CN107673351B - 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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- CN107673351B CN107673351B CN201711160726.1A CN201711160726A CN107673351B CN 107673351 B CN107673351 B CN 107673351B CN 201711160726 A CN201711160726 A CN 201711160726A CN 107673351 B CN107673351 B CN 107673351B
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- 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
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- 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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- 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
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- F25J2200/00—Processes or apparatus using separation by rectification
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- F25J2200/00—Processes or apparatus using separation by rectification
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- F25J2200/00—Processes or apparatus using separation by rectification
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- 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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- F25J2210/00—Processes characterised by the type or other details of the feed stream
- F25J2210/80—Carbon dioxide
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- F25J2215/00—Processes characterised by the type or other details of the product stream
- F25J2215/04—Recovery of liquid products
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- F25J2215/00—Processes characterised by the type or other details of the product stream
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- 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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- 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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- 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
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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 second level purification process, wherein pass through distillation second 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, it is low to the purity requirement of raw material by second level purification process, the loss of raw material is reduced, yield is improved.
Description
Technical field
The present invention relates to carbon dioxide production technical fields, and in particular, to a kind of producer of high-pureness carbon dioxide
Method.
Background technique
The purposes of carbon dioxide is very wide, can be widely applied to the industries such as food processing, machine-building, industrial chemicals,
It is general that purification production is carried out by petrochemical industry tail gas, and the food-grade carbon-dioxide being applied in food processing, purity requirement are high
Up to 99.9%.99.99% can reach for the purification of carbon dioxide on the market 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, however these methods pair
>=99% is needed in the purity requirement of the more demanding of raw materials for production, the carbon dioxide of raw materials for production, is producing purity
Need to be lost more raw material when 99.999% carbon dioxide product, loss is relatively large, and practicability is not high.
Summary of the invention
In view of the deficiencies 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, comprising the following steps:
(1) compression section
By the CO 2 raw material gas body containing impurity such as methane, ethylene, benzene, mechanical waters and chemically react excessive oxygen
Enter compression section after separator removes mechanical water, boosts to 0.1~0.35MPa, two-stage compression 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
CO 2 raw material gas body after compression containing methane, ethylene and benzene impurity is sent with excessive oxygen is chemically reacted
Enter de- hydrocarbon process, methane, ethylene and chemically react excessive oxygen in de- hydrocarbon reactor in temperature be 480~520 DEG C, pressure
For 2.3~2.8MPa, active component be platinum and palladium and carrier be aluminium oxide catalyst under the action of chemically react, it is raw
At carbon dioxide and water, the CO 2 raw material gas body after removing methane and ethylene be discharged from de- hydrocarbon reactor and with tube side
The CO 2 raw material gas body containing impurity such as trace methane, ethylene, benzene from compression section converges, and exchanges heat through heat exchanger
It is cooled by water device cooling again afterwards and separator is separated off mechanical water, be 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
When state, remaining adsorption tower is in reproduced state, and adsorption tower is in room temperature adsorbing contaminant, elevated temperature desorption impurity, by being seated in absorption
Aluminium oxide and silica gel absorber in tower contain trace methane, ethylene, oxygen, benzene and water vapor impurity to carry out autospasy hydrocarbon process
CO 2 raw material gas body in PPM grade micro water vapor and PPB grades of micro benzene impurity selective absorption, then will contain
There is the carbon dioxide gas of trace methane, ethylene, oxygen impurities to be sent to liquefaction process and distillation and purification process；
(4) liquefaction process
A part of the carbon dioxide gas for containing impurity from cleaning procedure as heat source gas through orifice flowmeter into
