CN102580342A - Process method for regenerating ionic liquid and separating and recovering absorbents - Google Patents
Process method for regenerating ionic liquid and separating and recovering absorbents Download PDFInfo
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- CN102580342A CN102580342A CN2011100079293A CN201110007929A CN102580342A CN 102580342 A CN102580342 A CN 102580342A CN 2011100079293 A CN2011100079293 A CN 2011100079293A CN 201110007929 A CN201110007929 A CN 201110007929A CN 102580342 A CN102580342 A CN 102580342A
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Abstract
The invention provides a process method for regenerating an ionic liquid and separating recovering absorbents. The method for regenerating an ionic liquid and separating recovering absorbents is implemented by taking steam such as water and ethanol as sweeping gases, adopting different tower types, sweeping and removing absorbent in the ionic liquid at the temperature of 40-200 DEG C and under the pressure of 0.01-2.0MPa, and condensing the swept gases to separate steam from the absorbents. According to the process method, steam is enabled to pass through the ionic liquid through a bubbling or gas-liquid inverse contact method, the mass transfer effect is enhanced by adopting various tower types, and the regeneration of the ionic liquid is realized; the steam is cooled into a liquid by condensing, and the absorbents are kept in a gaseous state, so that the swept absorbents are separated and recovered; and the condensed steam is reheated and applied to sweeping of the ionic liquid. Due to the adoption of the process method provided by the invention, the ionic liquid can be regenerated effectively in a short time, and the reutilization of the ionic liquid and separation and recovery of the absorbents are realized.
Description
Technical field
The present invention relates to the process of ionic liquid regeneration and absorption thing Separation and Recovery.Particularly, the present invention relates to ionic liquid and in regenerator, contact,, realize ionic liquid regeneration to purge the absorption thing in the ionic liquid with steam, and to absorbing the method that thing carries out Separation and Recovery.
Background technology
Ionic liquid is by organic cation and inorganic or organic anion is formed under room temperature to 100 ℃, is the salts substances of liquid condition.It is developed by traditional high-temperature molten salt, but with respect to the conventional ion compound, and ionic liquid is in a liquid state in the very wide temperature range near room temperature.Ionic liquid has a lot of good character: the liquid temperature wide ranges, from being lower than or, having good heat endurance and chemical stability near more than the room temperature to 300 ℃; Almost there is not vapour pressure; Ion liquid Adjustable structure, character is controlled; All show good dissolving ability to much organic with inorganic substances, can dissolve multiple gases.Based on above characteristic, ionic liquid is considered to a kind of environmentally friendly solvent.Many fields such as ionic liquid is widely used in synthesizing at present, separation, electrochemistry, and progressively replace the focus that conventional solvent becomes new industrial circle concern.Particularly in the extract and separate field, ionic liquid is absorbing, is separating SO
2, CO
2Etc. the aspect shown good application prospects.
Though ionic liquid is counted as a kind of green solvent, and absorbing, separating SO
2And CO
2Etc. the aspect shown good effect, but but there is certain degree of difficulty in the Separation and Recovery that absorbs the ion liquid regeneration in back and absorb thing.Traditional method mainly is high temperature and low-pressure distillation method.This method is under heat and low pressure, the absorption thing is evaporated from ionic liquid through the mode of diffusion, thereby reach ion liquid regeneration.This method exists following problem: at first, this method can not remove the absorption thing in the ionic liquid fully, can't obtain highly purified ionic liquid; Secondly, because viscosity of il is big, to absorb the thing diffusion process slower, so the ionic liquid regenerative process needs long time, and regeneration efficiency is low; Once more, because the vacuum when regenerating is depended in ion liquid regeneration to a great extent, and relatively difficulty of the higher vacuum of realization is gone up in industry, need consume lot of energy; At last, after the high-temperature vacuum processing, the absorption thing in the ionic liquid is difficult to be collected and utilize.
