CN109721054A - The production method and device of scale electronic grade high-purity carbon dioxide - Google Patents
The production method and device of scale electronic grade high-purity carbon dioxide Download PDFInfo
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- CN109721054A CN109721054A CN201910207776.3A CN201910207776A CN109721054A CN 109721054 A CN109721054 A CN 109721054A CN 201910207776 A CN201910207776 A CN 201910207776A CN 109721054 A CN109721054 A CN 109721054A
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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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- 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
- 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
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- F25J2205/00—Processes or apparatus using other separation and/or other processing means
- F25J2205/82—Processes or apparatus using other separation and/or other processing means using a reactor with combustion or catalytic reaction
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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
- F25J2205/00—Processes or apparatus using other separation and/or other processing means
- F25J2205/84—Processes or apparatus using other separation and/or other processing means using filter
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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
- F25J2215/80—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
- 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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- 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
- F25J2220/84—Separating high boiling, i.e. less volatile components, e.g. NOx, SOx, H2S
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
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- F25J2230/00—Processes or apparatus involving steps for increasing the pressure of gaseous process streams
- F25J2230/80—Processes or apparatus involving steps for increasing the pressure of gaseous process streams the fluid being carbon dioxide
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
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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
- F25J2245/02—Recycle of a stream in general, e.g. a by-pass stream
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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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- 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
- F25J2270/02—Internal refrigeration with liquid vaporising loop
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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
- 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
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Abstract
The present invention relates to carbon dioxide production technical fields, and in particular to a kind of production method and device of scale electronic grade high-purity carbon dioxide.The production method includes distillation unit, takes off hydrocarbon unit, dewatering unit, liquefaction unit, purifier units and gas recovery unit.The present invention provides the device of a set of large-scale production electronic grade high-purity carbon dioxide, the electronic grade high-purity carbon dioxide of production, purity can be up to 99.999% or more.The advantages that present invention simultaneously provides the devices that it is used, and have technical maturity easy to operate, and system runs smoothly, and operating cost is low, and resource utilization is high, and effects of energy saving and emission reduction is significant, stable product quality, gas reclaiming rate is high.
Description
Technical field
The present invention relates to carbon dioxide production technical fields, and in particular to a kind of scale electronic grade high-purity carbon dioxide
Production method and device.
Background technique
Current You Shangbaijia carbon dioxide production enterprise, country, due to the limitation of gas source and purification technique, product quality with
It is also irregular to purify cost.Its product orientation is concentrated mainly on industrial grade carbon-dioxide and food additives carbon dioxide.It is high
High-end product of the pure carbon dioxide as carbon dioxide field, since the limitation of its market demand and technical conditions enables many productions
Enterprise hangs back.
The high-purity carbon dioxide of domestic supply depends on domestic Pilot Unit and external import, largely
Constrain China's expanding economy.
Chinese patent 201811086098.1 discloses a kind of using multitower rectifying coproduction technical grade, food-grade and high-purity fluid
The device and method of body carbon dioxide.This method is the simple method of purification for utilizing rectifying, is extracted from the different height of rectifying column
The product of different levels, theoretically produce technical grade and food-grade liquid carbon dioxide may be implemented completely, but high-purity dioxy
It is very harsh to impurity requirement to change carbon, simple rectifying mode is difficult impurity to remove thoroughly, especially contains impurity in unstripped gas
Boiling point and the very close component of carbon dioxide, such as C2, C3, C4 boiling point and molecular structure and carbon dioxide connect very much
Closely, it is desirable to Control of Impurities is extremely difficult in 2PPM or less, so above-mentioned technique production technical grade and food-grade carbon-dioxide energy
Enough reach index of correlation, but it is just very harsh to produce requirement of the high-purity carbon dioxide to unstripped gas.
Chinese patent 20171160726.1 illustrates a kind of production method of high-pureness carbon dioxide, and this method is using biography
The pressure and temperature varying absorption method of system, which is product purity height, wider to the claimed range of gas source.Its disadvantage is mainly
Complex process, operation difficulty are larger；Power consumption is high (adsorbent regular regeneration, replacement)；Gas collection rate is low, simple by constantly adjusting
Whole pressure and temp is alternately repeated the mode of operation to control adsorbent to capture-release of carbon dioxide, must cause running
It results in waste of resources in the process.
Summary of the invention
In view of the deficiencies of the prior art, the object of the present invention is to provide a kind of large-scale production electronic grade high-purity carbon dioxide
Production method, have that technical maturity is easy to operate, operating cost is low, the high advantage of stable product quality, gas reclaiming rate；This hair
It is bright while its device used being provided.
The production method of large-scale production electronic grade high-purity carbon dioxide of the present invention is as follows:
Device used in production method is as follows:
The device includes rectifying column, and the gaseous phase outlet of rectifying column is connected with the cold source import of preheater, the cold source of heat exchanger
Outlet is connected with the import of dealkylation tower, and the outlet of dealkylation tower is connected with the heat source import of preheater；
The thermal source outlet of preheater is connected with the heat source import of ammonia cooler, the thermal source outlet of ammonia cooler and the first drying tower
Import is connected, and the outlet of the first drying tower is connected with the import of the second drying tower, the outlet and filter inlet of the second drying tower
It is connected；
Filter outlet is connected with plate-fin carbon dioxide condenser heat source import, the heat of plate-fin carbon dioxide condenser
Source outlet is connected with carbon dioxide buffer tank import, the import of the cold source outlet ammonia liquor separator of plate-fin carbon dioxide condenser
It is connected；
Carbon dioxide buffer tank outlet difference pass course a connects the cold source import of purifying column overhead condenser with route b
Cold source outlet with the feed inlet of purifying column, purifying column overhead condenser is connected with the cold source import of pressurization gas heat exchanger, increases
The cold source outlet of pressure gas heat exchanger is connected with the air entry of carbon-dioxide gas compressor, the exhaust outlet of carbon-dioxide gas compressor and increasing
The heat source import of gas heat exchanger is pressed to be connected, the heat exchange coil of the thermal source outlet of pressurization gas heat exchanger and the setting of purifying column lower part
