CN109813055A - NO in a kind of rectifying recovered flue gas2And SO2Method and apparatus - Google Patents
NO in a kind of rectifying recovered flue gas2And SO2Method and apparatus Download PDFInfo
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- CN109813055A CN109813055A CN201910037479.9A CN201910037479A CN109813055A CN 109813055 A CN109813055 A CN 109813055A CN 201910037479 A CN201910037479 A CN 201910037479A CN 109813055 A CN109813055 A CN 109813055A
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Abstract
The present invention principally falls into low temperature chemical industry rectification of gases separation field, and in particular to NO in a kind of rectifying recovered flue gas2And SO2Method and apparatus；The method combination high and low pressure distillation operation method, first rectifying column high-pressure rectification can be reduced because of NO2And SO2It divides lower caused compared with low boiling point, Second distillation column atmospheric distillation guarantee NO2And SO2Lower separating difficulty；Using semicontinuous rectificating method, the liquid holdup of first rectifying column tower reactor enters back into Second distillation column rectifying after reaching 50%-90%, is preferably controlled Second distillation column；The device has anti-corrosion function simultaneously.
Description
Technical field
The present invention principally falls into low temperature chemical industry rectification of gases separation field, and in particular to NO in a kind of rectifying recovered flue gas2
And SO2Method and apparatus.
Background technique
China is coal-fired big country in the world, and coal accounts for 75% or so of China's energy, and fire coal can generate a large amount of NOXWith
SO2.SO at present2Improvement mainly include wet process, semidry method and dry method three categories, also had developed in recent years including electron beam cigarette
Desulfurization technology, corona discharge pulse flue gas desulfurization technique, membrane absorption method, Technology for Microbial Desulfurization etc., but all in test rank
Section.The selective catalytic reduction method (SCR) that gas denitrifying technology is mainly gone into operation at this stage, selective non-catalytic reduction method
(SNCR) and the more mature technique of technologies such as SNCR-SCR combined denitration method, these techniques are in long-term operative practice
It there has been reliable equipment source of supply and field operation experiences.But above-mentioned all processing methods are all based on and will pollute
Object NOXAnd SO2The thinking consumed is converted, rather than carries out Resource recovery.In fact, high-purity SO2And NO2In metallurgy, change
Work, medicine etc. are multi-field to have significant application value, and a large amount of such gases are contained in flue gas, can be used to recycle completely.
Absorption, absorption and membrane separation technique are applied also more in the industry but cannot get high-purity gas, so product
Gas is difficult as high value resource；And rectifying this mature technological essence is exactly to purify again to purify.It grinds both at home and abroad at present
Study carefully cryogenic rectification it is more be space division, CO2Recycling liquefaction, hydro carbons and alkyl compound etc. separation, for sour gas
Rectifying research is less, high less of corrosivity.And this rectifying scheme is applied to fume treatment and recycling, principal component NO2With
SO2Obtained high-purity N O2And SO2It can be applied to other fields, generate very high economic benefit, it is contour to make up steel industry
Energy consumption industry implements a large amount of investments of energy-saving and emission-reduction.
In NOXAnd SO2Removal aspect, most widely used at present is selective catalytic reduction (SCR) and flue gas desulfurization
(FGD) technology, but fund cost and energy requirement are relatively high, and face complicated material processing challenge.White et al.
It proposes a kind of based on nitric acid and vitriol chamber chemical process removal NOX/SOXDistinct methods, using double absorption column respectively from high concentration
CO2Middle removal NOXAnd SOX；Stefano Lange et al. proposes the CO in the double pressure rectificating method removal natural gases of double tower2Group
Point；The XingXing Li et al. people of Xi'an Communications University is natural using the processing gas employing methanation of coke oven synthesis of single column cryogenic rectification
The pure CH4 of air lift, purity is up to 99.87%；DaIiel SalerIo et al. is reduced light by improving double column cryogenic rectifying device
The condenser heat load of matter gas separation ethylene；DanDumitrache et al. is realized low using single column cryogenic rectification
Temperature separation C isotope；J.Rafael Alc á Itara-Avilaa et al. realizes point of propylene propane by single column cryogenic rectification
From.So in terms of cryogenic gas rectifying, currently without NO2And SO2Rectification system；It is existing in terms of flue gas pollutant improvement
Smoke recycling main thought is conversion removal, rather than is recycled, for example SCR denitration is by spraying ammonia for NOXReaction is N2And H20,
It realizes that pollution-freeization is handled, but NO can not be recycledXResource；The calcium method of FGD flue gas desulfurization technique, magnesium processes, sodium method, ammonia process and have
Machine alkaline process is also all to be converted into corresponding sulfate and sulphite by the way that other materials are added, and is solid by gas resource conversion
Resource, but income is lower and cost is very high.