The entrance for entering the thick purifying column of distillation and purification process and the tower reactor coil pipe of smart purifying column sufficiently provides product liquid carbon dioxide and steams
Heat source needed for evaporating purification, is discharged, with the carbon dioxide gas containing impurity from cleaning procedure from the outlet of the tower reactor coil pipe
Another part of body, after the regulating valve outflow that the another part is controlled from the orifice flowmeter, which is merged together,
Evaporative condenser into liquefaction process liquefies, and most of carbon dioxide gas containing impurity is liquefied, then and not
Carbon dioxide condensation gas and micro methane, ethylene and oxygen are sent to distillation and purification process together；
(5) second level purification process is distilled
Two after the liquefaction containing uncooled carbon dioxide gas and trace methane, ethylene and oxygen from liquefaction process
The thick purifying column that carbonoxide is introduced into distillation and purification process carries out distilation, is from top to bottom respectively equipped with tower top in thick purifying column
Tubular heat exchanger, spray head, single layer corrugated plate regular packing and multiple tower reactor coil pipes, spray head connect the evaporative condenser of liquefaction process
Device, the carbon dioxide after the liquefaction containing uncooled carbon dioxide gas and trace methane, ethylene and oxygen are sprayed to from spray head
Thick purifying column tower bottom, 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, the temperature of the heat source gas flowed in tower reactor coil pipe is 29~30 DEG C, and the carbon dioxide after liquefaction is heated and rising of volatilizing,
The carbon dioxide gas of volatilization and the mixed gas of hydrocarbon impurities are by the liquid under single layer corrugated plate regular packing and spray head spray
The carbon dioxide of change exchanges heat, and the mixed gas of part volatilization liquefies and falls after rise to thick purifying column tower bottom, another part mixed gas
Tower top tubular heat exchanger is continued to rise to, the pressure of mixed gas is 2.3Mpa, is decompressed to 0.8Mpa by pressure reducing valve, temperature
Degree is down to -43~-47 DEG C, the heat transfer of mixture gas with rising, and the cooling mixed gas risen, wherein carbon dioxide gas is preferential
Condensing recovery, hydrocarbon impurities gas continue to rise, and will contain uncooled carbon dioxide gas and micro first from liquefaction process
Carbon dioxide after the liquefaction of alkane, ethylene and oxygen completes thick purification；
The liquefied carbon dioxide of thick purifying column tower bottom is passed through in smart purifying column, after thick purification in liquefied carbon dioxide
Containing trace methane, ethylene, in smart purifying column from top to bottom be equipped with lower layer's tubular heat exchanger, upper layer tubular heat exchanger, on
Layer corrugated plate regular packing, spray head, lower layer's corrugated plate regular packing and multiple tower reactor coil pipes, the number of the tower reactor coil pipe of smart purifying column
Amount is greater than the quantity of the tower reactor coil pipe of thick purifying column, and liquefied carbon dioxide is sprayed to the tower bottom of smart purifying column from spray head, multiple
Tower reactor coil pipe is immersed in liquefied carbon dioxide liquid, and multiple tower reactor coil pipes are passed through heat source gas, and liquefied carbon dioxide is heated
Form the mixed gas containing trace methane, ethylene, mixed gas volatilization rises, with spray downward liquefied carbon dioxide in
Lower layer's corrugated plate regular packing exchanges heat, and the partial CO 2 in mixed gas is condensed back to tower bottom, in remaining mixed gas
Upper layer corrugated plate regular packing is risen to, partial CO 2 is condensed back to tower bottom, and remaining mixed gas rises through lower stratose
Pipe heat exchanger heat exchange, part of carbon dioxide gas condensation liquefaction, another part mixed gas ascend into upper layer tubulation
Formula heat exchanger, the refrigerant of upper layer heat exchanger are liquefied ammonia, and liquefied ammonia is stored in the shell side of upper layer tubular heat exchanger, mixed gas with
Liquefied ammonia heat exchange, gaseous carbonate dioxide condensate.
Compared with prior art, the present invention can be obtained including following technical effect:
The production method of the high-pureness carbon dioxide of the application, will be former by thick purifying column by distillation second level purification process
The purity of material is promoted to 99.95%, then purity is promoted to 99.999% through smart purifying column, by second level purification process, to original
The purity requirement of material is low, reduces the loss of raw material, improves yield.
Detailed description of the invention
The drawings described herein are used to provide a further understanding of the present application, constitutes part of this application, this Shen
Illustrative embodiments and their description please are not constituted an undue limitation on the present application for explaining the application.In the accompanying drawings:
Fig. 1 is the flow chart of the production method of high-pureness carbon dioxide in embodiment.
