and pressure gauges are respectively arranged between the inert gas pipe and the first adsorption tower and between the inert gas pipe and the first standby tower.
As a preferable scheme, a flow velocity meter is further installed between the first adsorption tower/first standby tower and the catalytic tower, the flow velocity meter can ensure the flow velocity and pressure of the regeneration gas and the smooth completion of the regeneration, and the flow stabilizing valve is provided with an air inlet and an air outlet and can adjust the size of the outlet air flow.
Preferably, all the pipelines of the purification device are provided with control valves.
As a preferable scheme, the air inlet pipe is used for introducing carbon dioxide raw gas into the first adsorption tower or the first standby tower;
and introducing inert gas into the inert gas pipe at the speed of 5L/min to purge the silica gel in the first adsorption tower or the first standby tower.
And the silica gel in the first adsorption tower is used for adsorbing water in the carbon dioxide raw gas, and then inert gas is introduced at the speed of 5L/min to purge the silica gel. Due to CO2Colorless, odorless, and dangerous for suffocation when released into the environment, and CO dispersed in the air2It is also very corrosive to electric appliances and equipment, so that during regeneration, the nitrogen or argon of atmospheric components is used for purging, and only a small amount of CO is used in the later period2The replacement is carried out, and the purposes of safety and environmental protection are achieved.
As a preferable scheme, heating belts are arranged on the outer walls of the first adsorption tower and the first standby tower, silica gel is regenerated after water is adsorbed by the silica gel, and the first adsorption tower and the first standby tower are heated to 150 ℃ through the heating belts during regeneration.
Preferably, the catalyst in the catalytic tower is a nickel-palladium catalyst or a CTO-1 catalyst.
Preferably, polytetrafluoroethylene valves are respectively arranged at the gas inlet end and the gas outlet end of the first adsorption tower and the first standby tower.
The invention has the beneficial effects that:
(1) silica gel is preferably adopted as a pretreatment adsorbent filler, so that CO is increased2Middle H2And (4) adsorbing O.
(2) An inert gas purging design is adopted, and H is adsorbed by introducing nitrogen or argon of 5l/min2Purging with silica gel of O. Due to CO2Colorless, odorless, and dangerous for suffocation when released into the environment, and CO dispersed in the air2And the regeneration agent also has strong corrosivity on electric appliances and equipment, so that nitrogen or argon of atmospheric components is adopted for purging during regeneration, and only a small amount of CO2 is used for replacement in the later period, so that the purposes of safety and environmental protection are achieved.
(3) Introducing a proper amount of nitrogen into the system at the initial stage of silica gel regeneration, taking away a large amount of water, pumping out residual nitrogen and trace water in the adsorption tower, and supplementing CO in the pumping-out process2And can be used for replacing nitrogen in the adsorption tower.
Drawings
FIG. 1 is a schematic view of the overall structure of the present invention;
FIG. 2 is a front view of the present invention;
FIG. 3 is a side view of the present invention;
FIG. 4 is a top view of the present invention;
FIG. 5 is a schematic diagram of the present invention;
FIG. 6 is a raw gas chromatograph scan curve;
FIG. 7 is a scanning curve of a pure gas chromatograph
FIG. 8 is a plot of PPm change data for 150 ℃ impurities;
FIG. 9 is a plot of PPm change data for 200 ℃ impurities;
FIG. 10 is a plot of the PPm change data for the 250 ℃ impurity.
Detailed Description
The technical solution of the present invention is further described in detail with reference to the following specific examples, but the scope of the present invention is not limited to the following.
As shown in fig. 1 to 4, a carbon dioxide purification apparatus includes a first adsorption tower 1, a catalytic tower 2, and a second adsorption tower 16;
silica gel is filled in the first adsorption tower 1, activated carbon is filled in the second adsorption tower 3, and magnesium perchlorate is carried on the activated carbon;
the first adsorption tower 1 is provided with an air inlet pipe 13 and an inert gas pipe 5;
the inert gas pipe 5 is communicated with the gas inlet end of the first adsorption tower 1 through a stainless steel electromagnetic valve 14 and a flow stabilizing valve 11 in sequence, and the gas outlet end of the first adsorption tower 1 is connected with the catalytic tower 2;
the gas outlet pipeline of the catalytic tower 2 is connected with a second adsorption tower 16 sequentially through a corrugated pipe 7 and a metal filter 9, and the second adsorption tower 16 is provided with a pure gas pipeline 6.
