CN115518493A - Organic amine-alcohol aqueous sulfur dioxide liquid-liquid phase change absorbent and preparation method and application thereof - Google Patents

Organic amine-alcohol aqueous sulfur dioxide liquid-liquid phase change absorbent and preparation method and application thereof Download PDF

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CN115518493A
CN115518493A CN202211273455.1A CN202211273455A CN115518493A CN 115518493 A CN115518493 A CN 115518493A CN 202211273455 A CN202211273455 A CN 202211273455A CN 115518493 A CN115518493 A CN 115518493A
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liquid
absorbent
phase
phase change
piperazine
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魏凤玉
刁忠秀
宋小良
李淑全
苏文国
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Shuangdun Environment Technology Co ltd
Hefei University of Technology
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Shuangdun Environment Technology Co ltd
Hefei University of Technology
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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
    • B01D53/1481—Removing sulfur dioxide or sulfur trioxide
    • 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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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Analytical Chemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Treating Waste Gases (AREA)
  • Gas Separation By Absorption (AREA)

Abstract

The invention relates to the technical field of gas separation, energy conservation and emission reduction, in particular to an organic amine-alcohol water system SO 2 Liquid-liquid phase change absorbent and a preparation method and application thereof. The absorbent comprises the following components: 10-30 parts of piperazine organic amine, 5-60 parts of phase splitting agent and 0.1-10 parts of phase change additive; the piperazine organic amine contains an alkyl hydroxyl group, and the alkyl hydroxyl group is selected from one or two of hydroxyethyl or hydroxypropyl; the phase separation agent is selected from one or more than two of C4-C7 alcohols, and the phase change auxiliary agent is selected from inorganic acid or organic acid. The preparation method of the liquid-liquid phase change absorbent comprises the following steps: and adding the raw materials containing the piperazine organic amine, the phase-splitting agent and the phase-change assistant into water, and dissolving to obtain the liquid-liquid phase-change absorbent. The absorbent can increase SO 2 The desorption efficiency is reduced, the desorption energy consumption is reduced, and the operation cost of enterprises is greatly reduced.

Description

Organic amine-alcohol aqueous sulfur dioxide liquid-liquid phase change absorbent and preparation method and application thereof
Technical Field
The invention relates to the technical field of gas separation, energy conservation and emission reduction, and particularly relates to an organic amine-alcohol water system SO 2 Liquid-liquid phase change absorbent and preparation method and application thereof。
Background
Chemical absorption of SO 2 Or CO 2 The acid gas has the advantages of high absorption rate, large absorption capacity, good selectivity and the like, the process is mature, the application range of the acid gas concentration in the waste gas is wide, and the absorbed rich solution needs to be pyrolyzed at high temperature to absorb the acid gas SO 2 Or CO 2 The absorbent can be recycled, and the development of the absorbent is restricted by high energy consumption.
Phase change absorption refers to absorption of SO 2 Form supported SO during or after absorption 2 The lean and rich phases with larger quantity difference only send the rich phase with higher loading capacity into the regeneration tower, thereby greatly reducing the volume of the regeneration solution and remarkably reducing the regeneration energy consumption. SO reported at present 2 Most phase change absorbents are solvent-based and undergo a liquid-solid phase change after absorption. Chinese patent' a method for capturing CO by phase change 2 、SO 2 The mixed organic solution of acidic gas "(CN 201510675190.1) is prepared by absorbing SO with a mixed solution of organic amine absorbent such as chain polyamine, alcohol amine, and amide and organic solvent such as alcohol, ether, ketone, and ester 2 Separating the solid from the liquid, heating the solid to 115 deg.C and 0.27Mpa to obtain SO 2 And (4) recovering. However, these phase change absorbents have high viscosity, are not favorable for heat and mass transfer and fluid transportation, and require long phase separation time. In order to reduce the viscosity of an organic phase, the patent "a method for regenerating the organic phase after enhancing desulfurization and decarburization of a phase-change absorbent" (CN 201610440435.7) applies the displacement effect, cavitation effect and resonance effect of ultrasound to the phase-change absorbent to regenerate a rich solution, but an ultrasound device needs to be arranged in a regeneration tower, so that the system is complex, the investment is high, the ultrasound energy is consumed, and the practical industrial application is not easy to implement. In addition, the solid generated during phase change absorption is easy to block the pipeline, so that the practical application is not changed.
Due to SO content in industrial processes 2 The smoke is often a wet gas containing a large amount of saturated water, and the non-water-soluble phase-change absorbent cannot meet the industrial requirements. Chinese invention patent 'MDEA composite absorbent for acid gas separation and separation method' (CN 201610035154.3) based on MDEA dissolution assisting effectThe composite absorbent comprising MDEA, water-immiscible alcohols and water is a homogeneous phase before absorbing acid gas, a lean liquid phase with less acid gas load and a rich liquid phase with large acid gas load are formed after absorbing acid gas, and only the rich liquid phase enters a desorption unit, so that the desorption energy consumption is reduced. Due to H 2 S、SO 2 Etc. are toxic or corrosive, the examples of this patent are only to absorb CO 2 The advantages and features of the invented liquid-liquid phase change absorbent are illustrated by way of example. The patent "an absorbing liquid for capturing sulfur dioxide by phase change" (CN 201811230995.5) also discloses SO composed of alcohol amine absorbent, sulfone and water 2 Compared with the conventional desulfurization process, the absorption liquid reduces the desorption treatment capacity by 30-55 percent (mass fraction), and obviously reduces the desorption energy consumption.
