CN107673351A - A kind of production method of high-pureness carbon dioxide - Google Patents
A kind of production method of high-pureness carbon dioxide Download PDFInfo
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- CN107673351A CN107673351A CN201711160726.1A CN201711160726A CN107673351A CN 107673351 A CN107673351 A CN 107673351A CN 201711160726 A CN201711160726 A CN 201711160726A CN 107673351 A CN107673351 A CN 107673351A
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- carbon dioxide
- ethene
- liquefaction
- methane
- purifying column
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
- F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
- F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
- F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
- F25J3/0228—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream characterised by the separated product stream
- F25J3/0266—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream characterised by the separated product stream separation of carbon dioxide
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
- F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
- F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
- F25J3/08—Separating gaseous impurities from gases or gaseous mixtures or from liquefied gases or liquefied gaseous mixtures
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
- F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
- F25J2200/00—Processes or apparatus using separation by rectification
- F25J2200/04—Processes or apparatus using separation by rectification in a dual pressure main column system
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
- F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
- F25J2200/00—Processes or apparatus using separation by rectification
- F25J2200/38—Processes or apparatus using separation by rectification using pre-separation or distributed distillation before a main column system, e.g. in a at least a double column system
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
- F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
- F25J2200/00—Processes or apparatus using separation by rectification
- F25J2200/40—Features relating to the provision of boil-up in the bottom of a column
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
- F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
- F25J2200/00—Processes or apparatus using separation by rectification
- F25J2200/74—Refluxing the column with at least a part of the partially condensed overhead gas
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
- F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
- F25J2200/00—Processes or apparatus using separation by rectification
- F25J2200/80—Processes or apparatus using separation by rectification using integrated mass and heat exchange, i.e. non-adiabatic rectification in a reflux exchanger or dephlegmator
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
- F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
- F25J2205/00—Processes or apparatus using other separation and/or other processing means
- F25J2205/60—Processes or apparatus using other separation and/or other processing means using adsorption on solid adsorbents, e.g. by temperature-swing adsorption [TSA] at the hot or cold end
- F25J2205/66—Regenerating the adsorption vessel, e.g. kind of reactivation gas
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
- F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
- F25J2210/00—Processes characterised by the type or other details of the feed stream
- F25J2210/80—Carbon dioxide
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
- F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
- F25J2215/00—Processes characterised by the type or other details of the product stream
- F25J2215/04—Recovery of liquid products
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
- F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
- F25J2215/00—Processes characterised by the type or other details of the product stream
- F25J2215/80—Carbon dioxide
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
- F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
- F25J2220/00—Processes or apparatus involving steps for the removal of impurities
- F25J2220/80—Separating impurities from carbon dioxide, e.g. H2O or water-soluble contaminants
- F25J2220/82—Separating low boiling, i.e. more volatile components, e.g. He, H2, CO, Air gases, CH4
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
- F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
- F25J2245/00—Processes or apparatus involving steps for recycling of process streams
- F25J2245/90—Processes or apparatus involving steps for recycling of process streams the recycled stream being boil-off gas from storage
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
- F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
- F25J2270/00—Refrigeration techniques used
- F25J2270/90—External refrigeration, e.g. conventional closed-loop mechanical refrigeration unit using Freon or NH3, unspecified external refrigeration
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02C—CAPTURE, STORAGE, SEQUESTRATION OR DISPOSAL OF GREENHOUSE GASES [GHG]
- Y02C20/00—Capture or disposal of greenhouse gases
- Y02C20/40—Capture or disposal of greenhouse gases of CO2
Abstract
The present invention discloses a kind of production method of high-pureness carbon dioxide, it includes compression section, de- hydrocarbon process, cleaning procedure, liquefaction process and distillation two level purification process, wherein by distilling two level purification process, the purity of raw material is promoted to 99.95% by thick purifying column, purity is promoted to 99.999% through smart purifying column again, by two level purification process, the purity requirement to raw material is low, the loss of raw material is reduced, improves yield.
Description
Technical field
The present invention relates to carbon dioxide production technical field, in particular it relates to a kind of producer of high-pureness carbon dioxide
Method.