Therefore, how to improve ion liquid reproduction speed, reduce the energy consumption of ionic liquid regenerative process, and the absorption thing in the further Separation and Recovery ionic liquid, be ionic liquid is really realized industrial applications aspect gas removal key factor.
Summary of the invention
The object of the invention is exactly the problem that exists in the existing ionic liquid process of regenerating in order to solve, and from the angle of energy-saving and emission-reduction, sustainable development, improves the ionic liquid regeneration effect; Reduce the energy consumption in the regenerative process; And the absorption thing in the Separation and Recovery ionic liquid, realization absorbs the resource of thing, reduces process cost; Reduce environmental pollution, really realize green chemical industry.
The objective of the invention is to adopt following technical scheme to realize.
The invention provides the process of a kind of ionic liquid regeneration and absorption thing Separation and Recovery; This method comprises makes ionic liquid contact in regenerator with steam; Particularly steam passes ionic liquid; Stir, reduce the vapour pressure that the ionic liquid surface absorbs thing through air-flow, raising absorbs the mass transfer of thing in ionic liquid; Strengthen absorption thing diffusion velocity in gas phase through gas flow.Realize the step of ionic liquid regeneration.
The present invention comprises that also the gas that purges out through condensation, is condensed into liquid state with steam, keeps absorbing thing and is gaseous state, thereby will absorb the step of thing Separation and Recovery.
The present invention is reused for the step that ionic liquid purges after also comprising the liquid heat with condensation.
Ionic liquid regeneration that proposes among the present invention and absorption thing process for separating and recovering method comprise the steps:
⑴ make ionic liquid contact in regenerator with steam, to purge out the absorption thing in the ionic liquid;
⑵ make steam liquefaction with the method for the gas after purging among the step ⑴ through condensation, and keep the absorption thing to be gaseous state, thereby Separation and Recovery absorbs thing;
⑶ contact with ionic liquid after the liquid that obtains among the step ⑵ is reheated into steam, to be used to purge ionic liquid.
Steam is selected from one or more in water vapour, alcohol vapour, methanol steam and the ethyl acetate steam among the present invention; Preferably, said steam is water vapour.
Purge the condition that absorbs thing in the ionic liquid among the present invention and be preferably 40 ~ 200 ℃ of temperature, pressure 0.01 ~ 2.0 MPa; More preferably temperature is 80 ~ 150 ℃, pressure 0.05 ~ 0.20 MPa.
The condition of Separation and Recovery absorption thing is preferably 10 ~ 100 ℃ of temperature, pressure 0.01 ~ 2.0 MPa among the present invention; More preferably temperature is 0 ~ 50 ℃, and pressure is 0.05 ~ 0.20 MPa.
Regenerator described in the present invention is bubble tower, spray column, packed tower, plate column or combined regenerator.
Ionic liquid described in the present invention comprises guanidinium ionic liquid, alcamines ionic liquid, glyoxaline ion liquid, ion liquid of quaternaries, season phosphonium salt class ionic liquid, many nitrogen amine ionic liquid, pyridines ionic liquid, thiazoles ionic liquid, triazole ionic liquid, pyrrolin class ionic liquid, Thiazoling type ionic liquid and benzotriazole ionic liquid; Preferably, said ionic liquid is a glyoxaline ion liquid, for example 1-butyl-3-methyl imidazolium tetrafluoroborate, 1-butyl-3-methylimidazole bromine salt, 1-amine propyl group-3-methyl imidazolium tetrafluoroborate; Further preferably, said ionic liquid is guanidinium ionic liquid and many nitrogen amine ionic liquid, for example TMG lactate, triethylene tetramine lactate.
Absorption thing described in the present invention in the ionic liquid comprises sulfur dioxide, carbon dioxide, hydrogen sulfide etc.; The content range of said absorption thing is preferably 0.01 wt.% ~ 50 wt.%, more preferably 1 wt.% ~ 20 wt.%.