Disclosure of Invention
The invention solves the technical problems that: chemical absorption of CO by alcohol amine 2 、H 2 S field is widely applied, but to SO 2 Is poor and is due to SO 2 Strong corrosivity, poor stability of alcohol amine, and few alcohol amines are used as SO industrially 2 The absorbent of (1). The organic amine wet flue gas desulfurization technology has the advantages of high desulfurization rate, good selectivity, high recycling rate of the absorbent, no secondary pollution and the like, and is applied to the industries of nonferrous smelting, sulfuric acid industry, coal chemical industry and the like more and more widely at present. Most of the existing organic amine desulfurizer focuses on SO 2 In order to make the organic amine desulfurization process more efficient, the absorbent needs to be recycled after desorption, but the desorption efficiency, the recycling rate and the recycling effect of the existing absorbent still need to be improved; in addition, the absorbed rich amine solution needs to be heated at high temperature to desorb SO 2 Therefore, a large amount of raw steam is consumed, the regeneration energy consumption is high, the operation cost of enterprises is overhigh, and the wide application of the organic amine desulfurizer in industry is limited. From the industrial application perspective, the development of water-soluble SO 2 The liquid-liquid phase change absorbent has great significance for reducing the energy consumption of the organic amine desulfurization system, reducing the operation cost of the system and improving the economic benefit of enterprises.
The purpose of the invention is: provide an absorptionHigh efficiency, good selectivity, high desorption rate, low regeneration energy consumption, energy conservation and environmental protection of organic amine-alcohol water system SO 2 Liquid-liquid phase change absorbent for trapping SO 2 And the water-soluble paint can be dissolved in water and can be used in a water system environment.
In order to solve the above technical problems, the present invention provides an organic amine-alcohol aqueous SO system 2 Liquid-liquid phase change absorbent for absorbing SO 2 Then quickly divided into two water phases, wherein the lower water phase is SO 2 The upper aqueous phase is SO 2 A lean liquid phase. Only SO is required to be added 2 The rich liquid phase (lower water phase) is sent into a desorption tower for regeneration, thereby solving the problem of high desorption energy consumption of the existing non-phase change absorption system.
Specifically, aiming at the defects of the prior art, the invention provides the following technical scheme:
organic amine-alcohol water system SO 2 The liquid-liquid phase change absorbent is characterized by comprising the following components:
10-30 parts of piperazine organic amine, 5-60 parts of phase splitting agent and 0.1-10 parts of phase change additive; the piperazine organic amine contains an alkyl hydroxyl group, and the alkyl hydroxyl group is selected from one or two of hydroxyethyl or hydroxypropyl; the phase separation agent is selected from one or more than two of C4-C7 alcohols, and the phase change auxiliary agent is selected from inorganic acid or organic acid.
Preferably, in the liquid-liquid phase change absorbent, the absorbent comprises the following components: 15-30 parts of piperazine organic amine, 10-45 parts of phase separation agent and 0.1-5 parts of phase change assistant.
Preferably, in the liquid-liquid phase change absorbent, the piperazine organic amine is 20-30 parts by weight, preferably 25-30 parts by weight;
preferably, in the liquid-liquid phase change absorbent, the phase separation agent is 15-45 parts by weight, preferably 20-45 parts by weight, and more preferably 20-30 parts by weight;
preferably, in the liquid-liquid phase change absorbent, the phase change aid is 0.5 to 5 parts by weight, preferably 3 to 5 parts by weight.
Preferably, in the liquid-liquid phase change absorbent, the piperazine-based organic amine is one or more selected from N-hydroxyethyl piperazine, N-bis (2-hydroxyethyl) piperazine, N-bis (2-hydroxypropyl) piperazine, and N-hydroxyethyl-N-hydroxypropyl piperazine.
Preferably, in the liquid-liquid phase change absorbent, the piperazine-based organic amine contains at least N-hydroxyethyl piperazine.
Preferably, in the liquid-liquid phase change absorbent, the piperazine organic amine in the absorbent is a mixture of N, N-bis (2-hydroxyethyl) piperazine (BHEP) and N-hydroxyethyl piperazine (HEP) or a mixture of N, N-bis (2-hydroxypropyl) piperazine (HPP) and N-hydroxyethyl piperazine (HEP).
Preferably, in the liquid-liquid phase change absorbent, the N-hydroxyethyl piperazine accounts for 10 to 20 mass percent of the piperazine organic amine.
Preferably, in the liquid-liquid phase change absorbent, the phase separation agent is one or more selected from n-butanol, n-pentanol, sec-pentanol, cyclohexanol and 1, 7-heptanediol.
Preferably, in the liquid-liquid phase change absorbent, the number of hydroxyl groups of the phase separating agent is 1 to 2.
Preferably, in the liquid-liquid phase change absorbent, the phase change aid is one or more selected from sulfuric acid, phosphoric acid, hydrochloric acid and boric acid.
Preferably, in the liquid-liquid phase change absorbent, the phase change assistant is selected from boric acid, hydrochloric acid or phosphoric acid.
Preferably, in the liquid-liquid phase change absorbent, the absorbent further comprises water, and the weight part of the water is 30-70.
The invention also provides an organic amine-alcohol aqueous SO system 2 The preparation method of the liquid-liquid phase change absorbent is characterized by comprising the following steps:
adding raw materials containing piperazine organic amine, a phase-splitting agent and a phase-change assistant into water, and dissolving to obtain the organic amine-alcohol water system SO 2 Liquid-liquid phase change absorbent.
The invention also provides a method for collecting SO 2 The method is characterized by comprising the following steps:
(1) And (3) an absorption process: will contain SO 2 The gas is mixed with the liquid-liquid phase change absorbent, and after absorption reaction, the mixture is absorbedThe collected liquid is quickly divided into a lower water phase and an upper water phase;
(2) And (3) desorption process: heating and desorbing the lower water phase, mixing the lean solution obtained after desorption with the upper water phase obtained in the step (1), and recycling the lean solution as an absorbent.
Preferably, the trapped SO is 2 In the method of (3), the temperature in the absorption reaction process is 20-50 ℃, and the temperature in the desorption process is 80-120 ℃, preferably 100-110 ℃.
Preferably, the trapped SO is 2 In the method of (1), the SO is contained 2 In the gas of (2), SO 2 The volume fraction of (b) is 0.1% to 15%, preferably 5% to 15%. The flow rate of the gas is 1.0-2.0L/min.