Heat source import be connected, the thermal source outlet of heat exchange coil is connected with carbon dioxide product surge tank import,
The outlet of carbon dioxide product surge tank is connected with the heat source import of stripping tower tower bottom reboiler bottom, stripping tower tower bottom
The thermal source outlet of reboiler is connected with stripping tower import, and the outlet of stripping tower is connected with liquid CO 2 storage tank import, stripping tower
The gas outlet at top is connected with the cold source import of pressurization gas heat exchanger, the gas outlet of liquid CO 2 tank top and pressurization
The cold source import of gas heat exchanger is connected；
The gas vent of ammonia liquor separator is connected with the air entry of screw compressor, and the liquid outlet of ammonia liquor separator is logical
Liquid back pipe is crossed to be connected with the cold source import of plate-fin carbon dioxide condenser,
The heat source import of the heat exchange coil of the exhaust outlet and rectifying column of screw compressor is connected, and the heat source of heat exchange coil goes out
Mouth is connected with the import of ammonia storage tank, and the outlet of ammonia storage tank is connected with the cold source import of plate-fin carbon dioxide condenser, ammonia storage tank
Top gas outlet is connected with the import of evaporative condenser, and the outlet of evaporative condenser is connected with the import of Siphon pot, siphon
The outlet at bottom of tank is connected with the cold source import of screw-compression oil cooler, and the cold source of screw-compression oil cooler goes out
Mouth is connected with Siphon pot import, and the centre exit of Siphon pot is connected with the import of ammonia storage tank,
The outlet of ammonia storage tank is connected with the cold source import of the top of the distillation column condenser, and the cold source of the top of the distillation column condenser goes out
Mouth is connected with the import of ammonia liquor separator；
Wherein, the intracavitary portion of the tower of the rectifying column and purifying column sets gradually overhead condenser, destilling tower from top to bottom
And reboiler, reboiler, that is, heat exchange coil；Rectifying tower bottom is separately connected tower chamber and tower bottom reboiler shell side by extracting pipeline out
Import is extracted setting cryogenic shield on pipeline out and is pumped；
The production method the following steps are included:
(1) distillation unit
Unstripped gas is decompressed to 4.2-4.5MPa through throttling and enters rectifying column, ripple plate gauge is uniformly distributed after spray head sprays
On whole filler, after the exhaust heat exchange with the screw compressor in rectifier bottoms heat exchange coil, the lower liquid group of boiling point
Divide endothermic gasification, rises at the top of rectifying column, into de- hydrocarbon unit；
The higher liquid component of boiling point is deposited in rectifying tower bottom, extraction rear portion enter rectifying tower reboiler shell side with
It vaporizes return system after the screw compressor exhaust gas heat exchanging of tube side to be recycled, the high boiling component that cannot be vaporized is arranged through bottom
Mouth discharge is put, another part is back to rectifying column for adjusting rectifying column liquid level.
The core content of this unit is thoroughly to remove high boiling impurity by being precisely controlled regurgitant volume and boiling temperature again
The content of (free state water, high-carbon hydrocarbon), gas vent water is less than 5ppm,.
The high-temperature exhaust air of screw compressor is introduced into the heat exchange coil at destilling tower bottom as the source boiling hot again of carbon dioxide
It uses.High-temperature exhaust air entrance installs motor-driven valve and bypass, and the open degree by adjusting motor-driven valve and bypass is precisely controlled boils again
Temperature 60 DEG C (most preferably boiling temperature) again.Temperature is boiled again higher than 60 DEG C, turns motor-driven valve open degree down；Temperature is boiled again is lower than 60 DEG C,
Open big motor-driven valve open degree.Not only dexterously accomplish Waste Heat Reuse but also solve technologic heat source demand.It is greatly lowered simultaneously
Screw compressor high-temperature exhaust air enters the temperature before evaporative condenser, to greatly reduce the work of evaporative condenser
Make load, energy-saving effect is obvious.
Using tower bottom reboiler, destilling tower, the rectifying column of three tower of overhead condenser unification.Occupied area is small, fixed to throw
Money is few, and loss of refrigeration capacity is small.
Overhead condenser uses shell-and-tube heat exchanger, and tube side is liquefied ammonia, shell side carbon dioxide.Liquefied ammonia import is equipped with motor-driven valve
And flowmeter, the size of regurgitant volume is precisely controlled by adjusting the flow of liquefied ammonia (regurgitant volume in the side 2.0--3.0/h, according to production
Amount and different product grade are adjusted).The liquid CO 2 to flow back is uniformly distributed on corrugated plate regular packing, and from tower
The gas converting heat that bottom is boiled up again, so that the high-boiling-point impurity component (vaporous water, high-carbon hydrocarbon) in the gas be made to be condensed into again
Liquid is settled down to distillation tower bottom, to achieve the effect that separate high-boiling-point impurity.
Distillation tower bottom is equipped with cryogenic shield pump (one open one standby).The liquid component for being deposited to distillation tower bottom can gradually increase
More, processing will be unable to normally produce not in time.After the liquid composition at destilling tower bottom being extracted out by canned motor pump, be divided into two parts,
A part returns to destilling tower, for controlling the liquid level of destilling tower in reasonable range (1250-1750mm, too high or too low all shadows
Ring normal production technology)；Another part goes distillation tower reboiler, because still containing a large amount of carbon dioxide in the partially liq,
Heat absorption vaporization again, return system are recycled in reboiler.The impurity composition that cannot be vaporized gradually converges in reboiler bottom
Portion, the discharge outlet discharge system through bottom.
(2) hydrocarbon unit is taken off
The CO 2 raw material gas come at the top of autospasy hydrocarbon unit rectifying column is after throttling is decompressed to 3.5-3.8MPa, through cold source
Import enters preheater, after the gas converting heat after high-temperature oxydation, is reacted into dealkylation tower with excessive oxygen, gas after reaction
Body through heat source import enters preheater preheating material gas after being discharged by dealkylation tower, then by after the discharge of preheater thermal source outlet through heat
Source import enters ammonia cooler and low-temperature liquid ammonia exchanges heat, and the gas after heat exchange enters dewatering unit through thermal source outlet.
The core concept of this unit scheme be in the case where guaranteeing the process effective operation, effectively reduce operation at
This.
Domestic prior art is that the carbon dioxide of room temperature is heated to 300 DEG C or more using electric heater, this needs to consume
A large amount of electric energy, the high-temperature gas after catalytic oxidation need water cooling to be down to room temperature, this just needs to consume a large amount of cooling water, presses
3.5 tons of reacting dose per hour, minimum to need 30 vertical/hour cooling waters, operating cost is very high.
The present invention has carried out following innovation:
A, a shell-and-tube heat exchanger (preheater) is added before dealkylation tower, the gas before catalysis oxidation walks shell side, catalysis
Gas after oxidation walks tube side, using the high-temperature gas preheating material gas after catalytic oxidation, and changing in dealkylation tower lower part
It exchanges heat again in hot coil, so that unstripped gas temperature before entering electric heating is reached 180-200 DEG C, greatly reduce disappearing for electric energy
Consumption.The gas temperature after catalytic oxidation is down to 100-130 DEG C simultaneously, and significantly reduces the load of subsequent heat exchanger.