The volume flow of ionic liquid described in the present invention is preferably 1:10 ~ 1:10000, more preferably 1:50 ~ 1:5000 with the ratio of vapour volume flow.
Below will and absorb thing process for separating and recovering method and make more detailed description ionic liquid regeneration of the present invention:
The principle of ionic liquid regeneration provided by the invention and absorption thing process for separating and recovering method is: ionic liquid does not have vapour pressure, therefore in purge, does not have loss, and absorbs the high volatility of thing, can be through the method removal that purges.In purge, steam passes ionic liquid, stirs, reduces greatly the vapour pressure that liquid surface absorbs thing through air-flow, improves to absorb the mass transfer velocity of thing in ionic liquid; And, strengthened absorption thing diffusion velocity in gas phase through the diffusion that steam flows and carries solvent.After the condensation of gas that purges out, steam becomes liquid state, still keeps gaseous state and absorb thing, thereby realizes absorbing the Separation and Recovery of thing.
According to an embodiment of the invention, the technological process and the method for operating of ionic liquid regeneration provided by the invention and absorption thing Separation and Recovery are following:
As shown in Figure 1, the ionic liquid that needs are regenerated joins in the ionic liquid storage tank 2, ionic liquid is transported to the top inlet 5 of regenerator 1 with pump; Can be furnished with spray equipment on the regenerator 1; Ionic liquid is disperseed, ionic liquid through packing layer or column plate with remove the absorption thing, the bottom of the ionic liquid arrival regenerator after the purification after steam contacts; Reach can directly ionic liquid being discharged of purification standard, the circulation once more that does not reach standard gets into ionic liquid storage tank 2.Through the steam of pretreatment temperature between 40 ~ 200 ℃; Get in the tower from the air inlet 7 of regenerator 1 lower left; Distribution device is arranged in the tower; Pressure is 0.01 ~ 2.0 (absolute pressure) MPa, and gas passes packing layer or column plate, and the steam after will purging from the gas outlet 8 of regenerator 1 top is discharged.Gas after the discharge gets into condenser 3, through condensation steam wherein is condensed into liquid state, is used for ion liquid purging through reclaiming once more after storage tank 4 is collected, and gaseous state absorption thing is then discharged through exhaust outlet 9 and reclaimed.
In the regeneration of above-mentioned ionic liquid and absorb in the thing process for separating and recovering, the recovery time is depended on the content that absorbs thing in the ionic liquid and type, ionic liquid kind, temperature, pressure, steam and the ratio of ionic liquid volume flow and the factors such as effect of filler.
Compare with conventional ion liquid renovation process, process provided by the invention has the following advantages at least: at first, this method can farthest be removed the absorption thing in the ionic liquid, obtains highly purified ionic liquid; Secondly, can accomplish regeneration at short notice, significantly improve regeneration efficiency; Once more, this method has been avoided using higher vacuum, has solved the difficult problem of commercial Application intermediate ion liquid regeneration, has reduced energy consumption; At last, the present invention can effectively reclaim the absorption thing in the ionic liquid, reduces disposal of pollutants, is expected to realize resource, and the energy and resource have been practiced thrift in the recycle through purging steam simultaneously effectively.
Description of drawings
Fig. 1 is according to the ionic liquid regeneration of an embodiment of the invention and absorbs thing process for separating and recovering flow chart; Wherein, 1. regenerator; 2. ionic liquid storage tank; 3. condenser; 4. recovery storage tank; 5. inlet; 6. liquid outlet; 7. air inlet; 8. gas outlet; 9. exhaust outlet.
The specific embodiment
To combine embodiment that further detailed explanation is done in ionic liquid regeneration provided by the invention and absorption thing process for separating and recovering method below, but therefore not limit the present invention.
The present embodiment explanation uses water vapour to containing SO
21-butyl-3-methyl imidazolium tetrafluoroborate regenerate and SO
2Separation and Recovery adopts packed tower as regenerator, and the purging condition is 110 ℃, 0.10 MPa.
