CN114870570B - Liquid-solid phase-splitting absorbent for separating carbon dioxide - Google Patents
Liquid-solid phase-splitting absorbent for separating carbon dioxide Download PDFInfo
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- CN114870570B CN114870570B CN202210608707.5A CN202210608707A CN114870570B CN 114870570 B CN114870570 B CN 114870570B CN 202210608707 A CN202210608707 A CN 202210608707A CN 114870570 B CN114870570 B CN 114870570B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/14—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by absorption
- B01D53/1456—Removing acid components
- B01D53/1475—Removing carbon dioxide
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/14—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by absorption
- B01D53/1493—Selection of liquid materials for use as absorbents
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2252/00—Absorbents, i.e. solvents and liquid materials for gas absorption
- B01D2252/50—Combinations of absorbents
- B01D2252/504—Mixtures of two or more absorbents
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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
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/20—Air quality improvement or preservation, e.g. vehicle emission control or emission reduction by using catalytic converters
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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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- General Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Gas Separation By Absorption (AREA)
Abstract
The invention relates to a method for CO 2 The separated liquid-solid phase-splitting absorbent takes N-methyldiethanolamine as a main body and comprises an activating agent piperazine, an organic solvent and water, wherein the mass percentage of the N-methyldiethanolamine is 20-40%; 3-15% of piperazine as an activator; 30-60% of organic solvent and 0-40% of water; the liquid-solid phase-splitting absorbent absorbs CO 2 The gas source is a uniform liquid phase before absorbing CO 2 Spontaneously forming liquid-solid two phases after gas source, CO 2 Concentrating in solid phase, separating to obtain solid phase, desorbing only the solid phase, and recycling the absorbent obtained by desorption. Only the solid needs to be heated in the desorption process, no sensible heat of temperature rise and no latent heat of water evaporation are generated, and CO is further reduced 2 And (5) energy consumption is relieved.
Description
Technical Field
The invention belongs to the technical field of gas separation, and in particular relates to a method for separating CO 2 A separated liquid-solid phase absorbent.
Background
At present, the person skilled in the art keeps on developing novel efficient absorbents in the hope of reducing CO by chemical absorption 2 And (5) collecting energy consumption. A new class of absorbents, phase change absorbents, are proposed. Phase change absorbent for absorbing CO 2 Homogeneous phase of the front, absorb CO 2 After two phases are formed, CO is obtained 2 CO with extremely high loading 2 Enrichment phase, CO only 2 The enriched phase enters the desorption unit, so that the amount entering the desorption unit is reduced, and the energy consumption in the desorption process is reduced.
Chinese patent application 1MDEA composite absorbent for separating acid gas and separation method (application number 201610035154.3, publication date 2016, 5 and 4), chinese patent application "liquid-liquid phase absorbent for capturing carbon dioxide and application" (application number 201910378327.5, publication date 2019, 7 and 26), and Chinese patent application "reaction phase change CO" 2 The absorbent and the preparation method thereof (application number 201910771297.4, 9/22/2020) and Chinese patent application (application number 201911218162.1, 18/2020) both propose a phase-change absorbent for capturing carbon dioxide and a phase-change absorbent for capturing carbon dioxide, which absorb CO 2 After forming liquid-liquid phase separation, enriching CO 2 Is passed to a desorption unit. The energy in the desorption process is not fully used for CO 2 Desorption, and also a portion for solution heating and solvent evaporation.
To further reduce CO 2 Phase change absorbers that capture energy consumption, a class of liquid-solid phases, are developed by those skilled in the art. The phase change absorbent absorbs CO 2 After forming liquid-solid phase, enriching CO 2 Is fed into a desorption unit, and the energy of desorption is fully used for CO 2 And (5) desorption. Chinese patent application "system and method for capturing carbon dioxide" (application No. 201310046925.5, publication No. 2013, 8, 14) proposes the absorption of CO2 with amino-siloxane compounds to obtain a solid reaction product. Chinese patent application 'preparation of two-phase absorbent from ethylenediamine and DMA' for removing CO from biohydrogen alkane gas 2 The method (application number 201711311798.1, publication date 2018, 6, 19) proposed that ethylenediamine and DMA were mixed to obtain a liquid two-phase absorbent that reacted with CO2 to form a solid precipitate. The Chinese patent application (application No. 201310631961.8, publication No. 2014, 3 and 26) proposes a biphasic absorbent composed of enamine and an organic solvent, wherein the organic solvent is C1-C10 alcohols, toluene, DMF and DMAC, and carbon dioxide in the gas mixture is removed by precipitation after contacting with the absorbent. The components of the phase-change absorbent with the liquid-solid phase are volatile or not common amine, and have high price and economy to be checkedAnd (5) inspecting.