B, a shell-and-tube heat exchanger (ammonia cooler) is added after dealkylation tower, makes full use of liquid ammonia vaporization latent heat and catalysis oxygen
Gas after changing reaction carries out heat exchange, no longer adds a large amount of cooling needed for cooling tower required for common process and operation
Water has the advantages that process operation is steady, easy to operate, energy-saving.
(3) dewatering unit
The unstripped gas for carrying out autospasy hydrocarbon unit sequentially enters the first drying tower and the second drying tower is dehydrated, dewatered gas
Body enters liquefaction unit.
The core content of this unit scheme is that rough removing tower (the first drying tower) and fine removing tower (the second drying tower) is transported in technique
Being effectively applied in combination in row.
The present invention fully takes into account different product level and requires the difference of moisture content index, provided with different purification depth
Equipment.Rough removing tower selects aluminium oxide, and advantage is that dehydrating amount is big, and cost is relatively low.Fine removing tower uses efficient molecular sieve, and advantage is dehydration
Precision is high.The advantage for making full use of rough removing tower dehydrating amount big, effectively reduces product cost under the premise of meeting product quality.
After fine removing tower is dropped in rough removing tower when producing electronic grade high-purity carbon dioxide, to slightly take off later gas again into
Row processing, gives full play to the advantage of fine removing tower to guarantee the quality of product.
(4) liquefaction unit
For unstripped gas from dewatering unit after filter, expenditure and pressure to 3.0-3.5MPa enters plate through heat source import
Liquefied ammonia heat exchange after wing formula carbon dioxide condenser and throttling is condensed into liquid CO 2, and liquid CO 2 enters titanium dioxide
Carbon surge tank, subsequently into purifier units；
Ammonia after vaporization enters ammonia liquor separator and is separated, and the ammonia isolated enters screw compressor air-breathing,
The liquefied ammonia isolated returns to plate-fin carbon dioxide condenser through liquid back pipe and is recycled；1.1- is forced into through screw compressor
The tube side that the exhaust of 1.5MPa enters rectifying tower reboiler is back to ammonia storage tank after exchanging heat, and the ammonia in ammonia storage tank enters vaporation-type
After condenser is water cooled, it is condensed into liquid and flows into Siphon pot, the liquefied ammonia in Siphon pot is divided into two parts, and a part enters screw
Siphon pot is returned to after the oil cooler endothermic gasification of compressor, remaining part flows back to ammonia storage tank.
The core content of this unit scheme is combined using efficient plate-fin carbon dioxide condenser and ammonia liquor separator
Mode greatly improve heat exchange efficiency under the premise that security is guaranteed.
This programme substitutes shell-and-tube heat exchanger using the higher aluminum plate-fin type carbon dioxide condenser of heat exchange efficiency,
Equipment volume is small, good effect of heat exchange, and heat exchange rate is high.It, can not using heat exchange area, to be operated to the greatest extent using full-liquid type
The part ammoniacal liquor that has avoided enters suction chamber with screw compressor air-breathing and causes liquid hammer, and screw compressor is caused when serious
Damage.So the present invention adds ammonia liquor separator after plate-fin heat exchanger, ammonia liquor separator bottom level is higher than plate-fin
1.5 meters or more at the top of heat exchanger, ammonia liquor separator bottom is equipped with liquid back pipe, is connected with plate-fin heat exchanger for ammonia import and (throttles
After valve), the ammoniacal liquor for being deposited in ammonia liquor separator bottom flows back into plate-fin heat exchanger by the liquid back pipe of bottom at any time, thus thorough
Bottom solves the problems, such as screw machine liquid hammer.
(5) purifier units
Liquid CO 2 from liquefaction unit is divided into two parts, and a part passes through after throttling is decompressed to 2.5-3.0MPa
Feed inlet enters purifying column, is uniformly distributed in corrugated plate regular packing layer, higher with temperature next from tower bottom reboiler tube side
Gas converting heat after, boiling point lower component heat absorption vaporization ascends into the tube side of overhead condenser, after the throttling of shell side
Liquid CO 2 heat exchange, exchanges heat with the liquid CO 2 after the throttling of shell side, and the higher carbon dioxide of boiling point condenses again
For liquid, purification tower bottom is flowed back to；Another part is decompressed to 2.0MPa through throttling, enters purifying column overhead condenser by bottom
It is vaporized after shell side, with the gas converting heat of tube side, by entering recovery unit after the discharge of purifying column overhead condenser top；
The liquid CO 2 for flowing back into purification tower bottom is also classified into two parts, a part of thermal source outlet through heat exchange coil
Into carbon dioxide product surge tank, entering stripping tower by outlet outflow, boiling hot matchmaker is used again as low pressure, through throttling after heat exchange
Stripping tower is entered by top to 2.0MPa, enters liquid CO 2 storage tank, the purified tower lower part of remaining part after secondary stripping
Another outlet enters the tube side of tower bottom reboiler, exchanges heat with the pressurization gas heat exchanger high-temperature exhaust air of shell side, after endothermic gasification on
It rises to enter in the middle part of purifying column and be used as boiling hot source again.
The core content of this unit scheme is high-low pressure stripping and is precisely controlled stripping tower and boils temperature and overhead condenser again
Condensation temperature.
Using tower bottom reboiler, stripping tower, the rectifying column of three tower of overhead condenser unification, occupied area is small, fixed to throw
Money is few.Reboiler, overhead condenser have been all made of the mode of atmospheric carbon dioxide and liquid CO 2 heat exchange, have been not required to additional
Energy consumption.High pressure is boiled temperature again and is precisely controlled by pressurization gas heat exchanger at 25-30 DEG C, and overhead condenser temperature is by adjusting confession
Liquid measure is precisely controlled at -15-25 DEG C.Low pressure is boiled again using the liquid CO 2 after high pressure stripping as heat source, and temperature is controlled 5
DEG C, effect is preferably boiled again to reach, and low-boiling impurity composition (excess of oxygen, nitrogen) vaporization is enriched in tower top, through blow-down pipe
Discharge system；High boiling component (carbon dioxide) condensation liquefaction flows back to tower bottom.
