CN209442658U - A kind of production system of the ultrapure carbon dioxide of electron level - Google Patents
A kind of production system of the ultrapure carbon dioxide of electron level Download PDFInfo
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Abstract
The utility model belongs to gas generation field, the in particular to production system of a kind of ultrapure carbon dioxide of electron level.The production system specifically includes that carbon dioxide desulfurization tank (F1), regenerator (E1), heater (EH1), catalyzed conversion furnace (F2), water cooler (WE2), regenerative dryer, feed carbon dioxide subcooler (RU1), first order stripper (C1), first order stripper condenser (RU2), overhead separator (G1), C1 tower bottom reboiler (E2), second level stripper (C2), second level stripper condenser (RU3), overhead separator (G2), product carbon dioxide subcooler (RU4), the ultrapure carbon dioxide liquid basin (CG3) of electron level, C2 tower bottom reboiler (EH3), and several valves and pipeline for connecting each equipment.The production system and products thereof of the ultrapure carbon dioxide of electron level provided by the utility model can be widely applied, and have good market prospects.
Description
Technical field
The utility model belongs to gas generation field, the in particular to production system of a kind of ultrapure carbon dioxide of electron level.
Background technique
It is well known that carbon dioxide be mainly used for soda, gas shielded arc welding, tertiary oil recovery, supercritical fluid extraction,
Gas fertilizer, guarantor's solution, tobacco shred bulking etc., dosage and application range are all expanding year by year, it can be seen that, the separating-purifying of carbon dioxide
Technology is particularly important.The purification technique of carbon dioxide is CO2The basis of chemical developer and chemical field need to send out
One of critical issue of exhibition.With the fast development of the industries such as electronics, chemical industry, carbon dioxide chemical industry, electronics, metallurgy, food,
The fields such as machinery have been widely used, and at the same time, also increased dramatically to the demand of high-purity carbon dioxide.
Wherein, with the progress of the manufacturing technology of super large-scale integration, especially in the work cleaned to electronic component
In skill, correspondingly to the purity of carbon dioxide, more stringent requirements are proposed.
In regular industrial grade or the preparation method of food-grade carbon-dioxide, desulfurizing agent is generallyd use to reduce in product
Sulfur content, and with molecular sieve adsorption moisture, Some Enterprises also pass through the oxygen nitrogen that single tower distillation tower top discharge does not coagulate.In addition,
Food-grade carbon-dioxide is usually required using noble metal catalyst with the hydrocarbons content reduced in carbon dioxide of burning, so
And these devices carbon dioxide product produced is to obtain from the lower part of rectifying column, thus have more higher boiling miscellaneous
The purity of electron level is often not achieved so as to cause the purity of the carbon dioxide product as made from these prior arts for matter.
Currently, the domestic highest standard for carbon dioxide product is that GB 1886.228-2016 " mark by food safety country
Standard/food additives/carbon dioxide ".The standard is for food-class CO2" organoleptic requirements 3, physical and chemical index 18 " is defined,
Total 21 indexs (require CO after conversion2Purity >=99.9%).However, electronics industry is to CO234 index requests in, remove
Outside " benzene, methanol, acetaldehyde, ethylene oxide, vinyl chloride, hydrogen cyanide " 6 kinds of substances, cover in GB 1886.228-2016
All other requirements, and to CO2The requirement of overall purity is significantly larger than the existing standard.
Therefore, a kind of develop the ultrapure carbon dioxide of the electron level suitable for large-scale industrial production preparation process and its
Corresponding system becomes one of Research Challenges and hot spot of current Chemical R & D personnel.
Utility model content
The utility model is intended to overcome above-mentioned technological deficiency existing in the prior art, and provides a kind of efficiently using general
Logical technical grade or food-grade carbon-dioxide produce the method and its corresponding system of the ultrapure carbon dioxide of electron level, to meet precision
The ultrapure CO of large-scale use in the fields such as electronics industry2Demand.