In summary, it is of practical interest to develop a mature liquid-solid phase change absorber based on industrial applications.
Disclosure of Invention
In view of the drawbacks of the prior art, an object of the present invention is to provide a method for CO 2 Separated liquid-solid phase absorbent that absorbs CO 2 The front is a uniform liquid phase for absorbing CO 2 Spontaneously forming liquid-solid two phases after gas source, CO 2 Concentrating in solid phase, separating to obtain solid phase, desorbing only the solid phase, and recycling the absorbent obtained by desorption. Only the solid needs to be heated in the desorption process, no sensible heat of temperature rise and no latent heat of water evaporation are generated, and CO is further reduced 2 And (5) energy consumption is relieved.
In order to achieve the above purpose, the invention adopts the technical scheme that:
for CO 2 The separated liquid-solid phase-splitting absorbent takes N-methyldiethanolamine as a main body and comprises an activating agent piperazine, an organic solvent and water, wherein the mass percentage of the N-methyldiethanolamine is 20-40%; 3-15% of piperazine as an activator; the mass percentage of the organic solvent is 30-60%, the mass percentage of the water is 0-40%, and the sum of the total mass percentages is 100%. The liquid-solid phase-splitting absorbent absorbs CO 2 The gas source is a uniform liquid phase before absorbing CO 2 Spontaneously forming liquid-solid two phases after gas source, CO 2 Concentrating in solid phase, separating to obtain solid phase, desorbing only the solid phase, and recycling the absorbent obtained by desorption.
Preferably, in the liquid-solid phase-splitting absorbent, the mass percentage of N-methyldiethanolamine is 30% -40%, the mass percentage of piperazine as an activating agent is 3% -10%, the mass percentage of organic solvent is 40% -60%, the mass percentage of water is 0% -20%, and the sum of the mass percentages is 100%.
Preferably, in the liquid-solid phase-splitting absorbent, the mass percentage of N-methyldiethanolamine is 32%, the mass percentage of piperazine as an activator is 8%, the mass percentage of organic solvent is 40%, the mass percentage of water is 20%, and the sum of the total mass percentages is 100%.
Preferably, in the liquid-solid phase-splitting absorbent, the mass percentage of N-methyldiethanolamine is 37%, the mass percentage of piperazine as an activating agent is 3%, the mass percentage of organic solvent is 40%, the mass percentage of water is 20%, and the sum of the total mass percentages is 100%.
Preferably, in the liquid-solid phase-splitting absorbent, the mass percentage of N-methyldiethanolamine is 32%, the mass percentage of piperazine as an activator is 8%, the mass percentage of organic solvent is 60%, and the sum of the total mass percentages is 100%.
Preferably, the organic solvent is selected from any one or more of dimethyl sulfoxide, N-methylpyrrolidone, N-methylformamide and N, N-dimethylformamide, preferably N-methylpyrrolidone.
Further, the liquid-solid phase-splitting absorbent absorbs CO 2 Spontaneously forming liquid-solid two phases after gas source, CO 2 Enriched in the solid phase.
Further, the solid phase of the liquid-solid phase-splitting absorbent accounts for 5-50% of the volume of the liquid-solid phase-splitting absorbent.
Further, the liquid-solid phase-splitting absorbent absorbs CO 2 Spontaneously forming a liquid-solid phase after the air source, wherein the solid phase accounts for 5-50% of the volume of the liquid-solid phase-splitting absorbent; the solid phase is obtained through separation, only the solid phase is desorbed, and the absorbent obtained through desorption is recycled.
Preferably, the liquid-solid phase absorbent absorbs CO 2 The conditions of the air source are as follows: the pressure is normal pressure-3.0 MPaG, and the temperature is 20-80 ℃.
CO using the liquid-solid phase absorbent described above 2 A method of separation comprising the steps of: at a temperature of 20-80 ℃, CO 2 The pressure of the air source is normal pressure-3.0 MPaG, and the absorbent is mixed with CO 2 Gas source contact reaction, CO absorption 2 The gas source is a uniform liquid phase before absorbing CO 2 Spontaneously forming liquid-solid two phases after gas source, wherein the solid phase is CO 2 The enriched liquid phase and the solid phase account for 5 to 50 percent of the volume of the liquid-solid phase-splitting absorbent; introducing the rich liquid phase into a desorption unitAnd (3) desorbing the element, and recycling the absorbent obtained by desorption.
Still further, the CO 2 The gas source is flue gas, natural gas, shift gas or synthetic gas.
Compared with the prior art, the invention provides a method for preparing CO 2 The separated liquid-solid phase absorbent has the following advantages:
the main body of the liquid-solid phase-splitting absorbent is N-methyldiethanolamine, which has the advantage of low regeneration energy consumption and can reduce CO 2 Energy consumption is relieved; the activator component can improve the absorption of CO by the liquid-solid phase absorbent 2 Reduces the height of the absorption equipment and reduces the equipment investment.