(6) gas recovery unit
The carbon dioxide of purifying column overhead condenser shell side vaporization from purifier units, into liquid CO 2 storage tank
Flashed vapour when throttling and the carbon dioxide of heat absorption vaporization influenced by ambient temperature by pressurization gas heat exchanger cold source import into
Enter tube side, after the carbon-dioxide gas compressor high-temperature exhaust air heat exchange of shell side, outflow from the top into carbon-dioxide gas compressor air-breathing,
It is forced into 3.8MPa through compression, pressurization gas heat exchanger shell pass is discharged by carbon-dioxide gas compressor exhaust outlet, with tube side
After low temperature suction heat exchange, into after the heat exchange of the liquid CO 2 of purifying column tower bottom reboiler shell side and tube side, it is discharged by lower part.
This unit Center for architecture content is to be collected recycling and reusing to the flashed vapour in system, and make full use of dioxy
The heat exchange changed between the suction and discharge of carbon compressor meets process requirements.
A, a shell-and-tube heat exchanger (pressurization gas heat exchanger) is set before carbon-dioxide gas compressor, air-breathing walks tube side,
Shell side is walked in exhaust.In this way, the suction and discharge of compressor mutually carry out heat exchange, that is, suction temperature is improved, thus to compressor
Material requires no longer harsh (suction temperature can only use stainless steel -20, reach 0 or more, ordinary carbon steel), while dropping again
The low delivery temperature of compressor, to reduce the consumption of refrigerating capacity.
B, in addition, air-breathing and exhaust due to being homogenous quantities mutually exchange heat, the temperature-controllable after heat exchange: delivery temperature=
(delivery temperature-suction temperature)/2+3
Suction temperature=(delivery temperature-suction temperature)/2-3
What the delivery temperature after heat exchange met purifier units just boils temperature needs again, and the higher gas of the portion temperature is again
The secondary shell side for being introduced into stripping tower reboiler, the liquid carbon dioxide heat exchange again with tube side.The compressor of shell side after heat exchange
Delivery temperature enters condenser time condensation after being down to room temperature, it is no longer necessary to additional refrigerating capacity；The liquid carbon dioxide of tube side
Enter purifying column after heat absorption vaporization to use as boiling hot source again, and saves the heat needed for the partially liq carbon dioxide vaporizes
Source.
In compressor air suction into bypass is added before heat exchanger, under different environment temperatures, passes through and adjust bypass valve
Open degree adjusts the air inflow of heat exchanger tube pass, to reach the height of adjustment compressor air suction temperature, to adapt in difference
The difference of compressor suction and discharge temperature is required under environment temperature.
Wherein, preferred technical solution is as follows:
Solenoid valve is provided on the heat source import pipeline of the heat exchange coil of rectifying column.
The Liquid level of rectifying column is in 1250-1750mm.
Preheater, ammonia cooler and pressurization gas heat exchanger are shell-and-tube heat exchanger.
The temperature reacted in dealkylation tower is 320-350 DEG C.
Aluminium oxide is loaded in first drying tower, the second drying tower is built-in to fill out efficient molecular sieve, and the first drying tower is provided with two
It is a, it is parallel with one another between two the first drying towers.
Ammonia liquor separator bottom level is higher than at the top of plate-fin carbon dioxide condenser 1.5 meters or more.
There are two screw compressor settings, parallel with one another between two screw compressors.
Compared with prior art, beneficial effects of the present invention are as follows:
1, the present invention provides the device of a set of large-scale production electronic grade high-purity carbon dioxide, the electronic grade high-purities of production
Carbon dioxide, purity can be up to 99.999% or more, and described device is easy to operate, and system runs smoothly.
2, energy-saving effect is significant.Each unit uses mature energy-saving design, takes full advantage of what system itself generated
Waste heat, the energy consumption that entire technique does not externally supply.
3, environmentally friendly.Entire production process is generated without solid waste, dangerous waste, waste water, exhaust gas, is had no effect to environment.
4, resource utilization is high, again without any discharge outlet in addition to a small amount of nitrogen and excess of oxygen discharge, while returning including gas
Unit is received, has been truly realized and has made full use of every bit resource.
5, effects of energy saving and emission reduction is significant, for producing 50000 tons of liquid CO 2s per year, the annual discharge for reducing carbon dioxide
Amount reaches 2419000 cubic metres (4782 tons): 280 vertical/h*24*360=2419000 found * 1.977kg/ and found=4782000kg.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of apparatus of the present invention；
In figure: 1, rectifying column；2, preheater；3, dealkylation tower；4, ammonia cooler；5, the first drying tower；6, the second drying tower；7,
Filter；8, plate-fin carbon dioxide condenser；9, carbon dioxide buffer tank；10, purifying column；11, pressurization gas heat exchanger；
12, carbon-dioxide gas compressor；13, carbon dioxide product surge tank；14, stripping tower；15, liquid CO 2 storage tank；16, ammoniacal liquor
Separator；17, evaporative condenser；18, Siphon pot；19, ammonia storage tank；20, screw compressor；21, pipeline a；22, line b；
23, liquid back pipe；24, pipeline is extracted out；25, cryogenic shield pumps.
Specific embodiment
Below with reference to embodiment, the present invention will be further described, but does not limit the present invention.
Embodiment 1
As shown in Figure 1, device used in the production method includes rectifying column 1, the gaseous phase outlet of rectifying column 1 and pre-
The cold source import of hot device 2 is connected, and the cold source outlet of heat exchanger is connected with the import of dealkylation tower 3, the outlet of dealkylation tower 3 and preheater
2 heat source import is connected；
The thermal source outlet of preheater 2 is connected with the heat source import of ammonia cooler 4, the thermal source outlet of ammonia cooler 4 and the first drying
The import of tower 5 is connected, and the outlet of the first drying tower 5 is connected with the import of the second drying tower 6, the outlet and mistake of the second drying tower 6
7 import of filter is connected；
Load aluminium oxide in first drying tower 5, the second drying tower 6 is built-in to fill out efficient molecular sieve, and the first drying tower 5 is provided with
It is two, parallel with one another between two the first drying towers 5；
The outlet of filter 7 is connected with 8 heat source import of plate-fin carbon dioxide condenser, plate-fin carbon dioxide condenser 8
Thermal source outlet be connected with 9 import of carbon dioxide buffer tank, the cold source of plate-fin carbon dioxide condenser 8 exports ammonia liquor separator
16 import is connected；
The outlet of carbon dioxide buffer tank 9 respectively pass course a connected with route b the cold source of 10 overhead condenser of purifying column into
The feed inlet of mouth and purifying column 10, the cold source import of the cold source outlet and pressurization gas heat exchanger 11 of 10 overhead condenser of purifying column
It is connected, the cold source outlet of pressurization gas heat exchanger 11 is connected with the air entry of carbon-dioxide gas compressor 12, carbon-dioxide gas compressor
12 exhaust outlet is connected with the heat source import of pressurization gas heat exchanger 11, the thermal source outlet and purifying column of pressurization gas heat exchanger 11
The heat source import of the heat exchange coil of 10 lower parts setting is connected, the thermal source outlet of heat exchange coil and carbon dioxide product surge tank 13 into
Mouth is connected,
The outlet of carbon dioxide product surge tank 13 is connected with the heat source import of 14 tower bottom reboiler bottom of stripping tower, stripping tower
The thermal source outlet of 14 tower bottom reboilers is connected with 14 import of stripping tower, the outlet of stripping tower 14 and 15 import of liquid CO 2 storage tank
It is connected, the gas outlet at 14 top of stripping tower is connected with the cold source import of pressurization gas heat exchanger 11, liquid CO 2 storage tank 15
The gas outlet at top is connected with the cold source import of pressurization gas heat exchanger 11；
The gas vent of ammonia liquor separator 16 is connected with the air entry of screw compressor 20, the liquid of ammonia liquor separator 16
Outlet is connected by liquid back pipe 23 with the cold source import of plate-fin carbon dioxide condenser 8, and 16 bottom level of ammonia liquor separator is high
In 8 1.5 meters of top of plate-fin carbon dioxide condenser or more.