In addition, there is also following technical problems in the prior art: (1) current rectifying column separation gas is more primarily discrete
Common such as air, hydrocarbon gas, natural gas removal sour gas, separated isotopes etc., almost without there is the rectifying column can be with
Handle NO2And SO2This acidic corrosive gas system；(2) current cryogenic rectification or be pure low-pressure distillation such as space division,
It is pure high-pressure rectification such as natural gas removal CO2, it is more demanding for the concentration of component of feed gas, generally require rectifying master
Concentration of component is very high；(3) current hypothermia distillation device is mostly continuous rectification, continuous feed and output.
Summary of the invention
To solve the above problems, the present invention proposes NO in a kind of rectifying recovered flue gas2And SO2Method and apparatus, this method
In conjunction with high and low pressure distillation operation method, first rectifying column high-pressure rectification can be reduced because of NO2And SO2It divides lower caused lower
Boiling point, Second distillation column atmospheric distillation guarantee NO2And SO2Lower separating difficulty；Using semicontinuous rectificating method, the first rectifying
The liquid holdup of tower tower reactor enters back into Second distillation column rectifying after reaching 50%-90%, is preferably controlled Second distillation column；
The device has anti-corrosion function simultaneously.
The present invention is achieved by the following technical solutions:
NO in a kind of rectifying recovered flue gas2And SO2Method, described method includes following steps:
Step 1, high-temperature flue gas is subjected to pressurization cooling operation, the high-temperature flue gas is made to be cooled to 0~20 DEG C；
Step 2, flue gas after cooling in step 1 is entered into first rectifying column and carries out level-one high-pressure rectification, the NO of heavy constituent2
And SO2Enter tower reactor after mixing liquid condensation, light-component gas is distillated from tower top；
The light-component gas includes N2、CO2And NO；
Step 3, Second distillation column, atmospheric distillation point are pumped by metering pump into the mixing liquid of tower reactor in step 2
From NO2And SO2, tower reactor obtains high-purity NO2, tower top obtains high-purity SO2。
Further, when light-component gas described in step 2 is distillated from tower top, before the first rectifying column reaches and stablizes
It directly empties, after the Second distillation column starts rectifying, is collected into together with all discharge gas of the Second distillation column
In air accumulator, so as to multi-cycle separation next time, yield is improved.
Further, the main function of first rectifying column described in step 1 is to realize heavy constituent NO2And SO2Liquefaction and with
Remaining light component N2、O2、CO2, NO etc. separation；
The effect of Second distillation column described in step 3 is by the NO of the first rectifying column tower reactor2And SO2Liquid carries out thorough
Bottom separation, tower reactor NO2Purity up to 80% or more, the SO of tower top2Purity also up to 90% or more, realizes NO2And SO2Mention
Pure recycling.
Further, due to NO in gas source2And SO2Concentration it is lower, divide it is lower cause condensing temperature very low, in order to just
In with other equipment cooperation and Subzero valve, refrigeration equipment be applicable in, first rectifying column selects 1-20bar pressure adjustable
High-pressure rectification (controls pressure by compressor and the counterbalance valve of rectifying column rear end), so that first rectifying column condenser temperature controls
At -80 DEG C~-20 DEG C or so；Second distillation column is in order to realize lower separating difficulty, using atmospheric distillation；To realize double tower
Multiple supply voltage.
Further, the cooling heat exchanger in step 1 mainly plays pre-cooling, and the high-temperature flue gas of compressor out is condensed to
0~20 DEG C, reduce the load of the condenser of the first rectifying column tower top；
The condenser main function of the first rectifying column tower top is the NO in condensed components2And SO2, condensation temperature is -80
DEG C~-20 DEG C, refrigerant temperature still has lower temperature after heat exchange, can be used to prechilled feeds gas completely；Therefore by the first rectifying
Tower condenser refrigerant exit is connected with the heat exchanger refrigerant inlet before first rectifying column, realizes cascade heat exchange, saves cooling capacity and system
Cool equipment.