Preferably, the trapped SO is 2 In the method of (1), the time of the absorption process is 120 to 180min.
Preferably, the trapped SO is 2 In the method, the temperature of the desorption process is 105-110 ℃. The time of the desorption process is 0.5 to 3.5 hours, preferably 2.5 to 3.5 hours.
Preferably, the trapped SO is 2 In the method of (1), the volume of the lower aqueous phase in the absorption tower accounts for 20-90% of the total liquid phase volume, preferably, the volume of the lower aqueous phase in the absorption tower accounts for 40-90% of the total liquid phase volume, preferably 65-85%.
Preferably, the trapped SO is 2 In the method of (1), SO is added to the upper and lower aqueous phases 2 The concentration ratio of (3) to (15): 1, preferably (5-15): 1.
the invention also provides the organic amine-alcohol aqueous SO 2 The liquid-liquid phase change absorbent is applied to the field of flue gas desulfurization.
The invention has the advantages that:
(1) The phase change absorbent provided by the invention can improve SO 2 The desorption efficiency is reduced, the desorption energy consumption is reduced, the circulating absorption capacity and the circulating utilization effect of the absorbent are improved, and the operation cost of enterprises is greatly reduced.
(2) In the phase change absorbent provided by the invention, the low-polarity phase separating agent organic alcohol enables piperazine organic amine to absorb a small amount of SO 2 Then quickly divided into twoAn aqueous phase, and because only a very small amount of SO is loaded in the upper aqueous phase 2 Only the load SO is required 2 The aqueous phase is desorbed, so that the volume of desorbed pregnant solution is reduced, and the desorption energy consumption is obviously reduced.
(3) The piperazine organic amine and the organic alcohol with longer carbon chains in the phase change absorbent provided by the invention have high boiling points, and the volatility loss of the absorbent and a solvent is avoided.
(4) The phase change assistant in the phase change absorbent provided by the invention can reduce the volatilization loss of piperazine organic amine, increase the polarity of an absorption product and promote the occurrence of phase change.
(5) The phase change absorbent provided by the invention is aqueous solution, has low viscosity and excellent heat and mass transfer performance and conveying performance, so that a heat exchanger, a pump and the like in the conventional industrial organic amine desulfurization system do not need to be replaced and modified, and the use is convenient.
In summary, the present invention provides a phase change absorbent for SO 2 The method and the process for using the absorbent provided by the invention are energy-saving and environment-friendly, have no secondary pollution, can be recycled for many times, have better recycling rate and recycling effect, and have wide application prospect.
Detailed Description
In view of the current use for capturing SO 2 The absorption effect and the stability of the absorbent are all required to be improved, the invention mixes the specific phase-splitting agent with the piperazine organic amine absorbent, the phase-change assistant and water according to a proper proportion to form a brand new phase-change absorbent, and the absorbent has strong stability, high absorption efficiency and more energy-saving and environment-friendly use process.
In a preferred embodiment, the present invention provides a method for absorbing and separating SO 2 Organic amine-alcohol water system SO 2 The liquid-liquid phase change absorbent consists of an organic amine desulfurizer, a phase splitting agent, a phase change additive and water, wherein the organic amine desulfurizer is one of piperazine organic amines N-hydroxyethyl piperazine HEP, N-di (2-hydroxyethyl) piperazine BHEP, N-di (2-hydroxypropyl) piperazine HPP and N-hydroxyethyl-N-hydroxypropyl piperazine (HEHPP)Or a mixture of a plurality of the phase-separating agents, wherein the phase-separating agent is any one or a combination of two of C4-C7 alcohols, and the phase-change assistant is one or two of sulfuric acid, phosphoric acid, hydrochloric acid and boric acid.
In the liquid-liquid phase change absorbent, the mass fraction of the piperazine organic amine is 10-30%, the mass fraction of the phase-splitting agent is 5-60%, the mass fraction of the phase-change assistant is 0.1-10%, and the balance is water.
Preferably, in the liquid-liquid phase change absorbent, the mass fraction of the piperazine organic amine is 15-30%, the mass fraction of the phase separation agent is 15-45%, the mass fraction of the phase change assistant is 0.5-5%, and the balance is water.
Preferably, the piperazine organic amine in the liquid-liquid phase change absorbent is a mixture of N, N-bis (2-hydroxyethyl) piperazine BHEP and N-hydroxyethyl piperazine HEP or a mixture of N, N-bis (2-hydroxypropyl) piperazine HPP and N-hydroxyethyl piperazine HEP.
Preferably, the phase separating agent in the liquid-liquid phase change absorbent is any one or a combination of two of n-butyl alcohol, n-amyl alcohol, sec-amyl alcohol, cyclohexanol or 1, 7-heptanediol.
Preferably, the phase change absorbent absorbs SO by adjusting the composition ratio of the absorbent 2 Then liquid-liquid two phases are formed spontaneously, and the volume of the lower phase accounts for 20-85% of the volume ratio of the total liquid phase.
Preferably, the phase-change absorbent absorbs SO by adjusting the composition ratio of the absorbent 2 Then liquid-liquid two phases are formed spontaneously, and the volume of the lower phase accounts for 65-85% of the volume ratio of the total liquid phase.
In another preferred embodiment, the present invention provides for capturing SO 2 The method comprises the following steps:
will contain SO 2 After the flue gas and the absorbent are mixed and react, the absorbent is divided into a lower water phase and an upper water phase, the lower water phase is sent into a desorption device for desorption, and lean solution obtained after desorption is mixed with the upper water phase and used as the absorbent for recycling.