Specific embodiment
Multiple embodiments of the invention will be disclosed with schema below, as clearly stated, the details in many practices
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 invention, the details in these practices is non-essential.In addition, for the sake of simplifying schema,
Some known usual structures and component will be painted it in the drawings in simply illustrative mode.
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 in relative positional relationship, the motion conditions etc. under a certain particular pose (as shown in the picture) between each component, if should
When particular pose changes, then directionality instruction also correspondingly changes correspondingly.
It in addition, the technical solution between each embodiment can be combined with each other, but must be with ordinary skill
Based on personnel can be realized, this technical side will be understood that when the combination of technical solution appearance is conflicting or cannot achieve
The combination of case is not present, also not the present invention claims protection scope within.
1. compression section
The carbon dioxide for being about 70% or more by the carbon dioxide content containing impurity such as mechanical water, methane, ethylene, benzene is former
Expect gas after washing, adjust the slight excess of oxygen mix of chemical reaction entered with through orifice flowmeter, enters together pre-
Cooler 11 is pre-chilled, and enters compression section 10 after the first separator 12 removes mechanical water, boosts 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 temperature of the carbon dioxide gas containing impurity such as methane, ethylene, benzene and oxygen that three-stage blower 15 comes out is 110~120
DEG C, it is then delivered to de- hydrocarbon process 20.
2. de- hydrocarbon process
The carbon dioxide gas containing impurity such as methane, ethylene, benzene and oxygen from compression section 10 are first fed into 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, ethylene in de- hydrocarbon reactor 23 in the carbon dioxide gas containing impurity such as methane, ethylene, benzene with
Oxygen chemically reacts under the action of high temperature and pressure and active component are platinum and palladium, carrier are the catalyst of aluminium oxide, raw
At carbon dioxide and water.When de- hydrocarbon preheater 21 is tubular heat exchanger, the high-temperature gas come out from de- hydrocarbon reactor 23 is returned
The shell side of hydrocarbon preheater 21 back off, the carbon dioxide containing impurity such as methane, ethylene, benzene from compression section 10 with tube side
It after gas converting heat, first exchanges heat through heat exchanger 24 and following combined gas streams, using the cooling of water cooler 30 and second
40 separation machinery water of separator, into cleaning procedure 50.Contain first from compression section 10 by the de- removal of hydrocarbon process 20
Most methane, ethylene in the carbon dioxide gas of the impurity such as alkane, ethylene, benzene are converted into carbon dioxide and water, therefore,
Contain into the carbon dioxide gas of cleaning procedure 50 either with or without the trace methane and ethylene and micro amount of oxygen chemically reacted
Gas and the newly-generated but indissociable vapor of the second separator 40.De- hydrocarbon heater 22 can be electric heater.De- hydrocarbon is anti-
Answer device 23 that there can be the structure of general catalytic reactor.
3. cleaning procedure
Using temperature swing adsorption process, cleaning procedure 50 includes more adsorption tower switch operatings, is adsorbed when a certain or several
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, room temperature adsorbing contaminant, elevated temperature desorption impurity, by the aluminium oxide and silica gel absorber being seated in adsorption tower
To in the carbon dioxide gas containing impurity such as trace methane, ethylene, oxygen, benzene and vapor from the second separator 40
Micro water vapor (PPM grades) and micro-benzene (PPB grades) impurity selective absorption, to from the second separator 40 containing micro-
The carbon dioxide gas of the impurity such as amount methane, ethylene, oxygen, benzene and vapor is purified.
1. adsorbing
The carbon dioxide containing impurity such as trace methane, ethylene, 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 and benzene in the gas at adsorption column outlet end is made to reach corresponding design objective or regulation mark
Standard, is then delivered to liquefaction process 60 and distillation and purification process 70, and adsorbent is adsorbed close to stopping when being saturated.
2. inversely bleeding off pressure
After adsorption step, by the carbon dioxide gas containing impurity such as trace methane, ethylene, oxygen in adsorption tower 51
Body against absorption direction current limliting release discharge adsorption tower 51 outside, after pressure in adsorption tower 51 close to normal pressure.