Therefore, the utility model provides a kind of production system of ultrapure carbon dioxide of electron level comprising:
The intake pipeline 3 of gaseous carbon dioxide with pressure is connected to the entrance of carbon dioxide desulfurization tank F1, carbon dioxide desulfurization
The outlet of tank F1 connects the preheating entrance of regenerator E1, regenerator E1 by the export pipeline 4 of the carbon dioxide gas after desulfurization
Preheating outlet be sequentially connected heater EH1 and catalyzed conversion furnace F2；
Wherein, the outlet of catalyzed conversion furnace F2 connects the backheat by the carbon dioxide gas export pipeline 6 after taking off hydrocarbon
The recycling heat entrance of device E1；Titanium dioxide after de- hydrocarbon of the recycling heat outlet of the regenerator E1 by completing heat recovery
The export pipeline 7 of carbon gas connects the carbon dioxide entrance of water cooler WE2；
The carbon dioxide outlet of the water cooler WE2 is connected again by the carbon dioxide gas intake pipeline 8 before dehydration
The dry outlet of the drying entrance of raw formula drier, regenerative dryer passes through dewatered carbon dioxide gas export pipeline 9
The entrance of feed carbon dioxide subcooler RU1 is connected, the outlet of feed carbon dioxide subcooler RU1 passes through the raw material two after supercooling
Carbon oxide liquid export pipeline 13 connects the carbon dioxide entrance at the top of first order stripper C1；
The outlet of the tower top of first order stripper C1 is sequentially connected by the thick carbon dioxide export pipeline 15 containing fixed gas
First order stripper condenser RU2 and overhead separator G1；
Wherein, the outlet at the top of overhead separator G1 connects the thick carbon dioxide gas export pipeline 16 containing fixed gas, tower
Push up the reflux that separator G1 outlet at bottom connects the tower top of first order stripper C1 by thick carbon dioxide liquid export pipeline 17
Entrance；
The outlet of the tower reactor of first order stripper C1 connects liquid crude CO2Export pipeline is divided into two-way: first via liquid
The thick CO of body2Export pipeline is connected to the tower reactor entrance of first order stripper C1, and the first via liquid crude CO2Export pipeline
On be connected with C1 tower bottom reboiler E2；Second tunnel liquid crude CO2Export pipeline 18 is connected to the middle part of second level stripper C2
Carbon dioxide entrance；
The outlet of the tower top of second level stripper C2 passes through gas CO2Export pipeline is sequentially connected the condensation of second level stripper
Device RU3 and overhead separator G2；
Wherein, the export pipeline of gas phase carbon dioxide of the outlet connection containing fixed gas at the top of overhead separator G2, tower top
The bottom separator G2 bypass outlet is connected to the overhead reflux entrance of second level stripper C2, and overhead separator G2 bottoms goes out
Mouth connects the entrance of product carbon dioxide subcooler RU4, product carbon dioxide by the ultrapure carbon dioxide export pipeline 19 of liquid phase
The outlet of subcooler RU4 connects the ultrapure carbon dioxide liquid of electron level by the ultrapure carbon dioxide export pipeline 20 of liquid phase after supercooling
Body basin CG3；
Wherein, the second level stripper C2 is provided with C2 tower bottom reboiler EH3, the tower reactor of the second level stripper C2
Liquid CO of the outlet connection containing high-boiling-point impurity2Export pipeline 22.
Preferably, the feed carbon dioxide in the production system of the ultrapure carbon dioxide of above-mentioned electron level, after the supercooling
Liquid export line 13 passes sequentially through throttle valve, feed carbon dioxide liquid input tube line 14 is connected to the first order stripper
The carbon dioxide entrance at the top of C1.
The production system of the above-mentioned ultrapure carbon dioxide of electron level can be used for implementing a kind of life of ultrapure carbon dioxide of electron level
Production method comprising following steps:
Gaseous carbon dioxide with pressure is input in carbon dioxide desulfurization tank F1, after carbon dioxide desulfurization tank F1 exports desulfurization
Carbon dioxide gas；
Carbon dioxide gas after the desulfurization is introduced into regenerator E1 and preheats, and enters back into heater EH1 and is heated to 300
~500 DEG C, the carbon dioxide gas after de- hydrocarbon is exported subsequently into catalyzed conversion furnace F2, catalyzed conversion furnace F2；
Carbon dioxide gas after the de- hydrocarbon, which is introduced into regenerator E1, recycles heat, enters back into water cooler WE2, so
Enter regenerative dryer afterwards, regenerative dryer exports dewatered carbon dioxide gas；
The dewatered carbon dioxide gas enters feed carbon dioxide subcooler RU1, feed carbon dioxide subcooler
Feed carbon dioxide liquid after RU1 output supercooling；
Feed carbon dioxide liquid after the supercooling is throttled as feed carbon dioxide liquid；
The feed carbon dioxide liquid enters the top of first order stripper C1, as first order stripper phegma；
The tower top of first order stripper C1 exports the thick carbon dioxide containing fixed gas, the thick carbon dioxide containing fixed gas
It is introduced into first order stripper condenser RU2, enters back into overhead separator G1；Output is containing fixed gas at the top of overhead separator G1
Thick carbon dioxide gas, the bottom overhead separator G1 export thick carbon dioxide liquid, and the thick carbon dioxide liquid is back to the
The tower top of level-one stripper C1；
The thick CO of tower reactor output liquid of first order stripper C12, and split into two parts: first part liquid crude CO2Into
C1 tower bottom reboiler E2 is evaporated to gas, is then returned in first order stripper C1；Second part liquid crude CO2Into the second level
The middle part of stripper C2；
The tower top output gas CO of second level stripper C22, the gas CO2It is introduced into second level stripper condenser
RU3 enters back into overhead separator G2；The gas phase carbon dioxide containing fixed gas, overhead separator are exported at the top of overhead separator G2
The bottom G2 exports the ultrapure carbon dioxide of liquid phase, wherein a part of ultrapure carbon dioxide of liquid phase is back to second level stripper C2's
Tower top, the ultrapure carbon dioxide of another part liquid phase are input to electron level ultrapure two after product carbon dioxide subcooler RU4 supercooling
To get the ultrapure carbon dioxide product of electron level in carbon oxide liquid basin CG3；
Wherein, the second level stripper C2 is provided with C2 tower bottom reboiler EH3, the tower reactor of the second level stripper C2
Export the liquid CO containing high-boiling-point impurity2。
It is worth supplementary explanation, in the catalyzed conversion furnace F2, the NO that carries secretly in carbon dioxide gas2, NO divided
Solution passes through and excessive oxygen is added by the CH in carbon dioxide gas at oxygen and nitrogen4And other hydrocarbon conversions are two
Carbonoxide and water, so that taking off the content of the hydrocarbon in the carbon dioxide gas after hydrocarbon reduces to a certain extent.