There are two the settings of screw compressor 20, parallel with one another between two screw compressors 20.
The exhaust outlet of screw compressor 20 is connected the (heat exchange of rectifying column 1 with the heat source import of the heat exchange coil of rectifying column 1
Be provided on the heat source import pipeline of coil pipe solenoid valve for control boil temperature again), the thermal source outlet and ammonia storage tank of heat exchange coil
19 import is connected, and the outlet of ammonia storage tank 19 is connected with the cold source import of plate-fin carbon dioxide condenser 8,19 top of ammonia storage tank
Gas outlet is connected with the import of evaporative condenser 17, and the outlet of evaporative condenser 17 is connected with the import of Siphon pot 18, rainbow
The outlet at bottom of cucurbitula 18 is connected with the cold source import of 20 oil cooler of screw compressor, 20 oil cooler of screw compressor
Cold source outlet be connected with 18 import of Siphon pot, the centre exit of Siphon pot 18 is connected with the import of ammonia storage tank 19,
The outlet of ammonia storage tank 19 is connected with the cold source import of 1 overhead condenser of rectifying column, 1 overhead condenser of rectifying column it is cold
Source outlet is connected with the import of ammonia liquor separator 16；
Wherein, the intracavitary portion of tower of the rectifying column 1 and purifying column 10 sets gradually overhead condenser, distillation from top to bottom
Tower and reboiler, reboiler, that is, heat exchange coil；1 tower bottom of rectifying column is separately connected tower chamber and tower bottom reboiler by extracting pipeline 24 out
Shell side import extracts setting cryogenic shield on pipeline 24 out and pumps 25；
Preheater 2, ammonia cooler 4 and pressurization gas heat exchanger 11 are shell-and-tube heat exchanger.
The production method concrete operations are:
(1) distillation unit
Unstripped gas is decompressed to 4.2-4.5MPa through throttling and enters rectifying column 1, is uniformly distributed corrugated plating after spray head sprays
In structured packing, after the exhaust heat exchange with the screw compressor 20 in 1 bottom heat exchange coil of rectifying column, the lower liquid of boiling point
Body component (carbon dioxide, hydrogen, oxygen, nitrogen, methane, ethane, propane) endothermic gasification rises to 1 top of rectifying column, into de- hydrocarbon list
Member；
The higher liquid component of boiling point (free state water, high-carbon hydrocarbon) is deposited in 1 tower bottom of rectifying column, and extraction rear portion enters
Return system is vaporized after 20 exhaust gas heat exchanging of screw compressor of 1 reboiler shell side of rectifying column and tube side to be recycled, and is unable to vapour
The high boiling component of change is discharged through the bottom discharge port, and another part is used to adjust 1 liquid level of rectifying column back to rectifying column 1, by liquid
Position control is in 1250-1750mm.
(2) hydrocarbon unit is taken off
Carry out the CO 2 raw material gas at 1 top of autospasy hydrocarbon unit rectifying column after throttling is decompressed to 3.5-3.8MPa, through cold
Source import enters 2 shell side of preheater, and after (200 DEG C or so) of gas heat exchange after the high-temperature oxydation of tube side, temperature rises to 130 DEG C
Left and right enters dealkylation tower 3 again and after the high-temperature gas heat exchange after catalysis oxidation in the coil pipe of bottom by bottom, and temperature reaches 180-
It 200 DEG C, is carried out on the corrugated plate regular packing layer of 3 middle and upper part of dealkylation tower and under the action of excessive oxygen is in metal palladium catalyst
Reaction (temperature of reaction is 320-350 DEG C), combustible component (methane, ethane, the hydro carbons such as propane, alkanes, hydrogen) and oxygen occur
Oxidation reaction generates carbon dioxide and water, and gas enters preheater 2 through heat source import after being discharged by dealkylation tower 3 and preheats after reaction
Unstripped gas is cooled to 150 DEG C or so, then by entering ammonia cooler 4 and low temperature through heat source import after the discharge of 2 thermal source outlet of preheater
Liquefied ammonia heat exchange, the gas after heat exchange enter dewatering unit through thermal source outlet.
(3) dewatering unit
The unstripped gas for carrying out autospasy hydrocarbon unit sequentially enters the first drying tower 5 and the second drying tower 6 is dehydrated, dewatered
Gas enters liquefaction unit (moisture 1ppm or less).
Unstripped gas is after the discharge of the first drying tower 5, moisture content 5-10ppm.
(4) liquefaction unit
Unstripped gas from dewatering unit is after filter 7 (porcelain carving pipe), expenditure and pressure to 3.0-3.5MPa, through heat source into
The liquefied ammonia heat exchange that mouth enters after plate-fin carbon dioxide condenser 8 and throttling is condensed into liquid CO 2, liquid CO 2
Into carbon dioxide buffer tank 9, subsequently into purifier units；
Ammonia after vaporization enters ammonia liquor separator 16 and is separated, and the ammonia isolated enters the suction of screw compressor 20
Gas, the liquefied ammonia isolated return to plate-fin carbon dioxide condenser 8 through liquid back pipe 23 and are recycled；Add through screw compressor 20
Be depressed into 1.1-1.5MPa exhaust enter the tube side heat exchange of 1 reboiler of rectifying column after be back to ammonia storage tank 19, in ammonia storage tank 19
Ammonia enter evaporative condenser 17 it is water cooled after, be condensed into liquid and flow into Siphon pot 18, the liquefied ammonia in Siphon pot 18 is divided into two
Part, a part of (fraction) return to Siphon pot 18, remaining portion after entering the oil cooler endothermic gasification of screw compressor 20
(major part) is divided to flow back to ammonia storage tank 19.