With SO
21-butyl-3-the methyl imidazolium tetrafluoroborate of content 12.0% joins in the ionic liquid storage tank, with storage tank heat to 110 ℃, is transported to ionic liquid in the regenerator through pump, and regenerator is a packed tower, in Raschig ring is housed as filler.The top of regenerator is equipped with liquid distributor, and the bottom is for there being distribution device.Temperature in the tower is controlled to 110 ℃, and it is 1:2000 that the adjustments of gas flow makes ionic liquid volume and water vapour volume ratio, and pressure is 0.10 MPa; Ionic liquid is sprayed from cat head through circulating pump; Steam gets at the bottom of tower simultaneously, and cat head is discharged, and steam and ionic liquid carry out contact mass transfer at filling surface; After purging 0.5 hour through counter current contacting, SO in the ionic liquid
2Content can be reduced to 0.01%, and ionic liquid obtains regeneration.The gas of discharging through condenser, is cooled to 20 ℃, and water vapour is condensed into liquid storage tank, the SO of getting into
2Gas is collected through discharging behind the gas cleaning plant.Water in the storage tank reheats to 110 ℃ and gets back in the regenerator, and ionic liquid is purged.
The present embodiment explanation uses alcohol vapour to containing SO
21-butyl-3-methylimidazole bromine salt regenerate and SO
2Separation and Recovery adopts plate column as regenerator, and the purging condition is 90 ℃ of temperature, pressure 0.10 MPa.
With SO
2The 1-butyl of content 10%-3-methylimidazole bromine salt joins in the ionic liquid storage tank, with storage tank heat to 90 ℃, is transported to ionic liquid in the regenerator through pump, and regenerator is a plate column.Temperature in the tower is controlled to 90 ℃, and it is 1:2500 that the adjustments of gas flow makes ionic liquid volume and alcohol vapour volume ratio, and pressure is 0.10 MPa; Ionic liquid is sprayed from cat head through circulating pump; Gas gets at the bottom of tower simultaneously, and cat head is discharged, and steam and ionic liquid carry out contact mass transfer; After purging 1 hour through counter current contacting, SO in the ionic liquid
2Content can be reduced to 0.03%, and ionic liquid obtains regeneration.The steam of discharging through condenser, is cooled to 10 ℃, and alcohol vapour is condensed into liquid storage tank, the SO of getting into
2Gas is collected through discharging behind the gas cleaning plant.Ethanol in the storage tank reheats to 90 ℃ and gets back in the regenerator, and ionic liquid is purged.
The present embodiment explanation uses water vapour to containing SO
2The TMG lactate regenerate and SO
2Separation and Recovery adopts bubble tower as regenerator, and the purging condition is 120 ℃ of temperature, pressure 0.10 MPa.And contrast with conventional method, demonstrated the advantage of this method.
With SO
2The TMG lactate of content 15.0% joins in the ionic liquid storage tank, with storage tank heat to 120 ℃, is transported to ionic liquid in the regenerator through pump, and regenerator is a bubble tower.Temperature in the tower is controlled to 120 ℃, and it is 1:5000 that the adjustments of gas flow makes ionic liquid volume and water vapour volume ratio, and pressure is 0.10 MPa; Ionic liquid is injected from cat head through circulating pump; Gas gets at the bottom of tower simultaneously, and cat head is discharged, and sweep gas and ionic liquid carry out contact mass transfer; After purging 1 hour through Bubbling method, SO in the ionic liquid
2Content can be reduced to 0.57%, and ionic liquid obtains regeneration.The gas of discharging through condenser, is cooled to 50 ℃, and water vapour is condensed into liquid storage tank, the SO of getting into
2Gas is collected through discharging behind the gas cleaning plant.Water in the storage tank reheats to 120 ℃ and gets back in the regenerator, and ionic liquid is purged.