In another preferred embodiment, the present invention provides an organic amine-alcohol aqueous system SO 2 Liquid-liquid phase change absorbent in SO 2 Use in the field of capture comprising the steps of:
s1, using the piperazine organic amine as an absorbent, adding 10-30% of organic alcohol by mass, then adding 0.1-6.0% of acid by mass as a phase change additive, and finally preparing a homogeneous phase aqueous solution with a certain proportion of water as a phase change absorbent;
s2, using the phase change absorbent configured in the S1 for absorbing and separating SO-containing substances 2 The volume fraction is 0.1 to 15 percent and the rest is N 2 The absorption temperature of the simulated smoke is 20-50 ℃. Absorption of SO 2 Then spontaneously divided into two phases, the lower aqueous phase being SO 2 The enrichment phase of (1) is enriched with most of organic amine and SO 2 Organic amine salt, water and a small amount of phase separating agent after reaction; the upper water phase is SO 2 A lean phase of (A) containing small amounts of organic amine and SO 2 Organic amine salt after reaction, water and a large amount of phase separating agent.
S3, absorbing SO 2 Separating the upper water phase from the lower water phase, and desorbing and regenerating the lower water phase. Desorbing and regenerating at 100-120 deg.c for 0.5-3.5 hr to desorb SO 2 And (4) recycling. Mixing the rich-phase regenerated lean amine solution with the upper water phase to obtain the liquid-liquid phase change absorbent for circularly absorbing SO 2 。
The piperazine organic amine of the present invention refers to a compound having a piperazine structure, preferably, an alkylhydroxy group is connected to a nitrogen atom of the piperazine structure.
The organic amine-alcohol aqueous SO system of the present invention is further illustrated by the following specific examples 2 Liquid-liquid phase change absorbent, and preparation method and application thereof.
The piperazine organic amine HEHPP is N-hydroxyethyl piperazine, the organic amine BHEP is N, N-di (2-hydroxyethyl) piperazine, also called 1, 4-di (2-hydroxyethyl) piperazine, the organic amine HPP is N, N-di (2-hydroxypropyl) piperazine, also called 1, 4-di (2-hydroxypropyl) piperazine, prepared by the method of step A of example 1 in CN101584961A, and the organic amine HEHPP is N-hydroxyethyl-N-hydroxypropyl piperazine, also called 1- (2-hydroxyethyl) -4- (2-hydroxypropyl) piperazine) Piperazine, prepared by the procedure described in the example of CN103638779A, and other reagents purchased from the group of chinese pharmaceuticals. In the following examples, the simulated flue gas is subjected to SO removal 2 In addition, the rest is N 2 。
Example 1
Compounding N, N-di (2-hydroxyethyl) piperazine (BHEP), N-butanol and water, and adding sulfuric acid to prepare the compound for trapping SO 2 The liquid-liquid phase change absorbent. In the obtained absorbent, the mass fraction of BHEP is 30%, the mass fraction of n-butanol is 20%, the mass fraction of sulfuric acid is 3.5%, and the rest is water.
Will contain SO 2 And introducing the simulated flue gas with the concentration of 9% into 100g of absorbent, wherein the flow rate of the simulated flue gas is 1.4L/min, the absorption temperature is 25 ℃, and the absorption time is 120min. Absorption of SO 2 The absorbent automatically forms liquid-liquid two phases, wherein the lower water phase accounts for 80.7 percent of the total volume, and the lower water phase and the upper water phase contain SO 2 Is 10.8, SO of the absorbent 2 The pick-up was 0.6874mol/mol amine. Adding SO 2 Desorbing and regenerating the rich phase (namely the lower water phase) at 107 ℃ for 180min 2 The cyclic absorption EQ of (1) is 0.4342mol/mol amine, SO 2 The desorption rate was 74.6%.
Compared with the absorbent without n-butanol, the regenerated treatment liquid amount of the embodiment is reduced by 19%, the cyclic absorption amount EQ is improved by 26.4%, the desorption rate DE is improved by 12.8%, and the regeneration energy consumption Q is reduced by 34%. The viscosity of the absorption solution without n-butanol addition was 10.5cP, and the viscosity of the rich liquid phase of this example increased to 25.0cP, still lower.
Wherein, the absorbent absorbs SO in the upper and lower aqueous phases 2 The concentration was measured by iodometry and the viscosity was measured by a rotational viscometer.
Cyclic absorption EQ = absorption of SO by absorption liquid 2 The rich liquid SO obtained later 2 Loading and SO of the barren solution obtained after desorption 2 Difference in loading, i.e. SO desorbed from each mole of organic amine 2 Number of moles in molSO 2 Per mol of amine.
Desorption rate in desorption process DE = desorption of SO 2 Amount of (D)/SO in the pregnant solution before desorption 2 The amount of (B) is multiplied by 100 percent
The energy consumption Q in the desorption process refers to the desorption unit mass SO 2 The power consumption is GJ/tSO 2 。
Example 2
Mixing N, N-di (2-hydroxyethyl) piperazine (BHEP), N-butanol and water, and adding boric acid to obtain a solution for capturing SO 2 The absorbent of (1). In the obtained absorbent, the mass fraction of BHEP is 30%, the mass fraction of n-butanol is 20%, the mass fraction of boric acid is 3.5%, and the balance is water.
Will contain SO 2 And introducing the simulated flue gas with the concentration of 9.1% into 100g of absorbent, wherein the flow rate of the simulated flue gas is 1.4L/min, the absorption temperature is 25 ℃, and the absorption time is 120min. Absorption of SO 2 The absorbent forms liquid-liquid two phases, wherein the lower water phase accounts for 80.4% of the total volume, and the lower water phase and the upper water phase are SO 2 Is 11.2, SO of the absorbent 2 The absorption was 0.801mol/mol amine. Adding SO 2 Desorbing and regenerating the rich phase at 107 deg.C for 180min 2 Has a cyclic absorption EQ of 0.429mol/mol amine, SO 2 The desorption rate was 78.2%.
Compared with the homogeneous absorbent without n-butanol, the regenerated treating fluid amount of the embodiment is reduced by 21%, the cyclic absorption EQ is improved by 31.2%, the desorption DE is improved by 28.5%, and the regeneration energy consumption Q is reduced by 38.1%. The viscosity of the absorption solution without n-butanol was 11.3cP, and the viscosity of the rich liquid phase in this example was increased to 24.6cP, which was still small although the viscosity was slightly increased.