Background technology
The purposes of carbon dioxide is very wide, can be widely applied to the industries such as food processing, machine-building, industrial chemicals, its
Purification production is typically carried out by petrochemical industry tail gas, and it is high applied to the food-grade carbon-dioxide in food processing, its purity requirement
Up to 99.9%.The purification on the market for carbon dioxide can reach 99.99% at present, it can be difficult to reaching higher purity requirement
I.e. >=99.999%.And also have the method for the carbon dioxide product of production purity 99.999% on the market, but these methods pair
Higher in the requirement of raw materials for production, the purity requirement of the carbon dioxide of raw materials for production needs >=99%, is producing purity
Need that more raw material is lost during 99.999% carbon dioxide product, loss is relatively large, and practicality is not high.
The content of the invention
In view of the shortcomings of the prior art, the present invention provides a kind of production method of high-pureness carbon dioxide.
A kind of production method of high-pureness carbon dioxide disclosed by the invention, comprises the following steps:
(1) compression section
By the oxygen excessive with chemical reaction of the CO 2 raw material gas body containing impurity such as methane, ethene, benzene, mechanical waters
Enter compression section after separator goes out mechanical water, 0.1~0.35MPa, two-stage compression are boosted to through stage compressor
Machine boosts to 0.8~1.2MPa and three-stage blower boosts to 2.3~2.8MPa, is sent to after compression CO 2 raw material gas body de-
Hydrocarbon process;
(2) hydrocarbon process is taken off
The oxygen excessive with chemical reaction of CO 2 raw material gas body containing methane, ethene and benzene impurity after compression is entered
Enter de- hydrocarbon process, methane, the ethene oxygen excessive with chemical reaction in de- hydrocarbon reactor in temperature be 480~520 DEG C, pressure
It is raw to be chemically reacted in the presence of 2.3~2.8MPa, active component are platinum and palladium and carrier is aluminum oxide catalyst
Into carbon dioxide and water, remove the CO 2 raw material gas body after methane and ethene discharged from de- hydrocarbon reactor and with tube side
The CO 2 raw material gas body containing impurity such as trace methane, ethene, benzene from compression section converges, and is exchanged heat through heat exchanger
Water cooled but device cooling and separator are separated off mechanical water again afterwards, are sent to cleaning procedure;
(3) cleaning procedure
Using temperature swing adsorption process, more adsorption tower switch operatings, when wherein one or several adsorption towers are in adsorption-like
During state, remaining adsorption tower is in reproduced state, and adsorption tower is in normal temperature adsorbing contaminant, elevated temperature desorption impurity, by being seated in absorption
Aluminum oxide and silica gel absorber in tower contain trace methane, ethene, oxygen, benzene and vapor impurity to carry out autospasy hydrocarbon process
CO 2 raw material gas body in PPM levels micro water vapor and PPB levels micro-benzene impurity selective absorption, then will contain
There are trace methane, ethene, the carbon dioxide of oxygen impurities to be sent to liquefaction process and distilation process;
(4) liquefy process
A part for the carbon dioxide for containing impurity from cleaning procedure is entered as thermal source gas through orifice flowmeter
Enter the entrance of the thick purifying column of distilation process and the tower reactor coil pipe of smart purifying column, product liquid carbon dioxide is fully provided and steamed
The thermal source needed for purification is evaporated, is discharged from the outlet of the tower reactor coil pipe, with the carbon dioxide gas containing impurity from cleaning procedure
Another part of body, after the regulating valve outflow that the another part controls from the orifice flowmeter, the two parts merge together,
Evaporative condenser into liquefaction process is liquefied, and most of carbon dioxide containing impurity is liquefied, then with not
Carbon dioxide condensation gas and micro methane, ethene and oxygen are sent to distilation process together;
(5) two level purification process is distilled
Two after the liquefaction for containing uncooled carbon dioxide and trace methane, ethene and oxygen from liquefaction process
The thick purifying column that carbonoxide is introduced into distilation process carries out distilation, and tower top is from top to bottom respectively equipped with thick purifying column
Tubular heat exchanger, shower nozzle, individual layer corrugated plate regular packing and multiple tower reactor coil pipes, the evaporative condenser of shower nozzle connection liquefaction process
Device, containing uncooled carbon dioxide and trace methane, ethene and oxygen liquefaction after carbon dioxide be sprayed to from shower nozzle