3. heating desorption impurity
The description to distillation and purification process 70 seen below, from tower top tubular heat exchanger and lower layer's tubular heat exchanger shell
The admixture of gas that journey comes out is depressurized to 0.05MPa after 716/728 throttling expansion of regulating valve again, with the ball from supercooling process
A part of combined gas streams that the gas that tank 82 is discharged is formed after merging together enters heat exchanger 24, and carrys out autospasy hydrocarbon process
After the carbon dioxide gas heat exchange containing impurity such as trace methane, ethylene, oxygen, benzene and vapor of 20 de- hydrocarbon preheater 21
It is heated up into electric heater 25 to 180~235 DEG C, is desorbed in the adsorption tower 51 of impurity step into heating is in,
Adsorbent is rinsed against the direction of absorption, so that adsorbent impurity is heated desorption, adsorbent is sufficiently regenerated, then
It is discharged as exhaust gas.
4. cooling adsorbent
After heating desorption impurity step, the impurity such as adsorbent water and benzene in adsorption tower 51 have almost been obtained
Complete solution is inhaled, and another part of combined gas streams is fed directly to adsorption tower 51 at this time, the adsorbent in adsorption tower 51 is cooled
To≤25 DEG C.
5. adsorption tower pressurising
It is commonly referred to as a part of adsorption tower 52 by purification using come be switched to adsorbed state from reproduced state self
Treated, and the carbon dioxide gas containing impurity such as trace methane, ethylene and oxygen is pressurized to adsorptive pressure to adsorption tower 81
2.3~2.8MPa is prepared to enter into and adsorbs next time.
4. liquefaction process
The titanium dioxide containing impurity such as trace methane, ethylene and oxygen after purified treatment from cleaning procedure 50
A part of carbon gas enters the thick purifying column 71 of distillation and purification process 70 through orifice flowmeter 61 as heat source gas and essence purifies
The entrance of the tower reactor coil pipe 711/721 of tower 72, heat source needed for sufficiently providing product liquid carbon dioxide distilation, from tower reactor
The outlet of coil pipe 711/721 is discharged, and contains trace methane, ethylene and oxygen after purified treatment with from cleaning procedure 80
Another part of the carbon dioxide gas of the impurity such as gas is flowed out in the regulating valve 62 that the another part is controlled from orifice flowmeter 61
Afterwards, which merges together, and the first evaporative condenser 63 into liquefaction process 60 liquefies.The of liquefaction process 60
The cold source of one evaporative condenser 61 is that liquefied ammonia contains the impurity such as trace methane, ethylene and oxygen in the first evaporative condenser 63
Carbon dioxide gas sufficiently with liquefied ammonia carry out heat exchange, the liquefied ammonia liquid level in the first evaporative condenser 63 by regulating valve into
The accurate control of row, makes most carbon dioxide gas sufficiently be liquefied, becomes -23~-24 DEG C of liquid CO 2s, then send
Enter to distill second level purification process 70.