Adopt conventional method to SO
2The TMG lactate of content 15.0% is regenerated, and operating condition is 120 ℃, vacuum removal, vacuum is 0.09 MPa, remove 6 hours after, SO in the ionic liquid
2After content is 4.3%, 24 hour, SO in the ionic liquid
2Content still is 1.2%.Compare with method among the present invention, this method regeneration efficiency is low excessively.
The present embodiment explanation uses ethyl acetate steam to containing CO
2Tetraethyl amine alanine salt regenerate and Separation and Recovery CO
2, adopt bubble tower as regenerator, the purging condition is 90 ℃, 0.05 MPa.
With CO
2The tetraethyl amine alanine salt of content 2.0% joins in the ionic liquid storage tank, with storage tank heat to 90 ℃, is transported to ionic liquid in the regenerator through pump, and regenerator is a bubble tower.Temperature in the tower is controlled to 90 ℃, and it is that pressure is 0.05 MPa at 1:1500 that the adjustments of gas flow makes ionic liquid volume and ethyl acetate vapour volume ratio; Ionic liquid is injected from cat head through circulating pump; Gas gets at the bottom of tower simultaneously, and cat head is discharged, and ethyl acetate steam and ionic liquid are through the mode contact mass transfer of bubbling; After purging 0.5 hour, CO in the ionic liquid
2Content can be reduced to 0.05%, and ionic liquid obtains regeneration.The gas of discharging through condenser, is cooled to 10 ℃, and ethyl acetate steam is condensed into liquid storage tank, the CO of getting into
2Gas is collected through discharging behind the gas cleaning plant.Ethyl acetate in the storage tank reheats to 90 ℃ and gets back in the regenerator, and ionic liquid is purged.
The present embodiment explanation uses water vapour to containing H
2The triethylene tetramine lactate of S is regenerated and Separation and Recovery H
2S adopts bubble tower as regenerator, and the purging condition is 110 ℃, 0.10 MPa.
With H
2The triethylene tetramine lactate of S content 3.2% joins in the ionic liquid storage tank, with storage tank heat to 110 ℃, is transported to ionic liquid in the regenerator through pump, and regenerator is a bubble tower.Temperature in the tower is controlled to 110 ℃, and it is 1:2000 that the adjustments of gas flow makes ionic liquid volume and water vapour volume ratio, and pressure is 0.10 MPa; Ionic liquid is injected from cat head through circulating pump; Gas gets at the bottom of tower simultaneously, and cat head is discharged, and water vapour and ionic liquid are through the mode contact mass transfer of bubbling; After purging 0.5 hour, H in the ionic liquid
2S content can be reduced to 0.03%, and ionic liquid obtains regeneration.The gas of discharging through condenser, is cooled to 25 ℃, and water vapour is condensed into liquid storage tank, the H of getting into
2S gas is collected through discharging behind the gas cleaning plant.Water in the storage tank reheats to 110 ℃ and gets back in the regenerator, and ionic liquid is purged.
Embodiment 6
The present embodiment explanation uses water vapour to containing CO
2The triethylene tetramine lactate regenerate and Separation and Recovery CO
2, adopt bubble tower as regenerator, the purging condition is 120 ℃, 0.10 MPa.
With CO
2The triethylene tetramine lactate of content 17.6% joins in the ionic liquid storage tank, with storage tank heat to 120 ℃, is transported to ionic liquid in the regenerator through pump, and regenerator is a bubble tower.Temperature in the tower is controlled to 120 ℃, and it is 1:3500 that the adjustments of gas flow makes ionic liquid volume and water vapour volume ratio, and pressure is 0.10 MPa; Ionic liquid is injected from cat head through circulating pump; Gas gets at the bottom of tower simultaneously, and cat head is discharged, and water vapour and ionic liquid are through the mode contact mass transfer of bubbling; After purging 2.5 hours, CO in the ionic liquid
2Content can be reduced to 0.12%, and ionic liquid obtains regeneration.The gas of discharging through condenser, is cooled to 40 ℃, and water vapour is condensed into liquid storage tank, the CO of getting into
2Gas is collected through discharging behind the gas cleaning plant.Water in the storage tank reheats to 120 ℃ and gets back in the regenerator, and ionic liquid is purged.