Thick purifying column bottom of towe, tower reactor coil pipe are immersed in the carbon dioxide after liquefaction, the temperature of the carbon dioxide after liquefaction for -21~-
23 DEG C, in tower reactor coil pipe flowing have the carbon dioxide of distilation process, its temperature is 29~30 DEG C, the dioxy after liquefaction
Change carbon to be heated and volatilize and rise, the carbon dioxide of volatilization and the mixed gas of hydrocarbon impurities are regular by individual layer corrugated plating
Liquefied carbon dioxide under filler and shower nozzle spray exchanges heat, and the mixed gas of part volatilization liquefies and fallen after rise to thick purifying column tower
Bottom, another part mixed gas continue to rise to tower top tubular heat exchanger, and the pressure of mixed gas is 2.3Mpa, by decompression
Valve is decompressed to 0.8Mpa, and its temperature is down to -43~-47 DEG C, the heat transfer of mixture gas with rising, cools down the mixed gas of rising,
It is wherein carbon dioxide preferential condensation recovery, hydrocarbon impurities gas continues to rise, will be not cold from containing for liquefaction process
Coagulate the carbon dioxide after the liquefaction of carbon dioxide and trace methane, ethene and oxygen and complete thick purification;
The liquefied carbon dioxide of thick purifying column bottom of towe is passed through in smart purifying column, after thick purification in liquefied carbon dioxide
Containing trace methane, ethene, in smart purifying column from top to bottom be provided with lower floor's tubular heat exchanger, upper strata tubular heat exchanger, on
Layer corrugated plate regular packing, shower nozzle, lower floor's corrugated plate regular packing and multiple tower reactor coil pipes, the number of the tower reactor coil pipe of smart purifying column
For amount more than the quantity of the tower reactor coil pipe of thick purifying column, liquefied carbon dioxide is sprayed to the bottom of towe of smart purifying column from shower nozzle, multiple
Tower reactor coil pipe is immersed in liquefied carbon dioxide liquid, and multiple tower reactor coil pipes are passed through thermal source gas, and liquefied carbon dioxide is heated
Form the mixed gas containing trace methane, ethene, mixed gas volatilization rises, with spray downward liquefied carbon dioxide in
Lower floor's corrugated plate regular packing exchanges heat, the partial CO 2 condensing reflux in mixed gas to bottom of towe, in remaining mixed gas
Upper strata corrugated plate regular packing, partial CO 2 condensing reflux to bottom of towe are risen to, remaining mixed gas rises through lower stratose
Pipe heat exchanger exchanges heat, and which part carbon dioxide condensation liquefaction, another part mixed gas ascends into upper strata tubulation
Formula heat exchanger, the refrigerant of upper strata heat exchanger are liquefied ammonia, and liquefied ammonia is stored in the shell side of upper strata tubular heat exchanger, mixed gas with
Liquefied ammonia exchanges heat, gaseous carbonate dioxide condensate.
Compared with prior art, the present invention can be obtained including following technique effect:
The production method of the high-pureness carbon dioxide of the application is by distilling two level purification process, by thick purifying column by original
The purity of material is promoted to 99.95%, then purity is promoted into 99.999% through smart purifying column, by two level purification process, to original
The purity requirement of material is low, reduces the loss of raw material, improves yield.
Brief description of the drawings
Accompanying drawing described herein is used for providing further understanding of the present application, forms the part of the application, this Shen
Schematic description and description please is used to explain the application, does not form the improper restriction to the application.In the accompanying drawings:
Fig. 1 is the flow chart of the production method of high-pureness carbon dioxide in embodiment.
Embodiment
Multiple embodiments of the present invention, as clearly stated, the details in many practices will be disclosed with schema below
It will be explained in the following description.It should be appreciated, however, that the details in these practices is not applied to limit the present invention.Also
It is to say, in some embodiments of the present invention, the details in these practices is non-essential.In addition, for the sake of simplifying schema,
Some known usual structures will illustrate it in a manner of simply illustrative in the drawings with component.
It is to be appreciated that the directional instruction (such as up, down, left, right, before and after ...) of institute is only used in the embodiment of the present invention
In explaining the relative position relation under a certain particular pose (as shown in drawings) between each part, motion conditions etc., if should
When particular pose changes, then directionality instruction also correspondingly changes therewith.