(5) purifier units
Liquid CO 2 from liquefaction unit is divided into two parts, and a part of (accounting for 80%) is decompressed to 2.5- through throttling
Enter purifying column 10 through feed inlet after 3.0MPa, be uniformly distributed in corrugated plate regular packing layer, and from tower bottom reboiler tube side
After the higher gas converting heat of temperature come, the lower component heat absorption vaporization of boiling point ascends into the tube side of overhead condenser, with shell
Liquid CO 2 heat exchange after the throttling of journey, exchanges heat with the liquid CO 2 after the throttling of shell side, the higher dioxy of boiling point
Change carbon and be condensed into liquid again, flows back to 10 bottom of purifying column；Another part (accounting for 20%) is decompressed to 2.0MPa through throttling, by bottom
It is vaporized after into the shell side of 10 overhead condenser of purifying column, with the gas converting heat of tube side, by 10 overhead condenser top of purifying column
Enter recovery unit after discharge；
The liquid CO 2 for flowing back into 10 bottom of purifying column is also classified into two parts, and a part of (major part) is through heat exchange coil
Thermal source outlet enter carbon dioxide product surge tank 13, by outlet outflow enter stripping tower 14 as low pressure again boiling hot matchmaker make
With, it is throttled after heat exchange and stripping tower 14 is entered by top to 2.0MPa, liquid CO 2 storage tank 15 is entered after secondary stripping, it is remaining
The lower another outlet in purified 10 lower part of tower of part (fewer parts) enters the tube side of tower bottom reboiler, changes with the pressurization gas of shell side
Hot 11 high-temperature exhaust air of device exchanges heat, and ascends into after endothermic gasification in the middle part of purifying column 10 and uses as boiling hot source again.
(6) gas recovery unit
The carbon dioxide of 10 overhead condenser shell side of purifying column vaporization from purifier units is stored up into liquid CO 2
Tank 15 throttle when flashed vapour and it is influenced by ambient temperature heat absorption vaporization carbon dioxide by pressurization gas heat exchanger 11 cold source
Import enters tube side, after 12 high-temperature exhaust air of the carbon-dioxide gas compressor heat exchange of shell side, outflows from the top into pressurized carbon dioxide
12 air-breathing of contracting machine is forced into 3.8MPa through compression, is discharged into pressurization gas heat exchanger by 12 exhaust outlet of carbon-dioxide gas compressor
After 11 shell sides, with the low temperature suction heat exchange of tube side, into the liquid CO 2 of 10 tower bottom reboiler shell side and tube side of purifying column
After heat exchange, it is discharged by lower part.
The operational mode of described device:
Distillation unit-takes off hydrocarbon unit-dewatering unit (the first drying tower 5 and the second drying tower 6)-liquefaction unit-purification list
Member-gas recovery unit-finished product storage.
Claims (10)
1. a kind of production method of scale electronic grade high-purity carbon dioxide, it is characterised in that: used device includes rectifying
The gaseous phase outlet of tower (1), rectifying column (1) is connected with the cold source import of preheater (2), cold source outlet and the de- hydrocarbon of heat exchanger (2)
The import of tower (3) is connected, and the outlet of dealkylation tower (3) is connected with the heat source import of preheater (2),
The thermal source outlet of preheater (2) is connected with the heat source import of ammonia cooler (4), the thermal source outlet of ammonia cooler (4) and first dry
The import of dry tower (5) is connected, and the outlet of the first drying tower (5) is connected with the import of the second drying tower (6), the second drying tower (6)
Outlet be connected with filter (7) import,
Filter (7) outlet is connected with plate-fin carbon dioxide condenser (8) heat source import, plate-fin carbon dioxide condenser
(8) thermal source outlet is connected with carbon dioxide buffer tank (9) import, and the cold source of plate-fin carbon dioxide condenser (8) exports ammonia
The import of liquid/gas separator (16) is connected,
Carbon dioxide buffer tank (9) outlet difference pass course a (21) and route b (22) connection purifying column (10) overhead condenser
Cold source import and purifying column (10) feed inlet, purifying column (10) overhead condenser cold source outlet with pressurization gas heat exchanger
(11) cold source import is connected, the air entry phase of the cold source outlet and carbon-dioxide gas compressor (12) of pressurization gas heat exchanger (11)
Even, the exhaust outlet of carbon-dioxide gas compressor (12) is connected with the heat source import of pressurization gas heat exchanger (11), pressurization gas heat exchange
The thermal source outlet of device (11) is connected with the heat source import for the heat exchange coil that purifying column (10) lower part is arranged, and the heat source of heat exchange coil goes out
Mouth is connected with carbon dioxide product surge tank (13) import,
Carbon dioxide product surge tank (13) outlet is connected with the heat source import of stripping tower (14) tower bottom reboiler bottom, stripping tower
(14) thermal source outlet of tower bottom reboiler is connected with stripping tower (14) import, stripping tower (14) outlet and liquid CO 2 storage tank
(15) import is connected, and the gas outlet at the top of stripping tower (14) is connected with the cold source import of pressurization gas heat exchanger (11), liquid two
Gas outlet at the top of carbonoxide storage tank (15) is connected with the cold source import of pressurization gas heat exchanger (11),
The gas vent of ammonia liquor separator (16) is connected with the air entry of screw compressor (20), the liquid of ammonia liquor separator (16)
Body outlet is connected by liquid back pipe (23) with the cold source import of plate-fin carbon dioxide condenser (8),
The exhaust outlet of screw compressor (20) is connected with the heat source import of the heat exchange coil of rectifying column (1), the heat of heat exchange coil
Source outlet is connected with the import of ammonia storage tank (19), the outlet of ammonia storage tank (19) and the cold source of plate-fin carbon dioxide condenser (8)
Import is connected, and gas outlet is connected with the import of evaporative condenser (17) at the top of ammonia storage tank (19), evaporative condenser (17)
Outlet is connected with the import of Siphon pot (18), and the outlet at bottom of Siphon pot (18) is cold with screw compressor (20) oil cooler
Source import is connected, and the cold source outlet of screw compressor (20) oil cooler is connected with Siphon pot (18) import, Siphon pot (18)
Centre exit be connected with the import of ammonia storage tank (19),
The outlet of ammonia storage tank (19) is connected with the cold source import of rectifying column (1) overhead condenser, rectifying column (1) overhead condenser
Cold source outlet is connected with the import of ammonia liquor separator (16)；