As a preferable mode, the first adsorption tower 1 and the second adsorption tower 16 are provided with a first backup tower 3 and a second backup tower 12, respectively; switching valves 15 are provided between the first adsorption tower 1 and the first backup tower 3, and between the second adsorption tower 16 and the second backup tower 12, respectively, and the switching valves 15 are used to control the use states of the first adsorption tower 1, the second adsorption tower 16, the first backup tower 3, and the second backup tower 12.
The working principle is shown in fig. 5, the raw gas firstly enters a first adsorption tower 1 (an adsorption tower I and an adsorption tower II in fig. 5, one of the adsorption towers is used as a first adsorption tower 1, and the other is used as a first standby tower 3), the inert gas enters the first adsorption tower 1 from a right side valve, the first pretreatment is completed in the first adsorption tower 1, and silica gel is adopted in the first adsorption tower to carry out CO (carbon monoxide) treatment on CO2H in (1)2Removal of O, CO2Is stable in chemical property but is stable with H2O generates carbonic acid and is highly corrosive to metal materials and adsorbents. We prefer to use silica gel as the pre-treatment adsorbent filler, which is more stable than 3A molecular sieves under carbonic acid conditions. The regeneration temperature of silica gel only needs 150 ℃, the 3A molecular sieve needs high temperature of more than 300 ℃, the corrosivity of carbonic acid to materials can be further enhanced under the high temperature condition, and an anti-corrosion electromagnetic valve and a polytetrafluoroethylene pipeline are preferably adopted for transmission and control.
After the first part of treatment, the mixture enters a catalytic tower to be subjected to the second part of catalytic conversion treatment, and dried CO2By catalysis ofThe catalyst in the chemical tower 2 can be used for catalytic conversion, and the catalyst using active carbon as a carrier can be used for CO2Middle O2The catalytic conversion of (3) can convert methane, carbon monoxide, hydrocarbons, oxygen, and the like in carbon dioxide into carbon dioxide and water by using an activated carbon catalyst carrying a nano-level material such as nickel, palladium, platinum, and the like.
Finally, the carbon dioxide enters a second adsorption tower 16 (in the figure, an adsorption tower III and an adsorption tower IV are respectively a main tower and a standby tower) to carry out deep purification of a third part, and the carbon dioxide coming out of the second part only contains trace impurity H2And O. In the second adsorption tower 16, the adsorbent loaded with anhydrous magnesium perchlorate is preferably adopted, and deep dehydration can be carried out by using a 3A molecular sieve. The high-purity carbon dioxide is obtained by adopting a chemical adsorption method and a physical adsorption method.
As a preferable scheme, the gas inlet pipe 13 and the inert gas pipe 5 are respectively communicated with the first standby tower 3, a pressure gauge 8 is respectively arranged between the inert gas pipe 5 and the first adsorption tower 1 and the first standby tower 3, a flow rate meter 10 is further arranged between the first adsorption tower 1/the first standby tower 3 and the catalytic tower 2, and a control valve 15 is arranged in all pipelines of the purification device.
As a preferable scheme, the gas inlet pipe 13 is used for introducing carbon dioxide raw gas into the first adsorption tower 1 or the first standby tower 3; the inert gas pipe 5 is fed with an inert gas at a rate of 5L/min to purge the silica gel in the first adsorption column 1 or the first backup column 3.
As a preferable scheme, heating belts are arranged on the outer walls of the first adsorption tower 1 and the first standby tower 3, silica gel is regenerated after adsorbing water, and the first adsorption tower 1 and the first standby tower 3 are heated to 150 ℃ through the heating belts during regeneration.
As a preferable scheme, the catalyst in the catalytic tower 2 is a nickel-palladium catalyst or a CTO-1 catalyst.
As a preferable scheme, polytetrafluoroethylene valves 4 are respectively arranged at the air inlet end and the air outlet end of the first adsorption tower 1 and the first standby tower 3, wherein the polytetrafluoroethylene valve 4 at the upper side is used for controlling air inlet, and the polytetrafluoroethylene valve 4 at the lower side is a waste gas blow-down valve.
The catalytic tower 2 is a 304 stainless steel pipe body with phi 57 multiplied by 3mm and the length of 760mm, a quantitative nickel-palladium catalyst is filled in the catalytic tower, the catalytic conversion efficiency is ensured by a reasonable bed layer structure, and the catalytic tower with an air inlet and an air outlet is finally manufactured by welding argon protection gas.