In addition, the technical scheme between each embodiment can be combined with each other, but must be with ordinary skill
Personnel can be implemented as basis, and this technical side is will be understood that when the combination appearance of technical scheme is conflicting or can not realize
The combination of case is not present, also not within the protection domain of application claims.
1. compression section
The carbon dioxide for being about more than 70% by the carbon dioxide content containing impurity such as mechanical water, methane, ethene, benzene is former
Expect gas after washing, with adjusting the slight excess of oxygen mix of chemical reaction entered through orifice flowmeter, enter together pre-
The precooling of cooler 11, enter compression section 10 after the first separator 12 removes mechanical water, boosted to through stage compressor 13
0.1~0.35Mpa, split-compressor 14 boost to 0.8~1.2MPa and three-stage blower 15 boosts to 2.3~2.8MPa, from
The carbon dioxide containing impurity such as methane, ethene, benzene and the temperature of oxygen that three-stage blower 15 comes out are 110~120
DEG C, it is then delivered to de- hydrocarbon process 20.
2. de- hydrocarbon process
The carbon dioxide containing impurity such as methane, ethene, benzene and oxygen from compression section 10 initially enter de-
Hydrocarbon preheater 21 is preheating to 215~225 DEG C, is then heated to 480~520 DEG C by de- hydrocarbon heater 22, finally enters de- hydrocarbon
Reactor 23.Methane, ethene in de- hydrocarbon reactor 23 in the carbon dioxide containing impurity such as methane, ethene, benzene with
Oxygen chemically reacts in the presence of the catalyst that HTHP and active component are platinum and palladium, carrier are aluminum oxide, raw
Into carbon dioxide and water.When de- hydrocarbon preheater 21 is tubular heat exchanger, the high-temperature gas come out from de- hydrocarbon reactor 23 returns
The shell side of hydrocarbon preheater 21 back off, the carbon dioxide containing impurity such as methane, ethene, benzene from compression section 10 with tube side
After gas converting heat, first exchanged heat through heat exchanger 24 and following combined gas streams, then by the cooling of water cooler 30 and second
The separation machinery water of separator 40, into cleaning procedure 50.Removed by de- hydrocarbon process 20 and contain first from compression section 10
Most methane, ethene in the carbon dioxide of the impurity such as alkane, ethene, benzene are converted into carbon dioxide and water, therefore,
Contain into the carbon dioxide of cleaning procedure 50 either with or without the trace methane and ethene to be chemically reacted, and micro amount of oxygen
Gas and newly-generated but 40 indissociable vapor of the second separator.De- hydrocarbon heater 22 can be electric heater.De- hydrocarbon is anti-
Device 23 is answered to have the structure of general catalytic reactor.
3. cleaning procedure
Using temperature swing adsorption process, cleaning procedure 50 includes more adsorption tower switch operatings, when a certain or several absorption
When tower 51 is in adsorbed state, another or several adsorption towers 52 are in reproduced state, remaining one or several adsorption towers 53
Then it is in stand-by state, normal temperature adsorbing contaminant, elevated temperature desorption impurity, by the aluminum oxide and silica gel absorber being seated in adsorption tower
To in the carbon dioxide containing impurity such as trace methane, ethene, oxygen, benzene and vapor from the second separator 40
Micro water vapor (PPM levels) and micro-benzene (PPB levels) impurity selective absorption, to from the second separator 40 containing micro-
The carbon dioxide of the impurity such as amount methane, ethene, oxygen, benzene and vapor is purified.
1. adsorb
The carbon dioxide containing impurity such as trace methane, ethene, oxygen, benzene and vapor from the second separator 40
Gas enters from the bottom of adsorption tower, is discharged from the top of adsorption tower.In adsorption tower, adsorbent is to micro water vapor and micro
Benzene etc. is effectively adsorbed, and the indexs such as the water in the gas at adsorption column outlet end and benzene is reached respective design index or regulation mark
Standard, is then delivered to liquefaction process 60 and distilation process 70, and adsorbent adsorbs close to stopping during saturation.
2. inversely bleed off pressure
After adsorption step terminates, by the carbon dioxide gas containing impurity such as trace methane, ethene, oxygen in adsorption tower 51
Body against absorption direction current limliting release discharge adsorption tower 51 outside, terminate pressure in rear adsorption tower 51 close to normal pressure.