Preferably, in the production system of the ultrapure carbon dioxide of above-mentioned electron level, the dewatered carbon dioxide gas
Export pipeline 9 is divided into two-way: wherein the carbon dioxide gas of the regeneration to be connected to the regenerative dryer is defeated all the way
Enter pipeline 10, wherein another way is the carbon dioxide to be subcooled for being connected to the entrance of the feed carbon dioxide subcooler RU1
The intake pipeline 11 of gas.
It is further preferred that in the production system of the ultrapure carbon dioxide of above-mentioned electron level, the titanium dioxide of the regeneration
Having heaters EH2 is connected on carbon gas inlet pipe line 10.
It is further preferred that in the production system of the ultrapure carbon dioxide of above-mentioned electron level, the titanium dioxide to be subcooled
The intake pipeline 11 of carbon gas passes sequentially through the connection of the carbon dioxide gas export pipeline 12 after C1 tower bottom reboiler E2, precooling
To the entrance of the feed carbon dioxide subcooler RU1.
Preferably, the production system of the ultrapure carbon dioxide of above-mentioned electron level further includes carbon dioxide recovery basin CG2, is connected
It is connected to the thick carbon dioxide gas export pipeline 16 containing fixed gas and the liquid CO containing high-boiling-point impurity2Export pipeline 22；
Also, it is provided with liquefier RU5 in the carbon dioxide recovery basin CG2, the dioxy for cooling liquid recycling
Change carbon；Incoagulable gas outlet, the carbon dioxide recovery basin CG2 are provided at the top of the carbon dioxide recovery basin CG2
Bottom is provided with the carbon dioxide liquid outlet of recycling.
It is further preferred that the production system of the above-mentioned ultrapure carbon dioxide of electron level further includes the carbon dioxide being sequentially connected in series
Basin CG1, liquid pressing pump P1 and feed carbon dioxide vaporizer WE1；Wherein, the feed carbon dioxide vaporizer WE1
Outlet connect the intake pipeline 3 of the gaseous carbon dioxide with pressure.In the preferred embodiment, the electron level ultrapure two
The production method of carbonoxide is further comprising the steps of:
Feed carbon dioxide is extracted out from feed carbon dioxide basin CG1, after liquid pressing pump P1 pressurization, enters back into original
Carbon dioxide carburettors WE1 is expected, to generate the gaseous carbon dioxide with pressure.In this case, the electron level ultrapure two
The production method of carbonoxide by liquid CO 2 vaporization, heating, desulfurization, the behaviour such as catalyzed conversion, be adsorbed by drying, freeze, purify
Make unit composition, is used for purifying industrial grade or food-grade carbon-dioxide to the ultrapure carbon dioxide of electron level.
It is further preferred that in the production system of the ultrapure carbon dioxide of above-mentioned electron level, the regenerative dryer is
Two molecular sieve adsorber MS1 and MS2 in parallel.In this case, when a molecular sieve adsorber MS1 operation is used for drying
While, another molecular sieve adsorber MS2 can then carry out on-line regeneration.
It is further preferred that in the production system of the ultrapure carbon dioxide of above-mentioned electron level, the C1 tower bottom reboiler E2,
The C2 tower bottom reboiler EH3 is each independently electric heater or gas heater (i.e. heat exchanger).
In addition, it is further preferred that in the production method of the ultrapure carbon dioxide of the electron level, the raw material titanium dioxide
Carbon subcooler RU1, the first order stripper condenser RU2, the second level stripper condenser RU3, the product dioxy
The cooling medium changed in the carbon subcooler RU4 and liquefier RU5 is selected from the refrigerants such as liquefied ammonia, R404A.