Wherein, the intracavitary portion of tower of the rectifying column (1) and purifying column (10) sets gradually overhead condenser, distillation from top to bottom
Tower and reboiler, reboiler, that is, heat exchange coil；Rectifying column (1) tower bottom is separately connected tower chamber and tower bottom again by extracting pipeline (24) out
The import of device shell side is boiled, setting cryogenic shield pumps (25) in extraction pipeline (24)；
The production method the following steps are included:
(1) distillation unit
Unstripped gas is decompressed to 4.2-4.5MPa through throttling and enters rectifying column (1), ripple plate gauge is uniformly distributed after spray head sprays
On whole filler, after the exhaust heat exchange with the screw compressor (20) in the heat exchange coil of rectifying column (1) bottom, boiling point is lower
Liquid component endothermic gasification rises at the top of rectifying column (1), into de- hydrocarbon unit；The higher liquid component of boiling point is deposited in essence
Tower (1) tower bottom is evaporated, extraction rear portion enters rectifying column (1) reboiler shell side and screw compressor (20) exhaust of tube side is changed
It vaporizes return system after heat to be recycled, the high boiling component that cannot be vaporized is discharged through the bottom discharge port, and another part returns to
Rectifying column (1) is for adjusting rectifying column (1) liquid level；
(2) hydrocarbon unit is taken off
The CO 2 raw material gas come at the top of autospasy hydrocarbon unit rectifying column (1) through throttling be decompressed to 3.5-3.8MPa after through cold source into
Mouth enters preheater (2) and is reacted into dealkylation tower (3) with excessive oxygen after the gas converting heat after high-temperature oxydation, reacts
Gas is by entering preheater (2) preheating material gas through heat source import after dealkylation tower (3) discharge afterwards, then by preheater (2) heat source
Enter ammonia cooler (4) through heat source import after outlet discharge and low-temperature liquid ammonia exchanges heat, the gas after heat exchange enters de- through thermal source outlet
Water unit；
(3) dewatering unit
The unstripped gas for carrying out autospasy hydrocarbon unit sequentially enters the first drying tower (5) and the second drying tower (6) is dehydrated, dewatered
Gas enters liquefaction unit；
(4) liquefaction unit
Unstripped gas from dewatering unit is after filter (7), expenditure and pressure to 3.0-3.5MPa, enters plate wing through heat source import
Liquefied ammonia heat exchange after formula carbon dioxide condenser (8) and throttling is condensed into liquid CO 2, and liquid CO 2 enters dioxy
Change carbon surge tank (9), subsequently into purifier units；
Ammonia after vaporization enters ammonia liquor separator (16) and is separated, and the ammonia isolated enters screw compressor (20) suction
Gas, the liquefied ammonia isolated return to plate-fin carbon dioxide condenser (8) through liquid back pipe (23) and are recycled；Through screw compressor
(20) be forced into 1.1-1.5MPa exhaust enter rectifying column (1) reboiler tube side heat exchange after be back to ammonia storage tank (19), store
Ammonia in ammonia device (19) enter evaporative condenser (17) it is water cooled after, be condensed into liquid flow into Siphon pot (18), Siphon pot
(18) liquefied ammonia in is divided into two parts, returns to siphon after a part of oil cooler endothermic gasification for entering screw compressor (20)
Tank (18), remaining part flow back to ammonia storage tank (19)；
(5) purifier units
Liquid CO 2 from liquefaction unit is divided into two parts, and a part is after throttling is decompressed to 2.5-3.0MPa through feeding
Mouth enters purifying column (10), is uniformly distributed in corrugated plate regular packing layer, higher with temperature next from tower bottom reboiler tube side
Gas converting heat after, boiling point lower component heat absorption vaporization ascends into the tube side of overhead condenser, after the throttling of shell side
Liquid CO 2 heat exchange, exchanges heat with the liquid CO 2 after the throttling of shell side, and the higher carbon dioxide of boiling point condenses again
For liquid, purifying column (10) bottom is flowed back to；Another part is decompressed to 2.0MPa through throttling, enters purifying column (10) tower top by bottom
It is vaporized after the shell side of condenser, with the gas converting heat of tube side, by entering recycling after the discharge of purifying column (10) overhead condenser top
Unit；
The liquid CO 2 for flowing back into purifying column (10) bottom is also classified into two parts, a part of thermal source outlet through heat exchange coil
Into carbon dioxide product surge tank (13), entering stripping tower (14) as low pressure by outlet outflow, boiling hot matchmaker is used again, heat exchange
Entered stripping tower (14) to 2.0MPa by top by throttling, enters liquid CO 2 storage tank (15) after secondary stripping, it is remaining
Another outlet in part purified tower (10) lower part enters the tube side of tower bottom reboiler, high with the pressurization gas heat exchanger (11) of shell side
Warm exhaust gas heat exchanging is ascended into after endothermic gasification in the middle part of purifying column (10) and is used as boiling hot source again；
(6) gas recovery unit
The carbon dioxide of purifying column (10) overhead condenser shell side vaporization from purifier units, into liquid CO 2 storage tank
(15) carbon dioxide of flashed vapour and heat absorption vaporization influenced by ambient temperature when throttling is by the cold of pressurization gas heat exchanger (11)
Source import enters tube side, after the carbon-dioxide gas compressor high-temperature exhaust air heat exchange of shell side, outflows from the top into pressurized carbon dioxide
Contracting machine (12) air-breathing is forced into 3.8MPa through compression, is discharged into pressurization gas by carbon-dioxide gas compressor (12) exhaust outlet and is changed
After hot device (11) shell side, with the low temperature suction heat exchange of tube side, into the liquid of purifying column (10) tower bottom reboiler shell side and tube side
After carbon dioxide heat exchange, it is discharged by lower part.
2. the production method of scale electronic grade high-purity carbon dioxide according to claim 1, it is characterised in that: rectifying column
(1) solenoid valve is provided on the heat source import pipeline of heat exchange coil.
3. the production method of scale electronic grade high-purity carbon dioxide according to claim 1, it is characterised in that: rectifying column
(1) Liquid level is in 1250-1750mm.
4. the production method of scale electronic grade high-purity carbon dioxide according to claim 1, it is characterised in that: preheater
(2), ammonia cooler (4) and pressurization gas heat exchanger (11) are shell-and-tube heat exchanger.
5. the production method of scale electronic grade high-purity carbon dioxide according to claim 1, it is characterised in that: dealkylation tower
(3) temperature reacted in is 320-350 DEG C.