Another object of the present invention is to provide NO in a kind of rectifying recovered flue gas2And SO2Device, described device includes:
One for being pre-chilled the cooling heat exchanger of high-temperature flue gas；
One is used for the first rectifying column of high-pressure rectification；
One is used for the Second distillation column of atmospheric distillation；
One SO2Fluid reservoir；
The cooling heat exchanger, first rectifying column, Second distillation column and SO2Fluid reservoir is sequentially connected, and the SO2Liquid storage
Tank is connect with the condenser of the Second distillation column.
Further, described device further include:
The tail gas obtained after one tail gas and the Second distillation column processing for obtaining after handling first rectifying column stores
Carry out the air accumulator of multi-cycle separation；
The one gas mixing tank for mixing the gas in the air accumulator with high-temperature flue gas；
One is used for the compressor of compressed gas；
The air accumulator, gas mixing tank and compressor are sequentially connected with, the compressor other end and the cooling heat transferring
Device connection.
Further, described device further includes several needle-valves, air pump, flowmeter, check valve, metering pump, cryotrap
And counterbalance valve；
Several needle-valve setting positions include:
On pipeline between the air accumulator and the gas mixing tank,
On pipeline between the gas mixing tank and the compressor,
On pipeline after the first rectifying column tower reactor,
On the condenser of the Second distillation column,
On pipeline after the Second distillation column tower reactor；
The setting position of several air pumps includes:
On pipeline between the air accumulator and the gas mixing tank；
The setting position of several flowmeters includes:
High-temperature flue gas leads on the pipeline of the gas mixing tank,
On pipeline between the air accumulator and the gas mixing tank；
The setting position of several check valves includes:
High-temperature flue gas leads on the pipeline of the gas mixing tank,
On pipeline between the air accumulator and the gas mixing tank；
The setting position of several metering pumps includes:
On the pipeline that the first rectifying column tower reactor is connect with the Second distillation column,
On the pipeline of the Second distillation column tower reactor discharge liquid,
The SO2Storage tank is discharged on the pipeline of liquid；
The setting position of several cryotraps includes:
Between metering pump in the first rectifying column tower reactor and same pipeline,
Between metering pump in the Second distillation column tower reactor and same pipeline；
The setting position of several counterbalance valves includes:
On the pipeline of the first rectifying column tower top discharge light-component gas,
SO is discharged in the Second distillation column tower top2Pipeline on.
Further, the first rectifying column in described device, Second distillation column and all attachment components all have
Anti-corrosion ability, tower body and pipeline use 316L steel, fiber glass epoxy, organic toughened glass, epoxy phenol aldehyde glass steel, coal-tar epoxy
Glass reinforced plastics or other non-corrosive metal (NCM)s such as glass reinforced plastic, epoxy furans glass reinforced plastic and phenolic aldehyde furans glass reinforced plastic, seal assembly use fluorine-containing
The antiseptic rubbers product such as rubber or Oppanol.
Further, described device aims at the gas circulation distillation system of lab design, can more safely ensure reality
It tests personnel safety and saves gas waste；In the CO that first rectifying column stabilization sub stage, upper tower distillate2Etc. light components direct emission
(pollution-free and cheap)；Start to carry out first rectifying column and Second distillation column two-tower rectification after first rectifying column is stablized
Afterwards, first rectifying column tower top distillate gas and Second distillation column overhead distillate liquid and are mixed by heating evaporation, pass through
Heat tracing pipeline returns to anti-corrosion air accumulator, and after two-tower rectification all tends towards stability, feed gas is changed to air accumulator from source gas supply
With the circulation for realizing whole device (the mixed gas gas supply of air accumulator and high-temperature flue gas, including air accumulator also may be implemented in gas supply
Mixing with source one-component is to realize the constant of pan feeding concentration of component).
Further, described device reserves gas inlet passages, and industrial smoke (such as sintering device flue gas) is passing through depth
This device can be passed directly into after water removal and dedusting, collection and absorption and vacuum desorption to be handled；Including but not limited to flue gas,
It is rich in NO2And SO2But it is not aqueous, be free of and NO2And SO2The mixed gas of other sour gas similar in boiling point all can be used as
The gas source of this device.
Further, gas is passed through in described device, initially enters gas mixing tank buffering and mixing (flue gas in industry
Concentration is fluctuation, and gas mixing tank can guarantee the homogeneity on the time dimension of gas concentration as far as possible), then according to setting
Pressure enters compressor compresses to specified pressure, then enters the condensation that condenser carries out next step；The compressor is using resistance to
Corrode sealing element, compression ratio 6:1 carries cooling and decompressor, and with driving gas source, maximum moulding pressure is 2.0MPa.
Further, the compressor is corrosion resistant compressor.