The first adsorption tower 1, the second adsorption tower 16, the first standby tower 3 and the second standby tower 12 are 304 stainless steel tubes with the diameter of 76 x 4mm and the length of 760mm, a certain amount of silica gel and activated carbon (loaded with magnesium perchlorate) adsorbent is filled in the tubes, and the tubes are welded through argon protection gas to finally manufacture 2 sets of belt inlet and outlet ports.
The bellows 7 is designed as a stainless steel bellows valve.
The valves are all polytetrafluoroethylene valves, are specially equipped for corrosive gas, can effectively reduce the corrosion of carbon dioxide to the valves, and are installed at the front end of the adsorption tower, so that the gas at the section is raw gas.
The metal filter 9 is internally provided with a filter element with the filtering precision of 0.3 mu m and formed by sintering stainless steel, and can effectively filter particles with the filtering precision of more than or equal to 0.3 mu m in the gas, thereby ensuring the purity of the gas and being provided with an air inlet and an air outlet.
The components are connected with a pipeline with the diameter of 6mm, wherein the pipeline is 316L, and the gas purity is ensured through electrochemical internal and external polishing treatment.
This device is when purification carbon dioxide gas, makes gas get into first adsorption tower 1 earlier, utilizes the silica gel bed to adsorb water and carries out the preliminary treatment, rethread catalytic tower 2 afterwards, utilizes the nickel palladium catalyst that loads in catalytic tower 2 to carry out catalytic conversion, makes impurity such as hydrocarbons turn into water and carbon dioxide, has carried the active carbon of magnesium perchlorate in second adsorption tower 16 at last, adsorbs the water of trace in the gas, and the device wholly adopts automated control (PLC), easy operation.
And (3) experimental detection:
as shown in fig. 6, the scanning curve is an analysis of the raw gas:
printing time: 18 days 6 and 18 months in 2019, 13 minutes and 5 seconds at 18 hours
Sample introduction time: 19 days 2 month and 9 hours 20 minutes 41 seconds
Sample name: steel cylinder number of mixed gas (main gas distribution carbon dioxide gas +500ppm oxygen +1000ppm methane):
an analysis device: TCD-01 gas chromatograph bridge flow: 100MA device number:
carrier gas: high-purity hydrogen 99.9999% 20ml/min detection gas: 2 ml of
───────────────────────
Sequence number retention time name Peak area% Peak area
───────────────────────
1 0.007 1.077 3521
22.110 oxygen 23.4576653
37.195 methane 75.47246688
───────────────────────
Total 100326862
The peak area detected by the gas chromatograph and the corresponding PPm value need to be converted by the following formula.
As the raw gas analysis report data, if the PPm of oxygen is V, the PPm of the oxygen distribution gas is Y, and the peak area is S, then the V value of PPm of oxygen is equal to: v = Y/S.
From the above data, the oxygen content V =76653/500=153.3PPm, and similarly the methane content is 246.7 PPm.
The gas analysis after treatment is shown in fig. 7:
printing time: 18 days 6 and 18 months in 2019, and 53 minutes and 48 seconds at 18 hours
Sample introduction time: 19/2/2019, 38/23/12/min
Sample name: steel cylinder number of mixed gas (main gas distribution carbon dioxide gas +500ppm oxygen +1000ppm methane):
an analysis device: TCD-01 gas chromatograph bridge flow: 100mA device number:
carrier gas: high-purity hydrogen 99.9999% 20ml/min detection gas: 2 ml of
Working conditions of the apparatus
The diameter of the catalytic tower is 57mm, the height is 760mm, and the diameter-height ratio is 0.075: 1; the data detected by a TCD-01 gas chromatograph at a space velocity of 1.2h-1 and a temperature of 250 ℃ are shown in FIG. 7.
───────────────────────
Sequence number retention time name Peak area% Peak area
───────────────────────
1 0.010 98.9 13746
22.358 oxygen 1.096152
───────────────────────
Total 10013898
Wherein, PPm change data of impurities at 150 deg.C, 200 deg.C, 250 deg.C were measured, and the content curves thereof are shown with reference to FIGS. 8-10.