It is further preferred that the titanium dioxide in the production method of the ultrapure carbon dioxide of the electron level, after the desulfurization
H in carbon gas2S and SO2Respectively lower than 0.5mg/NM3；Hydrocarbon < 0.5ppm in carbon dioxide gas after the de- hydrocarbon.
Wherein, due to using the noble metal catalysts such as palladium, nickel, and the higher (300- of operating temperature in catalyzed conversion furnace F2
500 DEG C), the conversion ratio of hydrocarbon can be improved, so that the total hydrocarbon content < in the carbon dioxide gas after the de- hydrocarbon
0.5ppm。
It is worth noting that using the ultrapure carbon dioxide product of electron level made from production system described in the utility model
Middle CO2Purity >=99.9995%.Preferably, the oxygen in the ultrapure carbon dioxide product of the electron level, nitrogen, methane, an oxidation
Carbon, sulfur dioxide, total sulfur equal size≤50ppb, and total hydrocarbon, moisture≤100ppb.
It can be seen that technical solution provided by the utility model is mainly for carbon dioxide product made from prior art
Has the shortcomings that more high-boiling-point impurity, successfully developing and implementing a kind of twin-stage cryogenic rectification method reduces in carbon dioxide
The technique of high-boiling-point impurity content, and specifically provide the production method and its corresponding system of the ultrapure carbon dioxide of electron level.
In conclusion the cost of investment of device and system needed for the production method of the ultrapure carbon dioxide of electron level and
Operating cost is lower, and the production method of the ultrapure carbon dioxide of electron level is suitable for large-scale industrial production, securely and reliably；And
And according to CO in the ultrapure carbon dioxide product of electron level made from the production method2Purity be up to 99.9995% or more, because
This, meets the harsh standard and extensive demand in the fields such as precision electronic industries.In short, electron level provided by the utility model
Production system of ultrapure carbon dioxide and products thereof can be widely applied, and have good market prospects.
Detailed description of the invention
Fig. 1 is the structure of a preferred embodiment of the production system of the ultrapure carbon dioxide of electron level described in the utility model
Schematic diagram；
Wherein: 1- feed carbon dioxide export pipeline, the feed carbon dioxide export pipeline after 2- pressurization, 3- gaseous state with pressure
The intake pipeline of carbon dioxide, the export pipeline of the carbon dioxide gas after 4- desulfurization, 5- complete the dioxy after the desulfurization of preheating
Change carbon gas output tube line, 6- takes off the carbon dioxide gas export pipeline after hydrocarbon, and 7- completes the dioxy after the de- hydrocarbon of heat recovery
Change the export pipeline of carbon gas, the carbon dioxide gas intake pipeline before 8- dehydration, the dewatered carbon dioxide gas output of 9-
Pipeline, the carbon dioxide gas intake pipeline of 10- regeneration, the intake pipeline of carbon dioxide gas 11- to be subcooled, 12- are pre-
Carbon dioxide gas export pipeline after cooling, the feed carbon dioxide liquid export line after 13- supercooling, 14- raw material dioxy
Change carbon liquid body intake pipeline, thick carbon dioxide export pipeline of the 15- containing fixed gas, thick carbon dioxide gas of the 16- containing fixed gas
Export pipeline, the thick carbon dioxide liquid export pipeline of 17-, the second tunnel 18- liquid crude CO2Export pipeline, the ultrapure dioxy of 19- liquid phase
Change carbon export pipeline, the ultrapure carbon dioxide export pipeline of liquid phase after 20- supercooling, the carbon dioxide liquid efferent duct of 21- recycling
Line, liquid CO of the 22- containing high-boiling-point impurity2Export pipeline；
Wherein: CG1- feed carbon dioxide basin, CG2- carbon dioxide recovery basin, the ultrapure carbon dioxide of CG3- electron level
Liquid storage tank, P1- liquid pressing pump, WE1- feed carbon dioxide vaporizer, F1- carbon dioxide desulfurization tank, E1- regenerator,
EH1- heater, EH2- heater, EH3-C2 tower bottom reboiler, F2- catalyzed conversion furnace, WE2- water cooler, MS1- molecular sieve
Absorber, MS2- molecular sieve adsorber, E2-C1 tower bottom reboiler, G1- overhead separator, G2- overhead separator, RU1- raw material
Carbon dioxide subcooler, RU2- first order stripper condenser, the second level RU3- stripper condenser, RU4- product carbon dioxide
Subcooler, RU5- liquefier.