Further, the cooling heat exchanger uses shell and tube, and anti-corrosion material is made, and realizes the condensation of small amount of liquids,
Maximum effect realizes the pre-cooling before entering the first rectifying column, reduces the pressure of the condenser of the first rectifying column tower top.
Further, the first rectifying column and the Second distillation column are packed tower, and filler selects θ ring filler；
The first rectifying column operating pressure is controlled by inlet air compressor and tower top counterbalance valve, passes through overhead condenser reality
Existing portion gas (NO2And SO2) condensation liquefaction reflux, reflux ratio controls by Electrical heads, can be adjusted between 1-99；
Tower reactor temperature controllable evaporates kettle liquid, counter current contacting is carried out in rectifying column with top reflux liquid, in filler
Surface carries out liquid phase border heat and mass, so that volatile components CO in liquid phase2Into volatile component NO difficult in gas phase, gas phase2With
SO2It is transferred to liquid phase, to obtain SO in tower reactor2/NO2Mixing liquid, tower top obtain CO2/NO/N2/O2Deng difficult liquefied gas.
Further, described device uses semicontinuous rectifying pattern, has certain SO to first rectifying column tower reactor2/NO2Mixing
After liquid liquid holdup, the connection valve of first rectifying column and Second distillation column is opened, which is carried out by cryotrap
It is cooling, it is pumped into rectifying column two using metering pump, starts Second distillation column distillation process.Pass through Second distillation column tower top counterbalance valve
Second distillation column operating pressure is controlled, overhead condenser controls tower top temperature, and Electrical heads control reflux ratio 1-99 is adjustable, realizes
SO2And NO2Gas-liquid mass transfer heat exchange, to separate SO2And NO2, high-purity N O is respectively obtained in tower reactor and tower top2And SO2。
Further, to save experimental cost, reducing gas usage, the present apparatus recycles all gas；It will
It is passed through in air accumulator in the product that tower Second distillation column top and tower reactor and tower first rectifying column top obtain, and passes through gas cylinder tonifying Qi
Concentration mixed gas needed for obtaining；In the circulatory system, the pipeline flowed out to tower Second distillation column top and tower reactor liquid carries out companion
Heat makes all products gasify, the recycling for product of being more convenient for；
Further, since including SO to the separation of multi-pollutant in this recycling unit2、NO2Equal corrosive gas, thus it is whole
A distillation system is all made of equipment and device with Anticorrosive Character, and rectifying column is all made of anti-corrosion stainless steel material, seal assembly
Using rubber material such as polytetrafluoroethylene (PTFE).
The present invention has following advantageous effects:
(1) present invention is directed to NO2And SO2Sour corrosion system carries out separation recycling；Meanwhile the device of the invention is main
For handling the gas after flue gas pretreatment (water removal+absorption concentrate), and the combination of adsorption technology can be the short route the case where
Flue gas pollutant and NO are effectively administered in lower realization2And SO2Recycling combination.
(2) the device of the invention requires lower, concentration model to feed gas concentration using the double pressure two-tower rectification modes of height
It is very wide to enclose applicability.
(3) the device of the invention in order to realize the recycling of low concentration feeding gas and guarantee Second distillation column liquid into
The ease for operation of material, the semicontinuous distillation operation of ad hoc meter, increases valve between first rectifying column and Second distillation column, to guarantee the
The enough liquid of one tower bottom of rectifying tower is conveyed to Second distillation column charging.
(4) distillation technology has been applied in the purification recycling of acid strong corrosive gas by method of the invention, is widened
The application range of distillation technology.
(5) gas is better achieved in conjunction with double tower high-low pressure rectifying for the inlet gas of low concentration in method of the invention
The recycling of body.
(6) the semicontinuous distillation operation mode of method of the invention, so that the tower diameter of Second distillation column is no longer by inlet flow rate
The limitation of fluctuation can keep good liquid flooding rate with the unrestricted choice Second distillation column rectifying time, realize that preferably rectifying is imitated
Fruit.
(7) in the device of the invention air accumulator application, collect rectifying after gas mixing, accomplished toxic gas without row
It puts, not only ensure that safety, but also save experiment gas flow, also accomplished free from environmental pollution.
(8) method of the invention utilizes the N in multi-pollutant2/CO2/SO2/NO2Equal gases relative volatility is different and easy
In liquefaction the characteristics of, by flue gas multiple pollutant gas by pretreatment after be passed through recycling unit, pass through rectifying in control device
The conditions such as pressure tower, temperature, the number of plates (packed height), feed entrance point realize the separation to multi-pollutant gas and SO2/
NO2Purifying.