3. heating desorption impurity
The description to distilation process 70 seen below, from tower top tubular heat exchanger and lower floor's tubular heat exchanger shell
0.05MPa is depressurized to again after the adjusted throttling expansion of valve 716/728 of admixture of gas that journey comes out, with the ball from cooling working procedure excessively
The combined gas streams that the gas that tank 82 is discharged is formed after merging together are partly into heat exchanger 24, with carrying out autospasy hydrocarbon process
After the heat exchange of the carbon dioxide containing impurity such as trace methane, ethene, oxygen, benzene and vapor of 20 de- hydrocarbon preheater 21
It is heated up to 180~235 DEG C into electric heater 25, is desorbed into heating is in the adsorption tower 51 of impurity step,
Adsorbent is rinsed against the direction of absorption, adsorbent impurity is heated desorption, adsorbent is fully regenerated, then
Discharged as waste gas.
4. cool down adsorbent
After heating desorption impurity step terminates, the impurity such as adsorbent water and benzene in adsorption tower 51 has almost obtained
Complete solution is inhaled, and another part of combined gas streams now is fed directly into adsorption tower 51, the adsorbent in adsorption tower 51 is cooled
To≤25 DEG C.
5. adsorption tower pressurising
A part for the commonly referred to as adsorption tower 52 of adsorbed state is switched to pass through purification from reproduced state using to control oneself
The carbon dioxide containing impurity such as trace methane, ethene and oxygen after processing is pressurized to adsorptive pressure to adsorption tower 81
2.3~2.8MPa, it is prepared to enter into and adsorbs next time.
4. liquefy process
The titanium dioxide containing impurity such as trace methane, ethene and oxygen after purified treatment from cleaning procedure 50
A part for carbon gas enters the thick purifying column 71 of distilation process 70 through orifice flowmeter 61 as thermal source gas and essence purifies
The entrance of the tower reactor coil pipe 711/721 of tower 72, the thermal source needed for product liquid carbon dioxide distilation is fully provided, from tower reactor
The outlet discharge of coil pipe 711/721, with containing trace methane, ethene and oxygen after purified treatment from cleaning procedure 80
Another part of the carbon dioxide of the impurity such as gas, flowed out in the regulating valve 62 that the another part controls from orifice flowmeter 61
Afterwards, the two parts are merged together, and the first evaporative condenser 63 into liquefaction process 60 is liquefied.The of the process 60 that liquefies
The low-temperature receiver of one evaporative condenser 61 is liquefied ammonia, in the first evaporative condenser 63, contains the impurity such as trace methane, ethene and oxygen
Carbon dioxide fully carry out heat exchange with liquefied ammonia, the liquefied ammonia liquid level in the first evaporative condenser 63 is entered by regulating valve
The accurate control of row, makes most carbon dioxide fully be liquefied, turns into -23~-24 DEG C of liquid CO 2s, then send
Enter to distill two level purification process 70.
5. distill two level purification process
After the liquefaction for containing uncooled carbon dioxide and trace methane, ethene and oxygen from liquefaction process 60
The thick purifying column 71 that carbon dioxide is introduced into distillation two level purification process 70 carries out distilation, in thick purifying column 71 from top to bottom
Tower top tubular heat exchanger 714, shower nozzle 713, individual layer corrugated plate regular packing 712 and multiple tower reactor coil pipes 711 are respectively equipped with, is sprayed
First evaporative condenser 63 of first 713 connection liquefaction process 60, containing uncooled carbon dioxide and trace methane, ethene and
Carbon dioxide after the liquefaction of oxygen is sprayed to the thick bottom of towe of purifying column 71 from shower nozzle 713, and tower reactor coil pipe 711 is four tubules, sinks
It is dipped in the carbon dioxide after liquefaction, the temperature of the carbon dioxide after liquefaction is -21~-23 DEG C, is flowed in tower reactor coil pipe 711
The temperature of thermal source gas is 29~30 DEG C, i.e., the temperature difference of the carbon dioxide inside and outside tower reactor coil pipe 711 is close to 50 DEG C, the dioxy after liquefaction
Change carbon and hydrocarbon impurities therein are heated to boiling point and rising of volatilizing, the mixing of the carbon dioxide and hydrocarbon impurities of volatilization
The liquefied carbon dioxide exposure that gas is risen through under individual layer corrugated plate regular packing 713 sprays with shower nozzle 712 exchanges heat, part
The mixed gas of volatilization liquefies and falls after rise to the thick bottom of towe of purifying column 71, another part mixed gas and continue to rise to tower top shell and tube
Heat exchanger 714.Because the supply of thermal source only can not possibly make impurity volatilize, partial CO 2 can be made also to volatilize, individual layer corrugated plating