Example 3
Mixing N, N-di (2-hydroxyethyl) piperazine (BHEP), N-butanol and water, and adding phosphoric acid to obtain a mixture for capturing SO 2 The absorbent of (1). In the obtained absorbent, the mass fraction of BHEP is 30%, the mass fraction of n-butanol is 20%, the mass fraction of phosphoric acid is 3.5%, and the rest is water.
Will contain SO 2 And introducing the simulated flue gas with the concentration of 9.1% into 100g of absorbent, wherein the flow rate of the simulated flue gas is 1.4L/min, the absorption temperature is 25 ℃, and the absorption time is 120min. Absorption of SO 2 The latter absorbent forming liquidLiquid two phases, the lower aqueous phase accounts for 81.1% of the total volume, and the lower upper aqueous phase is SO 2 Is 12.9, SO of the absorbent 2 The absorption was 0.709mol/mol amine. Adding SO 2 Desorbing and regenerating the rich phase at 107 deg.c for 180min 2 Has a cyclic absorption EQ of 0.367mol/mol amine, SO 2 The desorption rate was 59.7%.
Compared with the homogeneous absorbent without n-butanol, the regenerated treatment liquid amount of the embodiment is reduced by 19%, the cyclic absorption amount EQ is improved by 27.8%, the desorption rate DE is improved by 32.3%, and the regeneration energy consumption Q is reduced by 33.4%. The viscosity of the absorption solution without n-butanol was 10.5cP, and the viscosity of the rich liquid phase in this example was increased to 30.2cP, which was slightly increased but still small.
Example 4
Mixing N, N-bis (2-hydroxyethyl) piperazine (BHEP), N-butanol and water, and adding hydrochloric acid to obtain a mixture for capturing SO 2 The absorbent of (1). In the obtained absorbent, the mass fraction of BHEP is 30%, the mass fraction of n-butanol is 20%, the mass fraction of hydrochloric acid is 3.5%, and the rest is water.
Will contain SO 2 And introducing the simulated flue gas with the concentration of 9.1% into 100g of absorbent, wherein the flow rate of the simulated flue gas is 1.4L/min, the absorption temperature is 25 ℃, and the absorption time is 120min. Absorption of SO 2 The absorbent forms liquid-liquid two phases, the lower aqueous phase accounts for 83.6 percent of the total volume, and the lower aqueous phase and the upper aqueous phase are SO 2 Is 8.1, SO of the absorbent 2 The absorption was 0.689mol/mol amine. SO is added 2 Desorbing and regenerating the rich phase at 107 deg.C for 180min 2 Has a cyclic absorption EQ of 0.385mol/mol amine, SO 2 The desorption rate was 42.3%.
Compared with a homogeneous absorbent without n-butanol, the regeneration treatment fluid amount of the embodiment is reduced by 17%, the cyclic absorption quantity EQ is improved by 25.4%, the desorption rate DE is improved by 20.8%, and the regeneration energy consumption Q is reduced by 32.1%. The viscosity of the absorption solution without n-butanol was 10.5cP, and the viscosity of the rich liquid phase in this example was increased to 28.5cP, which was slightly increased but still small.
Comparing examples 1 to 4, it can be found that the kind of the phase change assistant in the phase change absorbent has a certain influence on the phase change absorbent because the acid influences the polarity of the organic amine salt, and the polar organic amine salt has a strong salting-out capability and is dominant in the process of competing for free water with the organic solvent, and the organic solvent is discharged and separated into a liquid-liquid two phase.
Example 5
Mixing N, N-di (2-hydroxypropyl) piperazine (HPP), N-butanol and water, and adding boric acid to obtain the product for trapping SO 2 The absorbent of (1). In the obtained absorbent, the mass fraction of HPP is 20%, the mass fraction of n-butanol is 15%, the mass fraction of boric acid is 2.0%, and the balance is water.
Will contain SO 2 The simulated flue gas with the concentration of 11.1 percent is introduced into 100g of absorbent, the flow rate of the simulated flue gas is 1.6L/min, the absorption temperature is 25 ℃, and the absorption time is 120min. Absorption of SO 2 The absorbent forms liquid-liquid two phases, the lower aqueous phase accounts for 83.6 percent of the total volume, and the lower aqueous phase and the upper aqueous phase are SO 2 Is 8.21, SO of the absorbent 2 The uptake was 0.858mol/mol amine. SO is added 2 Desorbing and regenerating the rich phase at 106 deg.C for 180min 2 Has a cyclic absorption EQ of 0.415mol/mol amine, SO 2 The desorption rate was 80.6%.
Compared with the homogeneous absorbent without n-butanol, the regenerated treatment liquid amount of the embodiment is reduced by 16%, the cyclic absorption amount EQ is improved by 28.3%, the desorption rate DE is improved by 16.5%, and the regeneration energy consumption Q is reduced by 16.2%. The viscosity of the absorption solution without n-butanol was 6.1cP, and the viscosity of the rich liquid phase of this example was 8.1cP, but was still small.
Example 6
Mixing N, N-di (2-hydroxypropyl) piperazine (HPP), N-butanol and water, and adding boric acid to obtain the product for trapping SO 2 The absorbent of (1). In the obtained absorbent, the mass fraction of HPP is 20%, the mass fraction of n-butanol is 20%, the mass fraction of boric acid is 2.0%, and the balance is water.
Will contain SO 2 The simulated flue gas with the concentration of 11.1 percent is introduced into 100g of absorbent, and the flow velocity of the simulated flue gas is 1.6L/min, the absorption temperature is 25 ℃, and the absorption time is 120min. Absorption of SO 2 The latter absorbent forms a liquid-liquid two phase, the lower aqueous phase accounts for 78.3% of the total volume, and the lower aqueous phase and the upper aqueous phase contain SO 2 Concentration ratio of (3) to (7.81), SO of absorbent 2 The absorption was 0.809mol/mol amine. Adding SO 2 Desorbing and regenerating the rich phase at 106 deg.C for 180min 2 The cyclic absorption EQ of (1) is 0.469mol/mol amine, SO 2 The desorption rate was 83.6%.