(9) the device of the invention both can carry out the test of small flow in laboratory, in industrial smoke after can also amplifying
It is used in processing.
Detailed description of the invention
Fig. 1 is NO in rectifying recovered flue gas a kind of in the embodiment of the present invention2And SO2Apparatus structure schematic diagram.
The method flow schematic diagram that Fig. 2 is NO2 and SO2 in a kind of rectifying recovered flue gas in the embodiment of the present invention.
Description of symbols: 1- air accumulator；2- needle-valve；3- air pump；4- flowmeter；5- check valve；6- gas mixing tank；7-
Compressor；8- cooling heat exchanger；9- first rectifying column condenser；10- visor；11- first rectifying column；12- first rectifying column tower
Kettle；13- cryotrap；14- metering pump；15- Second distillation column；16- Second distillation column tower reactor；17- Second distillation column condenser；
18-SO2Fluid reservoir；19- counterbalance valve.
Specific embodiment
In order to make the objectives, technical solutions, and advantages of the present invention clearer, with reference to the accompanying drawings and embodiments, right
The present invention is explained in further detail.It should be appreciated that specific embodiment described herein is used only for explaining the present invention, and
It is not used in the restriction present invention.
On the contrary, the present invention covers any substitution done on the essence and scope of the present invention being defined by the claims, repairs
Change, equivalent method and scheme.Further, in order to make the public have a better understanding the present invention, below to of the invention thin
In section description, exhaustive presentation data details therein.The description of part without these details for a person skilled in the art
The present invention can also be understood completely.
Embodiment 1
The present embodiment proposes NO in a kind of rectifying recovered flue gas2And SO2Device, as shown in Figure 1, described device includes:
One for being pre-chilled the cooling heat exchanger of high-temperature flue gas；
One is used for the first rectifying column of high-pressure rectification；
One is used for the Second distillation column of atmospheric distillation；
One SO2Fluid reservoir；
The cooling heat exchanger, first rectifying column, Second distillation column and SO2Fluid reservoir is sequentially connected, and the SO2Liquid storage
Tank is connect with the condenser of the Second distillation column.
Described device further include:
The tail gas obtained after one tail gas and the Second distillation column processing for obtaining after handling first rectifying column stores
Carry out the air accumulator of multi-cycle separation；
The one gas mixing tank for mixing the gas in the air accumulator with high-temperature flue gas；
One is used for the compressor of compressed gas；
The air accumulator, gas mixing tank and compressor are sequentially connected with, the compressor other end and the cooling heat transferring
Device connection.
Described device further includes several needle-valves, air pump, flowmeter, check valve, metering pump, cryotrap and counterbalance valve；
Several needle-valve setting positions include:
On pipeline between the air accumulator and the gas mixing tank,
On pipeline between the gas mixing tank and the compressor,
On pipeline after the first rectifying column tower reactor,
On the condenser of the Second distillation column,
On pipeline after the Second distillation column tower reactor；
The setting position of several air pumps includes:
On pipeline between the air accumulator and the gas mixing tank；
The setting position of several flowmeters includes:
High-temperature flue gas leads on the pipeline of the gas mixing tank,
On pipeline between the air accumulator and the gas mixing tank；
The setting position of several check valves includes:
High-temperature flue gas leads on the pipeline of the gas mixing tank,
On pipeline between the air accumulator and the gas mixing tank；
The setting position of several metering pumps includes:
On the pipeline that the first rectifying column tower reactor is connect with the Second distillation column,
On the pipeline of the Second distillation column tower reactor discharge liquid,
The SO2Storage tank is discharged on the pipeline of liquid；
The setting position of several cryotraps includes:
Between metering pump in the first rectifying column tower reactor and same pipeline,
Between metering pump in the Second distillation column tower reactor and same pipeline；
The setting position of several counterbalance valves includes:
On the pipeline of the first rectifying column tower top discharge light-component gas,
SO is discharged in the Second distillation column tower top2Pipeline on.
The first rectifying column and Second distillation column are rectifying column；
The rectifying column and all attachment components all have anti-corrosion ability, and tower body and pipeline use 316L steel or epoxy
Glass reinforced plastic, organic toughened glass, epoxy phenol aldehyde glass steel, coal-tar epoxy glass reinforced plastic, epoxy furans glass reinforced plastic and phenolic aldehyde furans glass
The glass reinforced plastics such as glass steel or other non-corrosive metal (NCM)s, seal assembly use the antiseptic rubbers products such as fluorine-containing rubber or Oppanol.