Claims (10)
1. ionic liquid regeneration and absorb the process of thing Separation and Recovery, this method comprises makes ionic liquid contact in regenerator with steam, to purge the step of absorption thing in the ionic liquid.
2. process according to claim 1 is characterized in that, said method comprises that also the gas that purges out through condensation, is condensed into liquid state with steam, keeps absorbing thing and is gaseous state, thereby will absorb the step of thing Separation and Recovery.
3. process according to claim 1 is characterized in that, said method is reused for the step that ionic liquid purges after also comprising the liquid heat with condensation.
4. process according to claim 1 is characterized in that said method comprises the steps:
⑴ make ionic liquid contact in regenerator with steam, to purge out the absorption thing in the ionic liquid;
⑵ make steam liquefaction with the method for the gas after purging among the step ⑴ through condensation, and keep the absorption thing to be gaseous state, thereby Separation and Recovery absorbs thing;
⑶ contact with ionic liquid after the liquid that obtains among the step ⑵ is reheated into steam, is used to purge ionic liquid once more.
5. process according to claim 4 is characterized in that, purges the condition that absorbs thing in the ionic liquid and is preferably 40 ~ 200 ℃ of temperature, pressure 0.01 ~ 2.0 MPa; More preferably temperature is 80 ~ 150 ℃, pressure 0.05 ~ 0.20 MPa; The condition that Separation and Recovery absorbs thing is preferably 10 ~ 100 ℃ of temperature, pressure 0.01 ~ 2.0 MPa; More preferably temperature is 0 ~ 50 ℃, pressure 0.05 ~ 0.20 MPa.
6. process according to claim 4 is characterized in that, said regenerator is bubble tower, spray column, packed tower, plate column or combined regenerator; Said process for contact of gas-liquid comprises bubbling and gas-liquid counter current contacting.
7. process according to claim 4; It is characterized in that said ionic liquid comprises: guanidinium ionic liquid, alcamines ionic liquid, glyoxaline ion liquid, ion liquid of quaternaries, season phosphonium salt class ionic liquid, many nitrogen amine ionic liquid, pyridines ionic liquid, thiazoles ionic liquid, triazole ionic liquid, pyrrolin class ionic liquid, Thiazoling type ionic liquid and benzotriazole plasma liquid; Preferably, said ionic liquid is a glyoxaline ion liquid, for example 1-butyl-3-methyl imidazolium tetrafluoroborate, 1-butyl-3-methylimidazole bromine salt, 1-amine propyl group-3-methyl imidazolium tetrafluoroborate; Further preferably, said ionic liquid is guanidinium ionic liquid and many nitrogen amine ionic liquid, for example TMG lactate, triethylene tetramine lactate.
8. process according to claim 4 is characterized in that, the absorption thing in the described ionic liquid comprises sulfur dioxide, carbon dioxide, hydrogen sulfide etc.; The content range of said absorption thing is preferably 0.01 wt.% ~ 50 wt.%, more preferably 1 wt.% ~ 20 wt.%.
9. process according to claim 4 is characterized in that, said ionic liquid volume flow is preferably 1:10 ~ 1:10000, more preferably 1:50 ~ 1:5000 with the ratio of the volume flow of steam.
10. method according to claim 4 is characterized in that, said steam is selected from one or more in water vapour, alcohol vapour, methanol steam and the ethyl acetate steam; Preferably, said steam is water vapour.
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| CN110585860A (en) * | 2019-08-22 | 2019-12-20 | 太原师范学院 | Low-energy-consumption regenerated absorbent and method for absorbing sulfur dioxide in flue gas by using same |
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Application publication date: 20120718 |