Compared with the homogeneous absorbent without n-butanol, the regenerated treatment liquid amount of the embodiment is reduced by 22%, the cyclic absorption amount EQ is improved by 30.5%, the desorption rate DE is improved by 20.6%, and the regeneration energy consumption Q is reduced by 25.6%. The viscosity of the absorption solution without n-butanol was 6.1cP, and the viscosity of the rich liquid phase in this example was 10.5cP, but was still small.
Example 7
Mixing N, N-di (2-hydroxypropyl) piperazine (HPP), N-butanol and water, and adding boric acid to obtain the product for trapping SO 2 The absorbent of (1). In the obtained absorbent, the mass fraction of HPP is 20%, the mass fraction of n-butanol is 45%, the mass fraction of boric acid is 2.0%, and the balance is water.
Will contain SO 2 The simulated flue gas with the concentration of 11.1 percent is introduced into 100g of absorbent, the flow rate of the simulated flue gas is 1.6L/min, the absorption temperature is 25 ℃, and the absorption time is 120min. Absorption of SO 2 The latter absorbent forms liquid-liquid two phases, the lower aqueous phase accounts for 69.7% of the total volume, and the lower aqueous phase and the upper aqueous phase contain SO 2 Concentration ratio of 5.62, SO of the absorbent 2 The absorption was 0.756mol/mol amine. Adding SO 2 Desorbing and regenerating the rich phase at 106 deg.C for 180min 2 Has a cyclic absorption EQ of 0.505mol/mol amine, SO 2 The desorption rate was 86.1%.
Compared with a homogeneous absorbent without n-butanol, the regeneration treatment fluid amount of the embodiment is reduced by 30%, the cyclic absorption quantity EQ is improved by 31.2%, the desorption rate DE is improved by 27.6%, and the regeneration energy consumption Q is reduced by 20.9%. The viscosity of the absorption solution without n-butanol was 6.1cP, and the viscosity of the rich liquid phase of this example was 19.3cP, but was still small.
Comparing examples 5 to 7, it can be seen that the larger the mass fraction of n-butanol in the phase change absorbent, the more SO is absorbed 2 The lower the amount of the n-butanol is, the more obvious the influence effect is due to the fact that the mass transfer efficiency is reduced because the viscosity of the lower phase is increased after the absorption phase separation, and the mass fraction of the n-butanol is larger. However, with the increase of the mass fraction of the n-butanol, the reduction rate of the regeneration treatment liquid, the increase rate of the cyclic absorption amount, the increase rate of the desorption rate and the reduction rate of the regeneration energy consumption are gradually increased.
Example 8
Mixing N, N-di (2-hydroxypropyl) piperazine (HPP), N-butanol and water, and adding boric acid to obtain the product for trapping SO 2 The absorbent of (1). In the obtained absorbent, the mass fraction of HPP is 20%, the mass fraction of n-butanol is 20%, the mass fraction of boric acid is 1.2%, and the balance is water.
Will contain SO 2 The simulated flue gas with the concentration of 11.1 percent is introduced into 100g of absorbent, the flow rate of the simulated flue gas is 1.6L/min, the absorption temperature is 25 ℃, and the absorption time is 120min. Absorption of SO 2 The absorbent forms liquid-liquid two phases, wherein the lower aqueous phase accounts for 81.1 percent of the total volume, and the lower aqueous phase and the upper aqueous phase are SO 2 Has a concentration ratio of 3.99, SO of the absorbent 2 The absorption was 1.03mol/mol amine. Adding SO 2 Desorbing and regenerating the rich phase at 106 deg.C for 180min 2 Has a cyclic absorption EQ of 0.383mol/mol amine, SO 2 The desorption rate was 71.5%.
Compared with the homogeneous absorbent without n-butanol, the regenerated treatment liquid amount of the embodiment is reduced by 19%, the cyclic absorption amount EQ is improved by 28.0%, the desorption rate DE is improved by 32.0%, and the regeneration energy consumption Q is reduced by 19.8%. The viscosity of the absorption solution without n-butanol was 6.1cP, and the viscosity of the rich liquid phase of this example was 9.8cP, but was still small.
Example 9
Mixing N, N-di (2-hydroxypropyl) piperazine (HPP), N-butanol and water, and adding boric acid to obtain the product for trapping SO 2 The absorbent of (1). In the obtained absorbent, the mass fraction of HPP is 20%, the mass fraction of n-butanol is 20%, the mass fraction of boric acid is 0.32%, and the balance is water。
Will contain SO 2 The simulated flue gas with the concentration of 11.1 percent is introduced into 100g of absorbent, the absorption temperature is 25 ℃, and the absorption time is 120min. Absorption of SO 2 The absorbent forms liquid-liquid two phases, the lower aqueous phase accounts for 80.8 percent of the total volume, and the lower aqueous phase and the upper aqueous phase are SO 2 Has a concentration ratio of 3.24, SO of the absorbent 2 The absorption was 1.052mol/mol amine. Adding SO 2 Desorbing and regenerating the rich phase at 106 deg.C for 180min 2 Has a cyclic absorption EQ of 0.366mol/mol amine, SO 2 The desorption rate was 67%.
Compared with a homogeneous absorbent without n-butanol, the regeneration treatment liquid amount of the embodiment is reduced by 17.8%, the cyclic absorption amount EQ is increased by 25.4%, the desorption rate DE is increased by 25.5%, and the regeneration energy consumption Q is reduced by 17.8%. The viscosity of the absorption solution without n-butanol addition was 5.0cP, and the viscosity of the rich liquid phase of this example was 6.08cP, but was still small.
Comparing example 6 with examples 8 to 9, it can be seen that the larger the amount of the phase change aid used in the phase change absorbent, the larger the SO 2 The lower the load of (2), this is because acid will react with organic amine, make the active absorption amine number participating in absorption reduce, but improve the cyclic absorption capacity, reduce the regenerated liquid amount, reduce and desorb the energy consumption.