5. distilling second level purification process
After the liquefaction containing uncooled carbon dioxide gas and trace methane, ethylene and oxygen from liquefaction process 60
The thick purifying column 71 that carbon dioxide is introduced into distillation second level purification process 70 carries out distilation, in thick purifying column 71 from top to bottom
It is respectively equipped with tower top tubular heat exchanger 714, spray head 713, single layer corrugated plate regular packing 712 and multiple tower reactor coil pipes 711, is sprayed
First evaporative condenser 63 of first 713 connection liquefaction process 60, containing uncooled carbon dioxide gas and trace methane, ethylene and
Carbon dioxide after the liquefaction of oxygen is sprayed to thick 71 tower bottom of purifying column from spray head 713, and tower reactor coil pipe 711 is four tubules, sinks
In carbon dioxide after being dipped in 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 heat source gas is 29~30 DEG C, i.e. dioxy of the temperature difference of carbon dioxide inside and outside tower reactor coil pipe 711 close to 50 DEG C, after liquefaction
Change carbon and hydrocarbon impurities therein are heated to boiling point and rising of volatilizing, the mixing of the carbon dioxide gas and hydrocarbon impurities of volatilization
The liquefied carbon dioxide exposure that gas rises through under single layer corrugated plate regular packing 713 and the spray of spray head 712 exchanges heat, part
The mixed gas of volatilization liquefies and falls after rise to thick 71 tower bottom of purifying column, and another part mixed gas continues to rise to tower top shell and tube
Heat exchanger 714.Since the supply of heat source only can not make impurity volatilize, partial CO 2 can be made also to volatilize, single 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, rises to thick purifying column 71
For tower top outlet by 715 pressure reducing valve expenditure and pressure of regulating valve to 0.8Mpa, 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, keep the mixed gas risen cooling, due to the boiling point of carbon dioxide
Boiling point compared to methane, ethylene is higher, recycles carbon dioxide gas preferential condensation, and hydrocarbon impurities gas continues upper lifting
Sky, to realize the liquid containing uncooled carbon dioxide gas and trace methane, ethylene and oxygen from liquefaction process 60
Carbon dioxide after change completes thick purification；By slightly purifying purifying to for the carbon dioxide gas that can be 70% or more by purity
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 gas of the impurity such as alkane, ethylene and oxygen sufficiently provides product liquid two as heat source gas
Heat source needed for carbonoxide distilation, then be 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 liquefies.
The liquefied carbon dioxide of thick 71 tower bottom of purifying column is passed through in smart purifying column 72, liquefied titanium dioxide after thick purification
Contain trace methane, ethylene in carbon, is from top to bottom equipped with upper layer tubular heat exchanger 726, lower layer's shell and tube in smart purifying column 72
Heat exchanger 725, upper layer corrugated plate regular packing 724, spray head 723, lower layer'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 greater than the quantity of the tower reactor coil pipe 711 of thick purifying column 71 comprising 8
Tubule increases heat exchange area, on the basis of identical heat source, improves the utilization rate of heat source by the quantity of increase tubule,
Gaseous impurity is set to volatilize more clean thorough.Liquefied carbon dioxide is sprayed to the tower bottom of smart purifying column 72 from spray head, multiple
Tower reactor coil pipe 721 is immersed in liquefied carbon dioxide liquid, and multiple tower reactor coil pipes 721 are passed through heat source gas, liquefied titanium dioxide
The liquefied temperature of carbon is -21~-23 DEG C, and the temperature of the heat source gas flowed in tower reactor coil pipe 721 is 29~30 DEG C, liquefied
Carbon dioxide heating volatilization forms the mixed gas containing trace methane, ethylene, and mixed gas volatilization rises, downward with spray
Liquefied carbon dioxide exchange heat in lower layer's corrugated plate regular packing 722, the partial CO 2 in mixed gas is condensed back
To tower bottom, remaining mixed gas rises to upper layer corrugated plate regular packing 724, passes through upper layer corrugated plate regular packing 724 into one
Walk condensing recovery partial CO 2 gas therein.It is exchanged heat twice condensation by upper and lower two layers of corrugated plate regular packing, makes to mix
It closes most of carbon dioxide preferential condensation in gas and is back to tower bottom, improve the yield of carbon dioxide.Remaining mixed gas rises
It exchanges heat by lower layer's tubular heat exchanger 725, part of carbon dioxide gas condensation liquefaction, another part mixed gas rises
Into upper layer tubular heat exchanger 726, the refrigerant of upper layer tubular heat exchanger 726 is liquefied ammonia, and liquefied ammonia is stored in upper layer tubulation
The shell side of formula heat exchanger 726, mixed gas and liquefied ammonia exchange heat, gaseous carbonate dioxide condensate.And not liquefied titanium dioxide
The mixed gas of carbon rises to the tower top outlet of smart purifying column 72 by 727 expenditure and pressure of pressure reducing valve, then is back to lower layer's tower top
In tubular heat exchanger 725 with the heat transfer of mixture gas of rising.It is liquefied twice by upper and lower two layers of tubular heat exchanger and condenses two
Carbonoxide, different using the boiling point between gas with various, to recycle carbon dioxide, layer-by-layer 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, ethylene and oxygen
The entrance tower reactor coil pipe 721 of carbon dioxide gas is used as heat source gas, sufficiently provides needed for product liquid carbon dioxide distilation
Heat source, then from the outlet of tower reactor coil pipe 721 be discharged, discharge temperature be -9~-11 DEG C, into liquefaction process 60 first evaporation
Condenser 63 liquefies.