Described device aims at the gas circulation distillation system of lab design, can more safely ensure experimenter's safety
It is wasted with gas is saved；In the CO that first rectifying column stabilization sub stage, upper tower distillate2Etc. light components direct emission (it is pollution-free and
It is cheap)；After starting to carry out first rectifying column and Second distillation column two-tower rectification after first rectifying column is stablized, the first rectifying
Column overhead distillate gas and Second distillation column overhead distillate liquid and are mixed by heating evaporation, return by heat tracing pipeline
To anti-corrosion air accumulator, after two-tower rectification all tends towards stability, feed gas from source gas supply be changed to air accumulator gas supply it is whole to realize
(mixed gas that air accumulator and high-temperature flue gas also may be implemented supplies the circulation of a device, including air accumulator and single group of source
The mixing divided is to realize the constant of pan feeding concentration of component).
Described device reserves gas inlet passages, and industrial smoke (such as sintering device flue gas) is being removed water and removed by depth
This device can be passed directly into after dirt, collection and absorption and vacuum desorption to be handled；Including but not limited to flue gas, it is other to be rich in
NO2And SO2But it is not aqueous, be free of and NO2And SO2The mixed gas of other sour gas similar in boiling point all can be used as this device
Gas source.
Gas is passed through in described device, and initially entering gas mixing tank buffering and mixing, (concentration of flue gas is wave in industry
Dynamic, gas mixing tank can guarantee the homogeneity on the time dimension of gas concentration as far as possible), then entered according to setting pressure
Compressor compresses then enter the condensation that condenser carries out next step to specified pressure；The compressor uses corrosion-resistant sealing
Part, compression ratio 6:1 carry cooling and decompressor, and with driving gas source, maximum moulding pressure is 2.0MPa.
The compressor is corrosion resistant compressor.
The cooling heat exchanger uses shell and tube, and anti-corrosion material is made, and realizes the condensation of small amount of liquids, and maximum effect is real
Now enter the pre-cooling before the first rectifying column, reduces the pressure of the condenser of the first rectifying column tower top.
The first rectifying column and the Second distillation column are packed tower, and filler selects θ ring filler；
The first rectifying column operating pressure is controlled by inlet air compressor and tower top counterbalance valve, passes through overhead condenser reality
Existing portion gas (NO2And SO2) condensation liquefaction reflux, reflux ratio controls by Electrical heads, can be adjusted between 1-99；
Tower reactor temperature controllable evaporates kettle liquid, counter current contacting is carried out in rectifying column with top reflux liquid, in filler
Surface carries out liquid phase border heat and mass, so that volatile components CO in liquid phase2Into volatile component NO difficult in gas phase, gas phase2With
SO2It is transferred to liquid phase, to obtain SO in tower reactor2/NO2Mixing liquid, tower top obtain CO2/NO/N2/O2Deng difficult liquefied gas.
Described device uses semicontinuous rectifying pattern, has certain SO to first rectifying column tower reactor2/NO2Mixing liquid liquid holdup
Afterwards, the connection valve for opening first rectifying column and Second distillation column, which is cooled down by cryotrap, uses meter
Amount is pumped into rectifying column two, starts Second distillation column distillation process.Pass through the second essence of Second distillation column tower top counterbalance valve control
Tower operating pressure is evaporated, overhead condenser controls tower top temperature, and Electrical heads control reflux ratio 1-99 is adjustable, realizes SO2And NO2Gas
Liquid mass transfer heat exchange, to separate SO2And NO2, high-purity N O is respectively obtained in tower reactor and tower top2And SO2。
To save experimental cost, reducing gas usage, the present apparatus recycles all gas；It will be in the second essence of tower
It evaporates tower top and tower reactor and product that tower first rectifying column top obtains is passed through in air accumulator, and is dense needed for being obtained by gas cylinder tonifying Qi
Spend mixed gas；In the circulatory system, the pipeline flowed out to tower Second distillation column top and tower reactor liquid carries out heat tracing, makes all productions
Product gasification, the recycling for product of being more convenient for；
Further, since including SO to the separation of multi-pollutant in this recycling unit2、NO2Equal corrosive gas, thus it is whole
A distillation system is all made of equipment and device with Anticorrosive Character, and rectifying column is all made of anti-corrosion stainless steel material, seal assembly
Using rubber material such as polytetrafluoroethylene (PTFE).