6. the production method of scale electronic grade high-purity carbon dioxide according to claim 1, it is characterised in that: first is dry
Aluminium oxide is loaded in dry tower (5), the second drying tower (6) is built-in to fill out efficient molecular sieve, and there are two the first drying tower (5) settings, and two
It is parallel with one another between a first drying tower (5).
7. the production method of scale electronic grade high-purity carbon dioxide according to claim 1, it is characterised in that: ammoniacal liquor point
It is higher than at the top of plate-fin carbon dioxide condenser (8) 1.5 meters or more from device (16) bottom level.
8. the production method of scale electronic grade high-purity carbon dioxide according to claim 1, it is characterised in that: screw
There are two compressor (20) settings, parallel with one another between two screw compressors (20).
9. device used in a kind of any production method of claim 1-8, it is characterised in that: including rectifying column (1),
The gaseous phase outlet of rectifying column (1) is connected with the cold source import of preheater (2), cold source outlet and dealkylation tower (3) of heat exchanger (2)
Import is connected, and the outlet of dealkylation tower (3) is connected with the heat source import of preheater (2),
The thermal source outlet of preheater (2) is connected with the heat source import of ammonia cooler (4), the thermal source outlet of ammonia cooler (4) and first dry
The import of dry tower (5) is connected, and the outlet of the first drying tower (5) is connected with the import of the second drying tower (6), the second drying tower (6)
Outlet be connected with filter (7) import,
Filter (7) outlet is connected with plate-fin carbon dioxide condenser (8) heat source import, plate-fin carbon dioxide condenser
(8) thermal source outlet is connected with carbon dioxide buffer tank (9) import, and the cold source of plate-fin carbon dioxide condenser (8) exports ammonia
The import of liquid/gas separator (16) is connected,
Carbon dioxide buffer tank (9) outlet difference pass course a (21) and route b (22) connection purifying column (10) overhead condenser
Cold source import and purifying column (10) feed inlet, purifying column (10) overhead condenser cold source outlet with pressurization gas heat exchanger
(11) cold source import is connected, the air entry phase of the cold source outlet and carbon-dioxide gas compressor (12) of pressurization gas heat exchanger (11)
Even, the exhaust outlet of carbon-dioxide gas compressor (12) is connected with the heat source import of pressurization gas heat exchanger (11), pressurization gas heat exchange
The thermal source outlet of device (11) is connected with the heat source import for the heat exchange coil that purifying column (10) lower part is arranged, and the heat source of heat exchange coil goes out
Mouth is connected with carbon dioxide product surge tank (13) import,
Carbon dioxide product surge tank (13) outlet is connected with the heat source import of stripping tower (14) tower bottom reboiler bottom, stripping tower
(14) thermal source outlet of tower bottom reboiler is connected with stripping tower (14) import, stripping tower (14) outlet and liquid CO 2 storage tank
(15) import is connected, and the gas outlet at the top of stripping tower (14) is connected with the cold source import of pressurization gas heat exchanger (11), liquid two
Gas outlet at the top of carbonoxide storage tank (15) is connected with the cold source import of pressurization gas heat exchanger (11),
The gas vent of ammonia liquor separator (16) is connected with the air entry of screw compressor (20), the liquid of ammonia liquor separator (16)
Body outlet is connected by liquid back pipe (23) with the cold source import of plate-fin carbon dioxide condenser (8),
The exhaust outlet of screw compressor (20) is connected with the heat source import of the heat exchange coil of rectifying column (1), the heat of heat exchange coil
Source outlet is connected with the import of ammonia storage tank (19), the outlet of ammonia storage tank (19) and the cold source of plate-fin carbon dioxide condenser (8)
Import is connected, and gas outlet is connected with the import of evaporative condenser (17) at the top of ammonia storage tank (19), evaporative condenser (17)
Outlet is connected with the import of Siphon pot (18), and the outlet at bottom of Siphon pot (18) is cold with screw compressor (20) oil cooler
Source import is connected, and the cold source outlet of screw compressor (20) oil cooler is connected with Siphon pot (18) import, Siphon pot (18)
Centre exit be connected with the import of ammonia storage tank (19),
The outlet of ammonia storage tank (19) is connected with the cold source import of rectifying column (1) overhead condenser, rectifying column (1) overhead condenser
Cold source outlet is connected with the import of ammonia liquor separator (16)；
Wherein, the intracavitary portion of tower of the rectifying column (1) and purifying column (10) sets gradually overhead condenser, distillation from top to bottom
Tower and reboiler, reboiler, that is, heat exchange coil；Rectifying column (1) tower bottom is separately connected tower chamber and tower bottom again by extracting pipeline (24) out
The import of device shell side is boiled, setting cryogenic shield pumps (25) in extraction pipeline (24).
10. device according to claim 9, it is characterised in that: load aluminium oxide in the first drying tower (5), second is dry
Tower (6) is built-in to fill out efficient molecular sieve, and there are two the first drying tower (5) settings, parallel with one another between two the first drying towers (5).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910207776.3A CN109721054A (en) | 2019-03-19 | 2019-03-19 | The production method and device of scale electronic grade high-purity carbon dioxide |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201910207776.3A CN109721054A (en) | 2019-03-19 | 2019-03-19 | The production method and device of scale electronic grade high-purity carbon dioxide |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111453747A (en) * | 2020-04-08 | 2020-07-28 | 河北云瑞化工设备有限公司 | Device for preparing battery-grade lithium carbonate from crude lithium carbonate and using method of device |
| CN112357923A (en) * | 2020-11-10 | 2021-02-12 | 杨意斌 | Production process and device of high-purity liquid carbon dioxide |
| EP4390280A1 (en) * | 2022-12-12 | 2024-06-26 | L'air Liquide, Societe Anonyme Pour L'etude Et L'exploitation Des Procedes Georges Claude | Method and apparatus for separating a carbon dioxide-containing gas mixture |
-
2019
- 2019-03-19 CN CN201910207776.3A patent/CN109721054A/en not_active Withdrawn
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111453747A (en) * | 2020-04-08 | 2020-07-28 | 河北云瑞化工设备有限公司 | Device for preparing battery-grade lithium carbonate from crude lithium carbonate and using method of device |
| CN112357923A (en) * | 2020-11-10 | 2021-02-12 | 杨意斌 | Production process and device of high-purity liquid carbon dioxide |
| EP4390280A1 (en) * | 2022-12-12 | 2024-06-26 | L'air Liquide, Societe Anonyme Pour L'etude Et L'exploitation Des Procedes Georges Claude | Method and apparatus for separating a carbon dioxide-containing gas mixture |
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