Specific embodiment
The production system of the ultrapure carbon dioxide of electron level of a preferred embodiment according to the present utility model is specific to wrap
It includes:
The intake pipeline 3 of gaseous carbon dioxide with pressure is connected to the entrance of carbon dioxide desulfurization tank F1, carbon dioxide desulfurization
The outlet of tank F1 connects the preheating entrance of regenerator E1, regenerator E1 by the export pipeline 4 of the carbon dioxide gas after desulfurization
Preheating outlet be sequentially connected heater EH1 and catalyzed conversion furnace F2；
Wherein, the outlet of catalyzed conversion furnace F2 connects the backheat by the carbon dioxide gas export pipeline 6 after taking off hydrocarbon
The recycling heat entrance of device E1；Titanium dioxide after de- hydrocarbon of the recycling heat outlet of the regenerator E1 by completing heat recovery
The export pipeline 7 of carbon gas connects the carbon dioxide entrance of water cooler WE2；
The carbon dioxide outlet of the water cooler WE2 is connected again by the carbon dioxide gas intake pipeline 8 before dehydration
The dry outlet of the drying entrance of raw formula drier, regenerative dryer passes through dewatered carbon dioxide gas export pipeline 9
The entrance of feed carbon dioxide subcooler RU1 is connected, the outlet of feed carbon dioxide subcooler RU1 passes through the raw material two after supercooling
Carbon oxide liquid export pipeline 13 connects the carbon dioxide entrance at the top of first order stripper C1；
The outlet of the tower top of first order stripper C1 is sequentially connected by the thick carbon dioxide export pipeline 15 containing fixed gas
First order stripper condenser RU2 and overhead separator G1；
Wherein, the outlet at the top of overhead separator G1 connects the thick carbon dioxide gas export pipeline 16 containing fixed gas, tower
Push up the reflux that separator G1 outlet at bottom connects the tower top of first order stripper C1 by thick carbon dioxide liquid export pipeline 17
Entrance；
The outlet of the tower reactor of first order stripper C1 connects liquid crude CO2Export pipeline is divided into two-way: first via liquid
The thick CO of body2Export pipeline is connected to the tower reactor entrance of first order stripper C1, and the first via liquid crude CO2Export pipeline
On be connected with C1 tower bottom reboiler E2；Second tunnel liquid crude CO2Export pipeline 18 is connected to the middle part of second level stripper C2
Carbon dioxide entrance；
The outlet of the tower top of second level stripper C2 passes through gas CO2Export pipeline is sequentially connected the condensation of second level stripper
Device RU3 and overhead separator G2；
Wherein, the export pipeline of gas phase carbon dioxide of the outlet connection containing fixed gas at the top of overhead separator G2, tower top
The bottom separator G2 bypass outlet is connected to the overhead reflux entrance of second level stripper C2, and overhead separator G2 bottoms goes out
Mouth connects the entrance of product carbon dioxide subcooler RU4, product carbon dioxide by the ultrapure carbon dioxide export pipeline 19 of liquid phase
The outlet of subcooler RU4 connects the ultrapure carbon dioxide liquid of electron level by the ultrapure carbon dioxide export pipeline 20 of liquid phase after supercooling
Body basin CG3；
Wherein, the second level stripper C2 is provided with C2 tower bottom reboiler EH3, the tower reactor of the second level stripper C2
Liquid CO of the outlet connection containing high-boiling-point impurity2Export pipeline 22.
In a preferred embodiment, the operating pressure of first order stripper C1 is 2-2.5MPa, second level stripper C2
Operating pressure be 1.6-2.5MPa；Certainly, the operating pressure of stripper can be further improved, but mean to consume more
Material and may cause lower separative efficiency.
In a preferred embodiment, the feed carbon dioxide liquid export line 13 after the supercooling passes sequentially through throttling
Valve, feed carbon dioxide liquid input tube line 14 are connected to the carbon dioxide entrance at the top of the first order stripper C1.
In a preferred embodiment, the dewatered carbon dioxide gas export pipeline 9 is divided into two-way: wherein one
Road is the carbon dioxide gas intake pipeline 10 for the regeneration for being connected to the regenerative dryer, and wherein another way is to be connected to
The intake pipeline 11 of the carbon dioxide gas to be subcooled of the entrance of the feed carbon dioxide subcooler RU1.
In a further preferred embodiment, it is connected on the carbon dioxide gas intake pipeline 10 of the regeneration
Heater EH2.
In a further preferred embodiment, the intake pipeline 11 of the carbon dioxide gas to be subcooled successively leads to
Carbon dioxide gas export pipeline 12 after crossing C1 tower bottom reboiler E2, precooling is connected to the feed carbon dioxide subcooler
The entrance of RU1.
In a preferred embodiment, the production system of the ultrapure carbon dioxide of the electron level further includes carbon dioxide recovery
Basin CG2 is connected with the thick carbon dioxide gas export pipeline 16 containing fixed gas and the liquid CO containing high-boiling-point impurity2Output
Pipeline 22；
Also, liquefier RU5 is provided in the carbon dioxide recovery basin CG2, the carbon dioxide recovery basin CG2
Top is provided with incoagulable gas outlet, and the bottom carbon dioxide recovery basin CG2 is provided with the carbon dioxide liquid of recycling
Outlet.