The present embodiment is tested using described device, tests specific data are as follows: high-temperature gas mixture (simulated flue gas) entrance
Flow is 15L/miI, and gaseous mixture group is divided into NO2/SO2/CO2=5.0%/14.2%/80.8%, compressor delivery pressure
15bar, cooling heat exchanger condensation temperature are set as 0 DEG C；First rectifying column pressure 15bar, reflux ratio 0.56, theoretical cam curve
20, feedboard number 9；Second distillation column pressure 1.0bar, reflux ratio 0.46, theoretical cam curve 27, feedboard number 17.
By stable state rectifying, first rectifying column tower top CO2Purity is 0.999, Second distillation column tower top SO2Purity be
0.98 (volume fraction), Second distillation column tower reactor NO2Purity be 0.99 (volume fraction).
Embodiment 2
NO in a kind of rectifying recovered flue gas that the present embodiment proposes2And SO2Device it is substantially the same manner as Example 1, it is only different
:
Test specific data are as follows: high-temperature gas mixture (simulated flue gas) inlet flow rate 5L/miI, gaseous mixture group are divided into NO2/SO2/
CO2=21.6%/61.1%/17.3%, compressor delivery pressure 1.5bar, 0 DEG C of condenser condensation temperature；First rectifying column pressure
Power 1.1bar, reflux ratio 1.28, theoretical cam curve 27, feed tray number 13；Second distillation column pressure 1.05bar, reflux ratio
3.78, theoretical cam curve 7, feedboard number 3.
By stable state rectifying, NO2And SO2Purity be respectively 0.999 (volume fraction) and 0.99 (volume fraction).
Embodiment 3
The present embodiment proposes NO in a kind of rectifying recovered flue gas2And SO2Method, as shown in Fig. 2, the method is using real
Device described in example 1 is applied, described method includes following steps:
Step 1, high-temperature flue gas is subjected to pressurization cooling operation, the high-temperature flue gas is made to be cooled to 0~20 DEG C；
Step 2, flue gas after cooling in step 1 is entered into first rectifying column and carries out level-one high-pressure rectification, the NO of heavy constituent2
And SO2Enter tower reactor after mixing liquid condensation, light-component gas is distillated from tower top；
The light-component gas includes N2、CO2And NO；
Step 3, Second distillation column, atmospheric distillation point are pumped by metering pump into the mixing liquid of tower reactor in step 2
From NO2And SO2, tower reactor obtains high-purity NO2, tower top obtains high-purity SO2。
When light-component gas described in step 2 is distillated from tower top, the directly emptying before the first rectifying column reaches and stablizes,
After the Second distillation column starts rectifying, it is collected into air accumulator together with all discharge gas of the Second distillation column,
So as to multi-cycle separation next time, yield is improved.
The main function of first rectifying column described in step 1 is to realize heavy constituent NO2And SO2Liquefaction and with remaining light group
Divide N2、O2、CO2, NO etc. separation；
The effect of Second distillation column described in step 3 is by the NO of the first rectifying column tower reactor2And SO2Liquid carries out thorough
Bottom separation, tower reactor NO2Purity up to 80% or more, the SO of tower top2Purity also up to 90% or more, realizes NO2And SO2Mention
Pure recycling.
Due to NO in gas source2And SO2Concentration it is lower, divide it is lower cause condensing temperature very low, for the ease of being set with other
Applicable, the high-pressure rectification of first rectifying column selection 1-20bar pressure adjustable of standby cooperation and Subzero valve, refrigeration equipment
(pressure is controlled by compressor and the counterbalance valve of rectifying column rear end), so that condenser temperature control is at -80 DEG C~-20 DEG C or so；
Second distillation column is in order to realize lower separating difficulty, using atmospheric distillation；To realize the multiple supply voltage of double tower.
Cooling heat exchanger in step 1 mainly plays pre-cooling, and the high-temperature flue gas of compressor out is condensed to 0~20 DEG C,
Reduce the load of the condenser of the first rectifying column tower top；
The condenser main function of the first rectifying column tower top is the NO in condensed components2And SO2, condensation temperature is -80
DEG C~-20 DEG C, refrigerant temperature still has lower temperature after heat exchange, can be used to prechilled feeds gas completely；Therefore by the first rectifying
Tower condenser refrigerant exit is connected with the heat exchanger refrigerant inlet before first rectifying column, realizes cascade heat exchange, saves cooling capacity and system
Cool equipment.