Structured packing 713 is also impossible to the carbon dioxide of fully effective cooling volatilization, therefore is changed again by tower top tubular heat exchanger 713
The carbon dioxide of recuperation of heat volatilization.The pressure of mixed gas is 2.3Mpa, and temperature is about -5 DEG C, and it rises to thick purifying column 71
For tower top outlet by the pressure-reducing valve expenditure and pressure of regulating valve 715 to 0.8Mpa, its temperature is down to -43~-47 DEG C, then is back to tower top
With the heat transfer of mixture gas of rising in tubular heat exchanger 714, cool down the mixed gas of rising, due to the boiling point of carbon dioxide
Boiling point compared to methane, ethene is higher, reclaims carbon dioxide preferential condensation, and hydrocarbon impurities gas continues upper lifting
Sky, so as to realize the liquid containing uncooled carbon dioxide and trace methane, ethene and oxygen from liquefaction process 60
Carbon dioxide after change completes thick purification;Can purifying to the carbon dioxide that purity is more than 70% by slightly purifying
99.95% or so purity.And the temperature after purified treatment from cleaning procedure 50 is 28~32 DEG C and contains micro first
The entrance tower reactor coil pipe of the carbon dioxide of the impurity such as alkane, ethene and oxygen fully provides product liquid two as thermal source gas
Thermal source needed for carbonoxide distilation, then discharged from the outlet of tower reactor coil pipe, discharge temperature is -9~-11 DEG C, into liquefaction
First evaporative condenser 63 of process 60 is liquefied.
The liquefied carbon dioxide of the thick bottom of towe of purifying column 71 is passed through in smart purifying column 72, liquefied titanium dioxide after thick purification
Contain trace methane, ethene in carbon, upper strata tubular heat exchanger 726, lower floor's shell and tube are from top to bottom provided with smart purifying column 72
Heat exchanger 725, upper strata corrugated plate regular packing 724, shower nozzle 723, lower floor's corrugated plate regular packing 722 and multiple tower reactor coil pipes
721, the quantity of the tower reactor coil pipe 721 of smart purifying column 72 is more than the quantity of the tower reactor coil pipe 711 of thick purifying column 71, and it includes 8
Tubule, by increasing the quantity of tubule, heat exchange area is increased, on the basis of identical thermal source, improves the utilization rate of thermal source,
Gaseous impurity is set to volatilize more clean thorough.Liquefied carbon dioxide is sprayed to the bottom of towe of smart purifying column 72 from shower nozzle, multiple
Tower reactor coil pipe 721 is immersed in liquefied carbon dioxide liquid, and multiple tower reactor coil pipes 721 are passed through thermal source gas, liquefied titanium dioxide
The liquefied temperature of carbon is -21~-23 DEG C, and the temperature of the thermal source gas flowed in tower reactor coil pipe 721 is 29~30 DEG C, liquefied
Carbon dioxide heating volatilization, the mixed gas containing trace methane, ethene is formed, mixed gas volatilization rises, downward with spraying
Liquefied carbon dioxide exchanged heat in lower floor's corrugated plate regular packing 722, the partial CO 2 condensing reflux in mixed gas
To bottom of towe, remaining mixed gas rises to upper strata corrugated plate regular packing 724, enters one by upper strata corrugated plate regular packing 724
Partial CO 2 gas therein is reclaimed in step condensation.Exchanged heat twice condensation by upper and lower two layers of corrugated plate regular packing, make to mix
Close most of carbon dioxide preferential condensation in gas and be back to bottom of towe, improve the yield of carbon dioxide.Remaining mixed gas rises
Exchanged heat by lower floor's tubular heat exchanger 725, which part carbon dioxide condensation liquefaction, another part mixed gas rises
Into upper strata tubular heat exchanger 726, the refrigerant of upper strata tubular heat exchanger 726 is liquefied ammonia, and liquefied ammonia is stored in upper strata tubulation
The shell side of formula heat exchanger 726, mixed gas exchange heat with liquefied ammonia, gaseous carbonate dioxide condensate.And not liquefied titanium dioxide
The tower top outlet that the mixed gas of carbon rises to smart purifying column 72 passes through the expenditure and pressure of pressure-reducing valve 727, then is back to lower floor's tower top
In tubular heat exchanger 725 with the heat transfer of mixture gas of rising.Liquefied twice condensation two by upper and lower two layers of tubular heat exchanger
Carbonoxide, different using the boiling point between gas with various, so as to reclaim carbon dioxide, successively separating hydrocarbons impurity, improves yield.And
The temperature after purified treatment from cleaning procedure 80 is 28~32 DEG C and contains the impurity such as trace methane, ethene and oxygen
The entrance tower reactor coil pipe 721 of carbon dioxide is used as thermal source gas, fully provides needed for product liquid carbon dioxide distilation
Thermal source, then discharged from the outlet of tower reactor coil pipe 721, discharge temperature is -9~-11 DEG C, into the first evaporation of liquefaction process 60
Condenser 63 is liquefied.