In a further preferred embodiment, the production system of the ultrapure carbon dioxide of electron level further includes successively
Concatenated carbon dioxide basin CG1, liquid pressing pump P1 and feed carbon dioxide vaporizer WE1；Wherein, the raw material dioxy
The outlet for changing carbon vaporizer WE1 connects the intake pipeline 3 of the gaseous carbon dioxide with pressure.
In a further preferred embodiment, the regenerative dryer is two molecular sieve adsorbers in parallel
MS1 and MS2.
In a further preferred embodiment, the C1 tower bottom reboiler E2, the C2 tower bottom reboiler EH3 are respectively
It independently is electric heater or gas heater.
The utility model is further elaborated With reference to embodiment, but the utility model be not limited to it is following
Embodiment.Each step in the method is routine operation unless otherwise specified, and each equipment unless otherwise specified can be from public affairs
Open commercial sources acquisition, wherein several valves and pipeline for connecting each equipment are all made of side known in the art
Formula carries out type selecting, connection and installation and therefore repeats no more herein.
Embodiment 1
Using production system as shown in Figure 1 for producing the ultrapure carbon dioxide product of electron level:
Firstly, feed carbon dioxide (2MPa) is extracted out from feed carbon dioxide basin CG1, through liquid pressing pump P1 pressurization
To 3.1MPa, into feed carbon dioxide vaporizer WE1, to generate gaseous carbon dioxide with pressure, temperature is 3~5 DEG C.
Then, the gaseous carbon dioxide with pressure is input in carbon dioxide desulfurization tank F1；Carbon dioxide desulfurization tank F1
Under the action of the desulfurizing agents such as interior active carbon, iron oxide, zinc oxide, so that H2S and SO2It is removed, thus the dioxy after desulfurization
Change the H in carbon gas2S and SO2Respectively lower than 0.5mg/NM3；Carbon dioxide gas after the desulfurization is introduced into regenerator E1
Preheating, enters back into heater EH1 and is heated to 300~500 DEG C, subsequently into catalyzed conversion furnace F2.
The noble metal catalysts such as palladium, nickel are used in catalyzed conversion furnace F2, and operating temperature is 300~500 DEG C, being used for will
The NO carried secretly in carbon dioxide gas2, NO resolves into oxygen and nitrogen, while passing through addition excessive oxygen will be in carbon dioxide gas
CH4And other hydrocarbon conversions are carbon dioxide and water, so that taking off containing for the hydrocarbon in the carbon dioxide gas after hydrocarbon
Measure < 0.5ppm.
It is introduced into regenerator E1 from the carbon dioxide gas after the de- hydrocarbon that the catalyzed conversion furnace F2 is exported and recycles heat
Amount, enters back into water cooler WE2, the carbon dioxide gas before 15 DEG C or so of dehydration is cooled to by low temperature chilled water.
Carbon dioxide gas before the dehydration enters molecular sieve adsorber MS1 or MS2, is dried, to remove moisture removal,
To export dewatered carbon dioxide gas.
Wherein, when molecular sieve adsorber MS1/MS2 is run, another molecular sieve adsorber MS2/MS1 can be into
Row on-line regeneration.
The dewatered carbon dioxide gas splits into two strands, and wherein one is the carbon dioxide gas of regeneration,
The molecular sieve adsorber MS1 or MS2 is flowed into after heated device EH2 heating, also, the carbon dioxide flowed out after regenerating enters
In carbon dioxide recovery basin CG2；Wherein another stock is carbon dioxide gas to be subcooled, and it is pre- to enter C1 tower bottom reboiler E2
After being cooled to partial liquefaction, then flow into feed carbon dioxide subcooler RU1.
Feed carbon dioxide liquid after the feed carbon dioxide subcooler RU1 output supercooling, becomes raw material after throttling
Carbon dioxide liquid；The feed carbon dioxide liquid enters the top of first order stripper C1, returns as first order stripper
Flow liquid.
Wherein, the uprising gas of the bottom first order stripper C1 is the gaseous state CO evaporated in C1 tower bottom reboiler E22, from
And it can obtain containing fixed gas that (wherein, fixed gas is primarily referred to as low-boiling O in tower top2, N2Equal gases) thick carbon dioxide.
Therefore, the thick carbon dioxide containing fixed gas of the tower top output of the first order stripper C1 enters first order stripping
It is condensed into partially liq in tower condenser RU2, enters back into overhead separator G1；Output contains fixed gas at the top of overhead separator G1
Thick carbon dioxide gas, further flow into carbon dioxide recovery basin CG2；The bottom overhead separator G1 output thick two
Carbon oxide liquid, the thick carbon dioxide liquid are back to the tower top of first order stripper C1.