Example 10
Mixing N, N-bis (2-hydroxypropyl) piperazine (HPP), N-hydroxyethyl piperazine (HEP), N-butanol and water, and adding sulfuric acid to obtain a mixture for collecting SO 2 The absorbent of (1). In the obtained absorbent, the mass fraction of HPP is 18%, the mass fraction of HEP is 2%, the mass fraction of n-butanol is 20%, the mass fraction of sulfuric acid is 5.0%, and the balance is water.
Will contain SO 2 And introducing the simulated flue gas with the concentration of 9.1% into 100g of absorbent, wherein the flow rate of the simulated flue gas is 1.5L/min, the absorption temperature is 40 ℃, and the absorption time is 180min. Absorption of SO 2 The latter absorbent forms liquid-liquid two phases, the lower aqueous phase accounts for 79.9% of the total volume, and the lower upper aqueous phase is SO 2 Is 7.23, SO of the absorbent 2 The absorption was 0.649mol/mol amine. SO is added 2 Sending rich phase to solutionAbsorbing and regenerating, wherein the regeneration temperature is 106 ℃, the regeneration time is 180min 2 Has a cyclic absorption EQ of 0.50mol/mol amine, SO 2 The desorption rate was 85.6%.
Compared with the homogeneous absorbent without n-butanol, the regenerated treatment liquid amount of the embodiment is reduced by 20%, the cyclic absorption amount EQ is improved by 23.8%, the desorption rate DE is improved by 22.7%, and the regeneration energy consumption Q is reduced by 22.9%. The viscosity of the absorption solution without n-butanol was 5.8cP, and the viscosity of the rich liquid phase of this example was 10.2cP, but was still small.
Example 11
Mixing N, N-bis (2-hydroxyethyl) piperazine (BHEP), N-hydroxyethyl piperazine (HEP), cyclohexanol and water, and adding boric acid to obtain a mixture for collecting SO 2 The absorbent of (1). In the obtained absorbent, the mass fraction of BHEP was 25.5%, the mass fraction of HEP was 4.5%, the mass fraction of cyclohexanol was 30%, the mass fraction of boric acid was 0.50%, and the balance was water.
Will contain SO 2 The simulated flue gas with the concentration of 11.2 percent is introduced into 100g of absorbent at the flow rate of 1.5L/min, the absorption temperature is 40 ℃, and the absorption time is 180min. Absorption of SO 2 The absorbent forms liquid-liquid two phases, wherein the lower aqueous phase accounts for 76.0 percent of the total volume, and the lower aqueous phase and the upper aqueous phase are SO 2 Is 8.23, SO of the absorbent 2 The absorption was 1.1207mol/mol amine. SO is added 2 Desorbing and regenerating the rich phase at 105 deg.C for 180min 2 Has a cyclic absorption EQ of 0.53mol/mol amine, SO 2 The desorption rate was 82.3%.
Compared with a homogeneous absorbent without cyclohexanol, the regeneration treatment liquid volume is reduced by 24%, the cyclic absorption EQ is improved by 28.2%, the desorption rate DE is improved by 20.8%, and the regeneration energy consumption Q is reduced by 32.1%. The viscosity of the absorption solution without cyclohexanol added was 11.2cP, and the viscosity of the rich liquid phase in this example was 28.9cP, but it was still small.
Example 12
Mixing N, N-di (2-hydroxypropyl) piperazine (HPP), N-hydroxyethyl piperazine (HEP), 1, 7-heptanediol and water, and adding boric acid to obtain a mixture for trapping SO 2 The absorbent of (1). What is neededIn the obtained absorbent, the mass fraction of HPP is 25.5%, the mass fraction of HEP is 4.5%, the mass fraction of 1, 7-heptanediol is 30%, the mass fraction of boric acid is 0.5%, and the balance is water.
Will contain SO 2 The simulated flue gas with the concentration of 12.3 percent is introduced into 100g of absorbent at the flow rate of 1.5L/min, the absorption temperature is 45 ℃, and the absorption time is 180min. Absorption of SO 2 The absorbent forms liquid-liquid two phases, the lower water phase accounts for 77.5% of the total volume, and the lower water phase and the upper water phase are SO 2 Is 9.45, SO of the absorbent 2 The absorption was 1.089mol/mol amine. SO is added 2 Desorbing and regenerating the rich phase at 105 deg.C for 180min 2 Has a cyclic absorption EQ of 0.55mol/mol amine, SO 2 The desorption rate was 80.2%.
Compared with a homogeneous absorbent without 1, 7-heptanediol, the regeneration treatment liquid amount is reduced by 23%, the cyclic absorption amount EQ is improved by 20.2%, the desorption rate DE is improved by 25.6%, and the regeneration energy consumption Q is reduced by 22.6%. The viscosity of the absorption solution without 1, 7-heptanediol added was 12.1cP, and the viscosity of the rich liquid phase of this example was 29.5cP, but was still small.
Example 13
Mixing N, N-bis (2-hydroxyethyl) piperazine (BHEP), N-hydroxyethyl piperazine (HEP), N-amyl alcohol and water, and adding boric acid to prepare the compound for trapping SO 2 The absorbent of (1). In the obtained absorbent, the mass fraction of BHEP was 24%, the mass fraction of HEP was 6%, the mass fraction of n-pentanol was 25%, the mass fraction of boric acid was 3.52%, and the balance was water.
Will contain SO 2 The simulated flue gas with the concentration of 11.2 percent is introduced into 100g of absorbent at the flow rate of 1.5L/min, the absorption temperature is 25 ℃, and the absorption time is 180min. Absorption of SO 2 The absorbent forms liquid-liquid two phases, wherein the lower water phase accounts for 83.6 percent of the total volume, and the lower water phase and the upper water phase are SO 2 Is 8.1, SO of the absorbent 2 The absorption was 0.8023mol/mol amine. Adding SO 2 Desorbing and regenerating the rich phase at 105 deg.C for 180min 2 Has a cyclic absorption EQ of 0.65mol/mol amine, SO 2 The desorption rate was 76%.