By above-mentioned thick purifying column to the preliminary purification in liquefied carbon dioxide, its purity is set to be promoted to 99.95% left
The right side, then it is high by four layers of condensation liquefaction in smart purifying column, further purification, the purity of the liquefied carbon dioxide finally given
Up to 99.999%.
6. cross cooling working procedure
The product liquid carbon dioxide through distilation in smart purifying column 72 from distillation two level purification process 70 is sent
To the second evaporative condenser 81 for crossing cooling working procedure 80, the low-temperature receiver of the second evaporative condenser 81 for crossing cooling working procedure 80 is liquefied ammonia, the
In two evaporative condensers 81, the temperature of product liquid carbon dioxide further reduces, and is further reduced the product liquid of temperature
Carbon dioxide is sent to product liquid carbon dioxide basin 82 through sequencing valve and stored.
The upper only embodiments of the present invention, are not intended to limit the invention.For those skilled in the art
For, the present invention can have various modifications and variations.All any modifications made in spirit and principles of the present invention, it is equal
Replace, improve etc., it all should be included within scope of the presently claimed invention.
Claims (1)
1. a kind of production method of high-pureness carbon dioxide, it is characterised in that comprise the following steps:
(1) compression section
CO 2 raw material gas body containing impurity such as methane, ethene, benzene, mechanical waters and the excessive oxygen of chemical reaction are passed through
Separator is gone out to enter compression section after mechanical water, and 0.1~0.35MPa, split-compressor liter are boosted to through stage compressor
It is depressed into 0.8~1.2MPa and three-stage blower boosts to 2.3~2.8MPa, de- hydrocarbon work is sent to after compressing CO 2 raw material gas body
Sequence;
(2) hydrocarbon process is taken off
CO 2 raw material gas body containing methane, ethene and benzene impurity after compression is entered with the excessive oxygen of chemical reaction and taken off
Hydrocarbon process, methane, the ethene oxygen excessive with chemical reaction in de- hydrocarbon reactor in temperature be 480~520 DEG C, pressure be
Chemically react, generate in the presence of the catalyst that 2.3~2.8MPa, active component are platinum and palladium and carrier is aluminum oxide
Carbon dioxide and water, remove the CO 2 raw material gas body after methane and ethene discharge from de- hydrocarbon reactor and with tube side
Converge from the CO 2 raw material gas body containing impurity such as trace methane, ethene, benzene of compression section, after heat exchanger exchanges heat
Water cooled but device cooling and separator are separated off mechanical water again, are sent to cleaning procedure;
(3) cleaning procedure
Using temperature swing adsorption process, more adsorption tower switch operatings, when wherein one or several adsorption towers are in adsorbed state,
Remaining adsorption tower is in reproduced state, and adsorption tower is in normal temperature adsorbing contaminant, elevated temperature desorption impurity, by being seated in adsorption tower
Aluminum oxide and silica gel absorber are to carrying out the dioxy containing trace methane, ethene, oxygen, benzene and vapor impurity of autospasy hydrocarbon process
Change the micro-benzene impurity selective absorption of the micro water vapor and PPB levels of the PPM levels in carbon raw material gas, then will contain micro
Methane, ethene, the carbon dioxide of oxygen impurities are sent to liquefaction process and distilation process;
(4) liquefy process
A part for the carbon dioxide for containing impurity from cleaning procedure enters as thermal source gas through orifice flowmeter steams
Evaporate the entrance of the thick purifying column of purification process and the tower reactor coil pipe of smart purifying column, there is provided product liquid carbon dioxide distilation institute
The thermal source needed, discharged from the outlet of the tower reactor coil pipe, it is another with the carbon dioxide containing impurity from cleaning procedure