The thick CO of tower reactor output liquid of the first order stripper C12, and split into two parts: first part liquid crude CO2
It is evaporated to gas into C1 tower bottom reboiler E2, is then returned in first order stripper C1；Second part liquid crude CO2Into
The middle part of second level stripper C2.
Wherein, the second level stripper C2 is provided with C2 tower bottom reboiler EH3, for heating vaporization CO2As stripping
Bottom rise gas；The tower top output gas CO of the second level stripper C22, the gas CO2It is introduced into second level stripper
Condenser RU3 enters back into overhead separator G2；The gas phase carbon dioxide containing fixed gas, tower top are exported at the top of overhead separator G2
The bottom separator G2 exports the ultrapure carbon dioxide of liquid phase, wherein a part of ultrapure carbon dioxide of liquid phase is back to second level stripping
The tower top of tower C2, the ultrapure carbon dioxide of another part liquid phase is after product carbon dioxide subcooler RU4 supercooling, after supercooling is made
The ultrapure carbon dioxide of liquid phase, finally, flowing into the ultrapure carbon dioxide liquid basin CG3 of electron level, so that it is super to have obtained electron level
Pure carbon dioxide product.
The tower reactor of the second level stripper C2 exports the liquid CO containing high-boiling-point impurity2, further flow into titanium dioxide
Carbon recycles in basin CG2.
The liquefier RU5 being arranged in carbon dioxide recovery basin CG2 is used for the carbon dioxide of cooling liquid recycling；It is described
Incoagulable gas (predominantly oxygen and nitrogen) is exported at the top of carbon dioxide recovery basin CG2, the carbon dioxide recovery basin
The carbon dioxide liquid of the bottom CG2 output recycling, and the carbon dioxide liquid of the recycling is back to feed carbon dioxide basin
In CG1, to be recycled.
Wherein, the C1 tower bottom reboiler E2 is heat exchanger, and the C2 tower bottom reboiler EH3 is electric heater.
Wherein, the feed carbon dioxide subcooler RU1, the first order stripper condenser RU2, the second level vapour
Cooling medium in stripper condenser RU3, the product carbon dioxide subcooler RU4 and the liquefier RU5 is
R404A refrigerant.
Specific embodiment of the utility model is described in detail above, but it is merely an example, this is practical new
Type is not restricted to particular embodiments described above.To those skilled in the art, any pair of the utility model carries out
Equivalent modifications and substitution also all among the scope of the utility model.Therefore, in the spirit and model for not departing from the utility model
Lower made equal transformation and modification are enclosed, should all be covered in the scope of the utility model.
Claims (9)
1. a kind of production system of the ultrapure carbon dioxide of electron level characterized by comprising
The intake pipeline (3) of gaseous carbon dioxide with pressure is connected to the entrance of carbon dioxide desulfurization tank (F1), carbon dioxide desulfurization
The outlet of tank (F1) is returned by the preheating entrance of export pipeline (4) connection regenerator (E1) of the carbon dioxide gas after desulfurization
The preheating outlet of hot device (E1) is sequentially connected heater (EH1) and catalyzed conversion furnace (F2)；
Wherein, the outlet of catalyzed conversion furnace (F2) connects the backheat by the carbon dioxide gas export pipeline (6) after taking off hydrocarbon
The recycling heat entrance of device (E1)；Two after de- hydrocarbon of the recycling heat outlet of the regenerator (E1) by completing heat recovery
The carbon dioxide entrance of export pipeline (7) connection water cooler (WE2) of carbon oxide gas；
The carbon dioxide outlet of the water cooler (WE2) is connected again by the carbon dioxide gas intake pipeline (8) before dehydration
The dry outlet of the drying entrance of raw formula drier, regenerative dryer passes through dewatered carbon dioxide gas export pipeline
(9) entrance of feed carbon dioxide subcooler (RU1) is connected, after the outlet of feed carbon dioxide subcooler (RU1) is by supercooling
Feed carbon dioxide liquid export line (13) connection first order stripper (C1) top carbon dioxide entrance；
The outlet of the tower top of first order stripper (C1) is sequentially connected by the thick carbon dioxide export pipeline (15) containing fixed gas
First order stripper condenser (RU2) and overhead separator (G1)；
Wherein, the outlet at the top of overhead separator (G1) connects the thick carbon dioxide gas export pipeline (16) containing fixed gas, tower
It pushes up separator (G1) outlet at bottom and passes through the tower top of thick carbon dioxide liquid export pipeline (17) connection first order stripper (C1)
Reflux inlet；
The outlet of the tower reactor of first order stripper (C1) connects liquid crude CO2Export pipeline is divided into two-way: first via liquid
Thick CO2Export pipeline is connected to the tower reactor entrance of first order stripper (C1), and the first via liquid crude CO2Export pipeline
On be connected with C1 tower bottom reboiler (E2)；Second tunnel liquid crude CO2Export pipeline (18) is connected to second level stripper (C2)
The carbon dioxide entrance at middle part；
The outlet of the tower top of second level stripper (C2) passes through gas CO2Export pipeline is sequentially connected second level stripper condenser
(RU3) and overhead separator (G2)；
Wherein, the export pipeline of gas phase carbon dioxide of the outlet connection containing fixed gas at the top of overhead separator (G2), tower top point
From the overhead reflux entrance that the bottom device (G2) bypass outlet is connected to second level stripper (C2), is produced from the overhead separator bottom (G2)
Entrance of the product outlet by ultrapure carbon dioxide export pipeline (19) connection product carbon dioxide subcooler (RU4) of liquid phase, product
The outlet of carbon dioxide subcooler (RU4) connects electron level by the ultrapure carbon dioxide export pipeline (20) of liquid phase after supercooling and surpasses
Pure carbon dioxide liquid storage tank (CG3)；
Wherein, the second level stripper (C2) is provided with C2 tower bottom reboiler (EH3), the tower of the second level stripper (C2)
Liquid CO of the kettle outlet connection containing high-boiling-point impurity2Export pipeline (22).