Second, the liquid-solid phase absorbent of the present invention absorbs CO 2 The gas source is a uniform liquid phase before absorbing CO 2 Spontaneously forming liquid-solid two phases after gas source, CO 2 Concentrating in solid phase, separating to obtain solid phase, desorbing only the solid phase, and recycling the absorbent obtained by desorption. In the desorption process, only the solid needs to be heated, no sensible heat of temperature rise and no latent heat of water evaporation are generated, and CO is further reduced 2 And (5) energy consumption is relieved.
Detailed Description
The invention is further described below in connection with specific embodiments and examples.
Example 1
Mixing N-methyldiethanolamine, an activator piperazine, N, N-dimethylformamide and water to prepare 100g of absorbent, wherein the mass fraction of the N-methyldiethanolamine is 32%, the mass fraction of the activator piperazine is 8%, the mass fraction of the N, N-dimethylformamide is 40%, and the mass fraction of the water is 20%; at 40 ℃ and normal pressure, the mixed gas CO 2 A content of 50%, and is absorbed to saturation by the absorbent; CO absorption 2 The absorbent after the reaction forms a liquid-solid phase, and the solid phase is CO 2 The phase was concentrated to a volume of 5.0mL. CO 2 The solid phase accounts for 5% of the volume of the liquid-solid phase-splitting absorbent.
Example 2
Mixing N-methyldiethanolamine, piperazine as activator, dimethyl sulfoxide and water to obtain absorbent 100g, wherein N-methyl32% of the mass fraction of the base diethanolamine, 8% of the mass fraction of the piperazine as an activator, 40% of the mass fraction of the dimethyl sulfoxide and 20% of the mass fraction of the water; at 40 ℃ and normal pressure, the mixed gas CO 2 15% by weight, absorbed to saturation with the absorbent; CO absorption 2 The absorbent after the reaction forms a liquid-solid phase, and the solid phase is CO 2 The phase was concentrated to a volume of 17.0mL. CO 2 The solid phase accounts for 17% of the volume of the liquid-solid phase absorbent.
Example 3
Mixing N-methyldiethanolamine, an activator piperazine, N-methylpyrrolidone and water to prepare 100g of absorbent, wherein the mass fraction of the N-methyldiethanolamine is 37%, the mass fraction of the activator piperazine is 3%, the mass fraction of the N-methylpyrrolidone is 50%, and the mass fraction of the water is 10%; at 40 ℃ and normal pressure, the mixed gas CO 2 15% by weight, absorbed to saturation with the absorbent; CO absorption 2 The absorbent after the reaction forms a liquid-solid phase, and the solid phase is CO 2 The phase was concentrated to a volume of 40.0mL. CO 2 The solid phase accounts for 40% of the volume of the liquid-solid phase absorbent.
Example 4
Mixing N-methyldiethanolamine, an activator piperazine, N-methylpyrrolidone and water to prepare 100g of absorbent, wherein the mass fraction of the N-methyldiethanolamine is 30%, the mass fraction of the activator piperazine is 10%, the mass fraction of the N-methylpyrrolidone is 50%, and the mass fraction of the water is 10%; at 40 ℃ and normal pressure, the mixed gas CO 2 15% by weight, absorbed to saturation with the absorbent; CO absorption 2 The absorbent after the reaction forms a liquid-solid phase, and the solid phase is CO 2 The phase was concentrated to a volume of 7.0mL. CO 2 The solid phase accounts for 7% of the volume of the liquid-solid phase absorbent.
Example 5
Mixing N-methyldiethanolamine, an activator piperazine, N-methylpyrrolidone and water to prepare 100g of absorbent, wherein the mass fraction of the N-methyldiethanolamine is 32%, the mass fraction of the activator piperazine is 8%, the mass fraction of the N-methylpyrrolidone is 60%, and the mass fraction of the water is 0%; at a temperature of 40 c,atmospheric pressure, mixed gas CO 2 15% by weight, absorbed to saturation with the absorbent; CO absorption 2 The absorbent after the reaction forms a liquid-solid phase, and the solid phase is CO 2 The phase was concentrated to a volume of 20.0mL. CO 2 The solid phase accounts for 20% of the volume of the liquid-solid phase absorbent.