By above-mentioned thick purifying column to the preliminary purification in liquefied carbon dioxide, its purity is made to be promoted to 99.95% left side
The right side, then by four layers of condensation liquefaction in smart purifying column, further purify, the purity is high of finally obtained liquefied carbon dioxide
Up to 99.999%.
6. supercooling process
The product liquid carbon dioxide through distilation in smart purifying column 72 from distillation second level purification process 70 is sent
To the second evaporative condenser 81 of supercooling process 80, the cold source of the second evaporative condenser 81 of supercooling process 80 is liquefied ammonia, the
In two evaporative condensers 81, the temperature of product liquid carbon dioxide is further decreased, and is further reduced the product liquid of temperature
Carbon dioxide is sent to product liquid carbon dioxide basin 82 through sequencing valve and stores.
The upper only embodiments of the present invention, are not intended to restrict the invention.For those skilled in the art
For, the invention may be variously modified and varied.All any modifications made in spirit and principles of the present invention are equal
Replacement, improvement etc., should all be included within scope of the presently claimed invention.
Claims (1)
1. a kind of production method of high-pureness carbon dioxide, which comprises the following steps:
(1) compression section
By the CO 2 raw material gas body containing impurity such as methane, ethylene, benzene, mechanical waters and chemically react excessive oxygen process
Separator enters compression section after removing mechanical water, boosts to 0.1~0.35MPa, split-compressor liter through stage compressor
It is depressed into 0.8~1.2MPa and three-stage blower boosts to 2.3~2.8MPa, be sent to de- hydrocarbon work after compressing CO 2 raw material gas body
Sequence；
(2) hydrocarbon process is taken off
CO 2 raw material gas body after compression containing methane, ethylene and benzene impurity is taken off with excessive oxygen feeding is chemically reacted
Hydrocarbon process, methane, ethylene and the excessive oxygen of chemical reaction are in de- hydrocarbon reactor in temperature is 480~520 DEG C, pressure is
2.3~2.8MPa, active component be platinum and palladium and carrier be aluminium oxide catalyst under the action of chemically react, generate
Carbon dioxide and water, the CO 2 raw material gas body after removing methane and ethylene be discharged from de- hydrocarbon reactor and with tube side
Converge from the CO 2 raw material gas body containing impurity such as trace methane, ethylene, benzene of compression section, after heat exchanger exchanges heat
It is cooled by water device cooling again and separator is separated off mechanical water, is 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 room temperature adsorbing contaminant, elevated temperature desorption impurity, by being seated in adsorption tower
Aluminium oxide and silica gel absorber are to the dioxy containing trace methane, ethylene, oxygen, benzene and water vapor impurity for carrying out autospasy hydrocarbon process
The micro water vapor and PPB grades of micro benzene impurity selective absorption for changing the PPM grade in carbon raw material gas, then will contain micro
Methane, ethylene, oxygen impurities carbon dioxide gas be sent to liquefaction process and distillation and purification process；
(4) liquefaction process
A part of the carbon dioxide gas for containing impurity from cleaning procedure enters steaming through orifice flowmeter as heat source gas
The entrance for evaporating the thick purifying column of purification process and the tower reactor coil pipe of smart purifying column, provides product liquid carbon dioxide distilation institute
The heat source needed is discharged from the outlet of the tower reactor coil pipe, another with the carbon dioxide gas containing impurity from cleaning procedure
Part, after the regulating valve outflow that the another part is controlled from the orifice flowmeter, which is merged together, into liquefaction
The evaporative condenser of process liquefies, and most of carbon dioxide gas containing impurity is liquefied, then with uncooled dioxy
Change carbon gas and micro methane, ethylene and oxygen are sent to distillation and purification process together；