Part, after the regulating valve outflow that the another part controls from the orifice flowmeter, the two parts merge together, into liquefaction
The evaporative condenser of process is liquefied, and most of carbon dioxide containing impurity is liquefied, then with uncooled dioxy
Change carbon gas and micro methane, ethene and oxygen are sent to distilation process together;
(5) two level purification process is distilled
Titanium dioxide after the liquefaction for containing uncooled carbon dioxide and trace methane, ethene and oxygen from liquefaction process
The thick purifying column that carbon is introduced into distilation process carries out distilation, and tower top tubulation is from top to bottom respectively equipped with thick purifying column
Formula heat exchanger, shower nozzle, individual layer corrugated plate regular packing and multiple tower reactor coil pipes, the evaporative condenser of shower nozzle connection liquefaction process,
Containing uncooled carbon dioxide and trace methane, ethene and oxygen liquefaction after carbon dioxide be sprayed to from shower nozzle and slightly carry
Pure tower bottom of towe, tower reactor coil pipe are immersed in the carbon dioxide after liquefaction, and the temperature of the carbon dioxide after liquefaction is -21~-23 DEG C,
Flowing has the carbon dioxide of distilation process in tower reactor coil pipe, and its temperature is 29~30 DEG C, the carbon dioxide after liquefaction
It is heated and volatilizees and rise, the carbon dioxide of volatilization and the mixed gas of hydrocarbon impurities passes through individual layer corrugated plate regular packing
Liquefied carbon dioxide under being sprayed with shower nozzle exchanges heat, and the mixed gas of part volatilization liquefies and fallen after rise to thick purifying column bottom of towe,
Another part mixed gas continues to rise to tower top tubular heat exchanger, and the pressure of mixed gas is 2.3Mpa, by pressure-reducing valve
0.8Mpa is decompressed to, its temperature is down to -43~-47 DEG C, the heat transfer of mixture gas with rising, cools down the mixed gas of rising, is
Wherein carbon dioxide preferential condensation reclaims, and hydrocarbon impurities gas continues to rise, will be uncooled from containing for liquefaction process
Carbon dioxide and trace methane, ethene and oxygen liquefaction after carbon dioxide complete thick purification;
The liquefied carbon dioxide of thick purifying column bottom of towe is passed through in smart purifying column, contained after thick purification in liquefied carbon dioxide
Trace methane, ethene, lower floor's tubular heat exchanger, upper strata tubular heat exchanger, upper strata ripple are from top to bottom provided with smart purifying column
Card structured packing, shower nozzle, lower floor's corrugated plate regular packing and multiple tower reactor coil pipes, the quantity of the tower reactor coil pipe of smart purifying column are big
In the quantity of the tower reactor coil pipe of thick purifying column, liquefied carbon dioxide is sprayed to the bottom of towe of smart purifying column, multiple tower reactors from shower nozzle
Coil pipe is immersed in liquefied carbon dioxide liquid, and multiple tower reactor coil pipes are passed through thermal source gas, and liquefied carbon dioxide is by thermosetting
Mixed gas containing trace methane, ethene, mixed gas volatilization rise, with spraying downward liquefied carbon dioxide in lower floor
Corrugated plate regular packing exchanges heat, and partial CO 2 condensing reflux to bottom of towe, remaining mixed gas in mixed gas rises to
Upper strata corrugated plate regular packing, partial CO 2 condensing reflux to bottom of towe, remaining mixed gas rise through lower floor's shell and tube
Heat exchanger exchanges heat, and which part carbon dioxide condensation liquefaction, another part mixed gas ascends into upper strata shell and tube and changed
Hot device, the refrigerant of upper strata heat exchanger is liquefied ammonia, and liquefied ammonia is stored in the shell side of upper strata tubular heat exchanger, mixed gas and liquefied ammonia
Heat exchange, gaseous carbonate dioxide condensate.
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