Example 6
Mixing N-methyldiethanolamine, an activator piperazine, an organic solvent and water, wherein the organic solvent is a mixture of N, N-dimethylformamide and N-methylformamide, and 100g of absorbent is prepared, wherein the mass fraction of the N-methyldiethanolamine is 30%, the mass fraction of the activator piperazine is 10%, the mass fraction of the N, N-dimethylformamide is 25%, the mass fraction of the N-methylformamide is 10%, namely the mass fraction of the organic solvent is 35%, and the mass fraction of the water is 25%; at 40 ℃ and normal pressure, pure CO 2 Absorbing to saturation by using the absorbent; CO absorption 2 The absorbent after the reaction forms a liquid-solid phase, and the solid phase is CO 2 The phase was concentrated to a volume of 15.0mL. CO 2 The solid phase accounts for 15% of the volume of the liquid-solid phase-splitting absorbent.
Comparative example 1:
the preparation of the liquid-solid phase absorbent was carried out by the same procedure as in example 1 except that the organic solvent was replaced with n-propanol, and the remaining conditions were identical. But the absorbent prepared is in any CO 2 No phase separation occurs at all partial pressures.
Comparative example 2:
mixing N-methyldiethanolamine, an organic solvent and water, wherein the organic solvent is polyethylene glycol dimethyl ether, and preparing 100g of absorbent, wherein the mass fraction of the N-methyldiethanolamine is 30%, the mass fraction of the polyethylene glycol dimethyl ether is 20%, and the mass fraction of the water is 40%; the absorbent obtained is configured to absorb any CO 2 No phase separation occurs at all partial pressures.
Comparative example 3:
mixing N-methyldiethanolamine, piperazine as an activator, an organic solvent and water, wherein the organic solvent is N-methylpyrrolidone, and preparing 100g of absorbent, wherein the mass fraction of N-methyldiethanolamine is 35%, the mass fraction of piperazine is 5%, and the N-methylpyrrolidone is preparedThe mass fraction of the pyrrolidone is respectively 10%, 20% or 25% for experiments, the balance is the mass fraction of water, and the total mass fraction is 100%. The absorbent obtained is configured to absorb any CO 2 No phase separation occurs at all partial pressures.
Comparative example 4:
n-methyl diethanolamine, piperazine as an activator, an organic solvent and water are mixed, wherein the organic solvent is N-methyl pyrrolidone, 100g of absorbent is prepared, the mass fraction of the N-methyl diethanolamine is 39%, the mass fraction of the piperazine is 1%, the mass fraction of the N-methyl pyrrolidone is 50%, and the mass fraction of the water is 10%. The absorbent obtained is configured to absorb any CO 2 No phase separation occurs at all partial pressures.
Comparative example 5:
mixing N-methyldiethanolamine, an activator piperazine, an organic solvent and water, wherein the organic solvent is polyethylene glycol dimethyl ether, and preparing 100g of absorbent, wherein the mass fraction of the N-methyldiethanolamine is 30%, the mass fraction of the piperazine is 5%, the mass fraction of the polyethylene glycol dimethyl ether is 10%, and the mass fraction of the water is 55%. The absorbent obtained is configured to absorb any CO 2 No phase separation occurs at all partial pressures.
Comparative example 6:
mixing N-methyldiethanolamine, an activator morpholine, an organic solvent and water, wherein the organic solvent is polyethylene glycol dimethyl ether or sulfolane, and preparing 100g of absorbent, wherein the mass fraction of the N-methyldiethanolamine is 30%, the mass fraction of the morpholine is 5%, the mass fraction of the polyethylene glycol dimethyl ether or sulfolane is 10%, and the mass fraction of the water is 55%. The absorbent (organic solvent is polyethylene glycol dimethyl ether or sulfolane) obtained by the preparation method is prepared in any CO 2 No phase separation occurs at all partial pressures.
The above-described embodiments are merely illustrative of the present invention, which may be embodied in other specific forms or with other specific forms without departing from the spirit or essential characteristics thereof. The described embodiments are, therefore, to be considered in all respects as illustrative and not restrictive. The scope of the invention should be indicated by the appended claims, and any changes that are equivalent to the intent and scope of the claims are intended to be encompassed within the scope of the invention.
Claims (1)
1. CO by using liquid-solid phase-splitting absorbent 2 A method of separation characterized by: mixing N-methyldiethanolamine, an activator piperazine, N, N-dimethylformamide and water to prepare 100g of absorbent, wherein the mass fraction of the N-methyldiethanolamine is 32%, the mass fraction of the activator piperazine is 8%, the mass fraction of the N, N-dimethylformamide is 40%, and the mass fraction of the water is 20%; at 40 ℃ and normal pressure, the mixed gas CO 2 A content of 50%, and is absorbed to saturation by the absorbent; CO absorption 2 The absorbent after the reaction forms a liquid-solid phase, and the solid phase is CO 2 An enriched phase, volume 5.0 mL; CO 2 The enrichment phase accounts for 5% of the volume of the liquid-solid phase absorbent.
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