Claims (10)
1. NO in a kind of rectifying recovered flue gas2And SO2Method, which is characterized in that described method includes following steps:
Step 1, high-temperature flue gas is subjected to pressurization cooling operation, keeps the high-temperature flue gas cooling；
Step 2, flue gas after cooling in step 1 is entered into first rectifying column and carries out level-one high-pressure rectification, the NO of heavy constituent2And SO2
Enter tower reactor after mixing liquid condensation, light-component gas is distillated from tower top；
Step 3, Second distillation column is pumped by metering pump into the mixing liquid of tower reactor in step 2, atmospheric distillation separates NO2
And SO2, tower reactor obtains high-purity NO2, tower top obtains high-purity SO2。
2. NO in a kind of rectifying recovered flue gas according to claim 12And SO2Method, which is characterized in that institute in step 2
When stating light-component gas and being distillated from tower top, the directly emptying before the first rectifying column reaches and stablizes, when the Second distillation column
After starting rectifying, it is collected into air accumulator together with all discharge gas of the Second distillation column, so as to circulation next time
Separation improves yield.
3. NO in a kind of rectifying recovered flue gas according to claim 12And SO2Method, which is characterized in that institute in step 3
Second distillation column is stated by the NO of the first rectifying column tower reactor2And SO2Liquid is completely separated, tower reactor NO2Purity it is reachable
80% or more, the SO of tower top2Purity also up to 90% or more, realizes NO2And SO2Purification recycling.
4. NO in a kind of rectifying recovered flue gas according to claim 12And SO2Method, which is characterized in that described first
Rectifying column select 1-20bar pressure adjustable high-pressure rectification so that the first rectifying column tower top condenser temperature control-
80 DEG C~-20 DEG C；
The Second distillation column uses atmospheric distillation；Realize the multiple supply voltage of double tower.
5. NO in a kind of rectifying recovered flue gas according to claim 12And SO2Method, which is characterized in that in step 1
High-temperature flue gas is condensed to 0~20 DEG C by cooling heat exchanger, reduces the load of the condenser of the first rectifying column tower top.
6. NO in a kind of any one according to claim 1~5 rectifying recovered flue gas2And SO2Method formed device,
It is characterized in that, described device includes:
One for being pre-chilled the cooling heat exchanger of high-temperature flue gas；
One is used for the first rectifying column of high-pressure rectification；
One is used for the Second distillation column of atmospheric distillation；
One SO2Fluid reservoir；
The cooling heat exchanger, first rectifying column, Second distillation column and SO2Fluid reservoir is sequentially connected, and the SO2Fluid reservoir with
The condenser of the Second distillation column connects.
7. device according to claim 6, which is characterized in that by the condenser refrigerant exit of the first rectifying column tower top
It is connected with the cooling heat exchanger refrigerant inlet, realizes cascade heat exchange, save cooling capacity and refrigeration equipment.
8. device according to claim 6, which is characterized in that described device further include:
The tail gas obtained after one tail gas and the Second distillation column processing for obtaining after handling first rectifying column, which stores, to follow
The air accumulator of ring separation；
The one gas mixing tank for mixing the gas in the air accumulator with high-temperature flue gas；
One is used for the compressor of compressed gas；
The air accumulator, gas mixing tank and compressor are sequentially connected with, and the compressor other end and the cooling heat exchanger connect
It connects.
9. device according to claim 6, which is characterized in that the first rectifying column, the second rectifying in described device
Tower and all attachment components all have an anti-corrosion ability, tower body and pipeline using 316L steel, fiber glass epoxy, organic toughened glass,
Epoxy phenol aldehyde glass steel, coal-tar epoxy glass reinforced plastic, epoxy furans glass reinforced plastic, phenolic aldehyde furans glass reinforced plastic or other non-corrosive metal (NCM)s,
Seal assembly uses antiseptic rubber product.
10. device according to claim 6, which is characterized in that the first rectifying column and the Second distillation column are
Packed tower, filler select θ ring filler.
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| CN112797733A (en) * | 2020-12-20 | 2021-05-14 | 宋晅任 | Waste gas recycling treatment method |
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| CN103920365A (en) * | 2014-04-21 | 2014-07-16 | 广西大学 | Method for recycling nitrogen gas and sulfur dioxide from calcining iron pyrite burner gas through variable-voltage variable-frequency adsorption |
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| CN103920365A (en) * | 2014-04-21 | 2014-07-16 | 广西大学 | Method for recycling nitrogen gas and sulfur dioxide from calcining iron pyrite burner gas through variable-voltage variable-frequency adsorption |
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