2. the production system of the ultrapure carbon dioxide of electron level according to claim 1, which is characterized in that after the supercooling
Feed carbon dioxide liquid export line (13) passes sequentially through throttle valve, feed carbon dioxide liquid input tube line (14) is connected to
The carbon dioxide entrance at the top of the first order stripper (C1).
3. the production system of the ultrapure carbon dioxide of electron level according to claim 1, which is characterized in that described dewatered
Carbon dioxide gas export pipeline (9) is divided into two-way: being wherein all the way the regeneration for being connected to the regenerative dryer
Carbon dioxide gas intake pipeline (10), wherein another way is the entrance for being connected to the feed carbon dioxide subcooler (RU1)
Carbon dioxide gas to be subcooled intake pipeline (11).
4. the production system of the ultrapure carbon dioxide of electron level according to claim 3, which is characterized in that the regeneration
Having heaters (EH2) is connected on carbon dioxide gas intake pipeline (10).
5. the production system of the ultrapure carbon dioxide of electron level according to claim 3, which is characterized in that described to be subcooled
Carbon dioxide gas after the intake pipeline (11) of carbon dioxide gas passes sequentially through C1 tower bottom reboiler (E2), precools exports
Pipeline (12) is connected to the entrance of the feed carbon dioxide subcooler (RU1).
6. the production system of the ultrapure carbon dioxide of electron level according to claim 1, which is characterized in that further include titanium dioxide
Carbon recycles basin (CG2), is connected with thick carbon dioxide gas export pipeline (16) containing fixed gas and containing high-boiling-point impurity
Liquid CO2Export pipeline (22)；
Also, it is provided with liquefier (RU5) in the carbon dioxide recovery basin (CG2), the carbon dioxide recovery basin
(CG2) top is provided with incoagulable gas outlet, and carbon dioxide recovery basin (CG2) bottom is provided with the titanium dioxide of recycling
Carbon liquid outlet.
7. the production system of the ultrapure carbon dioxide of electron level described according to claim 1~any one of 6, which is characterized in that
It further include the carbon dioxide basin (CG1) being sequentially connected in series, liquid pressing pumps (P1) and feed carbon dioxide vaporizer (WE1)；
Wherein, the outlet of the feed carbon dioxide vaporizer (WE1) connects the intake pipeline (3) of the gaseous carbon dioxide with pressure.
8. the production system of the ultrapure carbon dioxide of electron level described according to claim 1~any one of 6, which is characterized in that
The regenerative dryer is two molecular sieve adsorbers (MS1, MS2) in parallel.
9. the production system of the ultrapure carbon dioxide of electron level described according to claim 1~any one of 6, which is characterized in that
The C1 tower bottom reboiler (E2), the C2 tower bottom reboiler (EH3) are each independently electric heater or gas heater.
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Effective date of registration: 20210514 Address after: 201800 rooms 202 and 204, building 3, 150 Heyu Road, Jiading District, Shanghai Patentee after: SHANGHAI QIYUAN GAS DEVELOPMENT Co.,Ltd. Address before: 201800 150 Heyu Road, Jiading District, Shanghai Patentee before: SHANGHAI QIYUAN AIR SEPARATE TECHNOLOGY DEVELOPMENT Co.,Ltd. |
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Inventor after: Zhou Darong Inventor after: Yu Jian Inventor after: Chen Zhicheng Inventor before: Zhou Darong Inventor before: Yu Jian Inventor before: Chen Zhicheng |
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