Compared with the homogeneous absorbent without n-pentanol, the regenerated treating fluid amount of the embodiment is reduced by 16%, the cyclic absorption EQ is improved by 26.2%, the desorption DE is improved by 20.8%, and the regeneration energy consumption Q is reduced by 32.1%. The absorption liquid without n-pentanol added had a viscosity of 10.5cP, and the rich liquid phase of this example had a viscosity increase of 27.5cP, which was slightly increased but still small.
Example 14 Cyclic absorption Desorption
Mixing N, N-di (2-hydroxyethyl) piperazine (BHEP), N-hydroxyethyl piperazine (HEP), N-butanol and water, and adding boric acid to obtain the product for trapping SO 2 The absorbent of (1). In the obtained absorbent, the mass fraction of BHEP was 22.5%, the mass fraction of HEP was 2.5%, the mass fraction of n-butanol was 25%, the mass fraction of boric acid was 3.52%, and the balance was water.
Will contain SO 2 The simulated flue gas with the concentration of 8.0 percent is introduced into 100g of absorbent, the flow rate of the simulated flue gas is 1.2L/min, the absorption temperature is 25 ℃, and the absorption time is 150min. Absorption of SO 2 The absorbent forms liquid-liquid two phases, the lower aqueous phase accounts for 77.3 percent of the total volume, and the lower aqueous phase and the upper aqueous phase are SO 2 Is 13.12, SO of the absorbent 2 The absorption was 1.103mol/mol amine. Adding SO 2 Desorbing and regenerating the rich phase at 105 deg.C for 180min 2 Has a cyclic absorption EQ of 0.615mol/mol amine, SO 2 The desorption rate was 86.9%.
And mixing the desorbed and regenerated amine liquid with the upper water for cyclic absorption. After 4 times of circulating absorption, the lower water phase accounts for 79.2 percent of the total volume, and the lower water phase and the upper water phase contain SO 2 Concentration ratio of (3) to (3) SO of the absorbent 2 The absorption amount is 0.905mol/mol of amine, SO 2 The cyclic absorption EQ of (1) is 0.695mol/mol amine, SO 2 The desorption rate was 98.1%.
Compared with a homogeneous absorbent without n-butanol, the regeneration treatment liquid amount is reduced by 21%, the cyclic absorption amount EQ is improved by 25.8%, the desorption rate DE is improved by 35.6%, and the regeneration energy consumption Q is reduced by 44.1%. The viscosity of the absorption solution without n-butanol addition was 8.5cP, and the viscosity of the rich liquid phase of this example was 28.6cP, but was still small.
The cyclic load of the liquid-liquid phase change absorbent is larger than that of a homogeneous absorbent, which shows that the liquid-liquid phase change absorbent has good regeneration performance and can obviously reduce regeneration energy consumption, and the water system phase change absorbent has wide application prospect.

Claims (10)

1. Organic amine-alcohol water system SO 2 The liquid-liquid phase change absorbent is characterized by comprising the following components:
10-30 parts of piperazine organic amine, 5-60 parts of phase splitting agent and 0.1-10 parts of phase change additive; the piperazine organic amine contains an alkyl hydroxyl group, and the alkyl hydroxyl group is selected from one or two of hydroxyethyl or hydroxypropyl; the phase separation agent is selected from one or more than two of C4-C7 alcohols, and the phase change assistant is selected from inorganic acid or organic acid.
2. The liquid-liquid phase change absorbent of claim 1, wherein the liquid-liquid phase change absorbent comprises the following components: 15-30 parts of piperazine organic amine, 10-45 parts of phase separation agent and 0.1-5 parts of phase change assistant.
3. The liquid-liquid phase change absorbent according to claim 1 or 2, wherein the piperazine-based organic amine is one or more selected from N-hydroxyethylpiperazine, N-bis (2-hydroxyethyl) piperazine, N-bis (2-hydroxypropyl) piperazine, and N-hydroxyethyl-N-hydroxypropylpiperazine.
4. The liquid-liquid phase change absorbent according to claim 3, wherein the piperazine-based organic amine contains at least N-hydroxyethyl piperazine.
5. The liquid-liquid phase transition absorbent according to any one of claims 1 to 4, wherein the phase-separating agent is selected from one or more of n-butanol, n-pentanol, s-pentanol, cyclohexanol, or 1, 7-heptanediol.
6. The liquid-liquid phase change absorbent according to any one of claims 1 to 5, wherein the phase change aid is one or more selected from sulfuric acid, phosphoric acid, hydrochloric acid, and boric acid.
7. The organic amine-alcohol aqueous system SO according to any one of claims 1 to 6 2 The preparation method of the liquid-liquid phase change absorbent is characterized by comprising the following steps:
and adding the raw materials containing the piperazine organic amine, the phase-splitting agent and the phase-change assistant into water, and dissolving to obtain the liquid-liquid phase-change absorbent.
8. Trapped SO 2 The method is characterized by comprising the following steps:
(1) The absorption process comprises the following steps: will contain SO 2 Is mixed with the liquid-liquid phase change absorbent according to any one of claims 1 to 6, and after the absorption reaction, the absorption liquid is rapidly divided into a lower aqueous phase and an upper aqueous phase;
(2) And (3) desorption process: heating and desorbing the lower water phase, mixing the lean solution obtained after desorption with the upper water phase obtained in the step (1), and recycling the lean solution as an absorbent.
9. The method according to claim 8, wherein the temperature during the absorption reaction is 20-50 ℃ and the temperature during the desorption reaction is 80-120 ℃, preferably 100-110 ℃.
10. Organic amine-alcohol aqueous SO system according to any one of claims 1 to 6 2 The liquid-liquid phase change absorbent is applied to the field of flue gas desulfurization.
CN202211273455.1A 2022-10-18 2022-10-18 Organic amine-alcohol aqueous sulfur dioxide liquid-liquid phase change absorbent and preparation method and application thereof Pending CN115518493A (en)

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