The foregoing is illustrative of the preferred embodiments of this invention, and it is to be understood that the invention is not limited to the precise form disclosed herein and that various other combinations, modifications, and environments may be resorted to, falling within the scope of the concept as disclosed herein, either as described above or as apparent to those skilled in the relevant art. And that modifications and variations may be effected by those skilled in the art without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (9)
1. A carbon dioxide purification device is characterized by comprising a first adsorption tower (1), a catalytic tower (2) and a second adsorption tower (16);
silica gel is filled in the first adsorption tower (1), activated carbon is filled in the second adsorption tower (3), and magnesium perchlorate is carried on the activated carbon;
the first adsorption tower (1) is provided with an air inlet pipe (13) and an inert gas pipe (5);
the inert gas pipe (5) is communicated with the gas inlet end of the first adsorption tower (1) sequentially through a stainless steel electromagnetic valve (14) and a flow stabilizing valve (11), and the gas outlet end of the first adsorption tower (1) is connected with the catalytic tower (2);
the gas outlet pipeline of the catalytic tower (2) is connected with the second adsorption tower (16) sequentially through a corrugated pipe (7) and a metal filter (9), and the second adsorption tower (16) is provided with a pure gas pipeline (6).
2. A carbon dioxide purification apparatus according to claim 1, wherein the first adsorption tower (1) and the second adsorption tower (16) are provided with a first backup tower (3) and a second backup tower (12), respectively;
switch valves (15) are respectively arranged between the first adsorption tower (1) and the first standby tower (3) and between the second adsorption tower (16) and the second standby tower (12), and the switch valves (15) are used for controlling the use states of the first adsorption tower (1), the second adsorption tower (16), the first standby tower (3) and the second standby tower (12).
3. Carbon dioxide purification device according to claim 2, wherein the gas inlet pipe (13) and the inert gas pipe (5) are further in communication with the first backup tower (3), respectively, and a pressure gauge (8) is arranged between the inert gas pipe (5) and the first adsorption tower (1) and the first backup tower (3), respectively.
4. A carbon dioxide purification apparatus according to claim 3, wherein a flow rate meter (10) is further installed between the first adsorption tower (1)/first backup tower (3) and the catalytic tower (2).
5. A carbon dioxide purification device according to claim 1, characterized in that all the pipes of the purification device are fitted with control valves (15).
6. Carbon dioxide purification device according to any one of claims 1-5, wherein the inlet pipe (13) is used for introducing carbon dioxide raw gas into the first adsorption tower (1) or the first standby tower (3).
7. The carbon dioxide purification device according to claim 6, wherein heating belts are arranged on the outer walls of the first adsorption tower (1) and the first backup tower (3), the silica gel is regenerated after adsorbing water, the first adsorption tower (1) and the first backup tower (3) are heated to 150 ℃ through the heating belts during regeneration, and the inert gas is introduced into the inert gas pipe (5) at a speed of 5L/min to purge the silica gel in the first adsorption tower (1) or the first backup tower (3).
8. A carbon dioxide purification apparatus according to claim 7, wherein the catalyst in the catalytic tower (2) is a nickel palladium catalyst or a CTO-1 catalyst.
9. The carbon dioxide purification device according to claim 8, wherein the air inlet end and the air outlet end of the first adsorption tower (1) and the first standby tower (3) are respectively provided with a polytetrafluoroethylene valve (4).
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| Application Number | Priority Date | Filing Date | Title |
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| CN202010251583.0A CN111533129A (en) | 2020-04-01 | 2020-04-01 | Carbon dioxide purification device |
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| CN202010251583.0A CN111533129A (en) | 2020-04-01 | 2020-04-01 | Carbon dioxide purification device |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN201545703U (en) * | 2009-09-28 | 2010-08-11 | 苏州市金宏气体有限公司 | Device for purifying carbon dioxide in recovered dry ice waste gas |
| CN104862607A (en) * | 2015-05-25 | 2015-08-26 | 北京科技大学 | Pipeline steel resistant to carbon dioxide corrosion and preparation method thereof |
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- 2020-04-01 CN CN202010251583.0A patent/CN111533129A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN201545703U (en) * | 2009-09-28 | 2010-08-11 | 苏州市金宏气体有限公司 | Device for purifying carbon dioxide in recovered dry ice waste gas |
| CN104862607A (en) * | 2015-05-25 | 2015-08-26 | 北京科技大学 | Pipeline steel resistant to carbon dioxide corrosion and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 四川石油管理局, 石油工业出版社 * |
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