(5) second level purification process is distilled
Titanium dioxide after the liquefaction containing uncooled carbon dioxide gas and trace methane, ethylene and oxygen from liquefaction process
The thick purifying column that carbon is introduced into distillation and purification process carries out distilation, is from top to bottom respectively equipped with tower top tubulation in thick purifying column
Formula heat exchanger, spray head, single layer corrugated plate regular packing and multiple tower reactor coil pipes, spray head connect the evaporative condenser of liquefaction process,
Carbon dioxide after liquefaction containing uncooled carbon dioxide gas and trace methane, ethylene and oxygen is sprayed to from spray head slightly to be mentioned
Pure tower tower bottom, 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,
The temperature of the heat source gas flowed in tower reactor coil pipe is 29~30 DEG C, and the carbon dioxide after liquefaction is heated and rising of volatilizing, volatilization
Carbon dioxide gas and hydrocarbon impurities mixed gas sprayed by single layer corrugated plate regular packing and spray head under it is liquefied
The mixed gas of carbon dioxide heat exchange, part volatilization liquefies and falls after rise to thick purifying column tower bottom, and another part mixed gas continues
Tower top tubular heat exchanger is risen to, the pressure of mixed gas is 2.3Mpa, is decompressed to 0.8Mpa, temperature drop by pressure reducing valve
To -43~-47 DEG C, the heat transfer of mixture gas with rising cools down the mixed gas risen, wherein carbon dioxide gas preferential condensation
Recycling, hydrocarbon impurities gas continue to rise, and will contain uncooled carbon dioxide gas and trace methane, second from liquefaction process
Carbon dioxide after the liquefaction of alkene and oxygen completes thick purification；
The liquefied carbon dioxide of thick purifying column tower bottom is passed through in smart purifying column, is contained in liquefied carbon dioxide after thick purification
Trace methane, ethylene are from top to bottom equipped with lower layer's tubular heat exchanger, upper layer tubular heat exchanger, upper layer wave in smart purifying column
Card structured packing, spray head, lower layer'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 tower bottom of smart purifying column, multiple tower reactors from spray head
Coil pipe is immersed in liquefied carbon dioxide liquid, and multiple tower reactor coil pipes are passed through heat source gas, and liquefied carbon dioxide is by thermosetting
Mixed gas containing trace methane, ethylene, mixed gas volatilization rise, and downward liquefied carbon dioxide is in lower layer with spray
Corrugated plate regular packing exchanges heat, and the partial CO 2 in mixed gas is condensed back to tower bottom, remaining mixed gas rises to
Upper layer corrugated plate regular packing, partial CO 2 are condensed back to tower bottom, and remaining mixed gas rises through lower layer's shell and tube
Heat exchanger heat exchange, part of carbon dioxide gas condensation liquefaction, another part mixed gas ascend into upper layer shell and tube and change
The refrigerant of hot device, upper layer heat exchanger is liquefied ammonia, and liquefied ammonia is stored in the shell side of upper layer tubular heat exchanger, mixed gas and liquefied ammonia
Heat exchange, gaseous carbonate dioxide condensate.
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| CN108821288B (en) * | 2018-07-03 | 2020-08-07 | 杭州快凯高效节能新技术有限公司 | Preparation device and preparation process for producing high-quality liquid carbon dioxide |
| CN108975337B (en) * | 2018-08-29 | 2020-06-12 | 诸暨市霞伟花木场 | Liquid carbon dioxide production equipment |
| CN109704341A (en) * | 2019-03-12 | 2019-05-03 | 陕西裕隆气体有限公司 | The system of lighter hydrocarbons impurity in a kind of novel carbon dioxide removal |
| CN110422844A (en) * | 2019-08-20 | 2019-11-08 | 天津中科拓新科技有限公司 | A method of electronics grade carbon-dioxide is prepared by raw material of flue gas |
| CN111672236A (en) * | 2020-05-19 | 2020-09-18 | 茂名华粤华源气体有限公司 | Preparation method for separating and purifying liquid carbon dioxide |
| CN215113521U (en) * | 2021-03-24 | 2021-12-10 | 惠州凯美特气体有限公司 | Liquid carbon dioxide production equipment and system |
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