CN112337285A - Iron-based ion desulfurization solution and regeneration method thereof - Google Patents

Iron-based ion desulfurization solution and regeneration method thereof Download PDF

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CN112337285A
CN112337285A CN201910730764.9A CN201910730764A CN112337285A CN 112337285 A CN112337285 A CN 112337285A CN 201910730764 A CN201910730764 A CN 201910730764A CN 112337285 A CN112337285 A CN 112337285A
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iron
ionic liquid
based ionic
desulfurization
solution
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余江
张丽
刘雪珂
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Anqing Beihuada Science And Technology Park Co ltd
Beijing University of Chemical Technology
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Anqing Beihuada Science And Technology Park Co ltd
Beijing University of Chemical Technology
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D53/00Separation 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
    • B01D53/34Chemical or biological purification of waste gases
    • B01D53/74General processes for purification of waste gases; Apparatus or devices specially adapted therefor
    • B01D53/77Liquid phase processes
    • B01D53/78Liquid phase processes with gas-liquid contact
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D53/00Separation 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
    • B01D53/34Chemical or biological purification of waste gases
    • B01D53/46Removing components of defined structure
    • B01D53/48Sulfur compounds
    • B01D53/52Hydrogen sulfide
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D53/00Separation 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
    • B01D53/34Chemical or biological purification of waste gases
    • B01D53/73After-treatment of removed components
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D53/00Separation 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
    • B01D53/34Chemical or biological purification of waste gases
    • B01D53/74General processes for purification of waste gases; Apparatus or devices specially adapted therefor
    • B01D53/86Catalytic processes
    • B01D53/8603Removing sulfur compounds
    • B01D53/8612Hydrogen sulfide
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D2251/00Reactants
    • B01D2251/10Oxidants
    • B01D2251/102Oxygen
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D2251/00Reactants
    • B01D2251/60Inorganic bases or salts

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Abstract

The invention discloses an iron-based ion doctor solution, which relates to the technical field of doctor solutions and is provided based on the problem of poor regeneration effect of the existing iron-based ion doctor solution, and the iron-based ion doctor solution is mainly prepared from the following raw materials: the ionic liquid comprises an iron-based ionic liquid, an organic solvent and a copper-based ionic liquid, wherein the iron-based ionic liquid and the organic solvent are mixed to form a composite ionic liquid, the volume ratio of the iron-based ionic liquid to the organic solvent is 30:1-20, and the volume ratio of the composite ionic liquid to the copper-based ionic liquid is 8: 1. The invention also provides a regeneration method of the iron-based ion desulfurization solution; the invention has the beneficial effects that: the transition metal Cu (II) is introduced into the desulfurization solution, and CuS precipitate is produced in the desulfurization process to promote a desulfurization system to carry out H reaction2Absorption of S is as followsThe method is beneficial to the oxidation of CuS by Fe (III) -IL to convert into a sulfur product, and simultaneously cuprous ions are generated in the reaction process to catalyze the conversion process of Fe (II) to Fe (III), thereby improving the regeneration effect.

Description

Iron-based ion desulfurization solution and regeneration method thereof
Technical Field
The invention relates to the technical field of desulfurization solutions, and particularly relates to an iron-based ion desulfurization solution and a regeneration method thereof.
Background
The iron-based ionic liquid is a green environment-friendly non-aqueous phase wet oxidation desulfurizer, has the advantages of good thermal stability, low saturated vapor pressure, excellent catalytic oxidation performance, no secondary pollution, high sulfur capacity and the like, and is widely applied to the purification of sulfur-containing gas.
The iron-based ionic liquid has a good desulfurization effect in the aspect of absorbing hydrogen sulfide oxide, the pH is not required to be adjusted in the desulfurization process, and multiple side reactions are not generated. The desulfurization process of the iron-based ionic liquid is realized by the following ways:
2Bmin[Fe(III)xCly]+H2S→2H{Bmin[Fe(II)xCly]}+S↓
4H{Bmin[Fe(II)xCly]}+O2→4BminFe(III)xCly]+2H2O
in the reaction process, Fe (III) is reduced into Fe (II), the viscosity of a desulfurization system is further increased due to the generation of Fe (II), the gas-liquid mass transfer effect is poor, and the desulfurization effect and the regeneration effect are not ideal. In the prior art, an organic solvent is added into an iron-based ionic liquid to form a composite ionic liquid, so that the viscosity of a desulfurization system is reduced, and the gas-liquid mass transfer process is enhanced.
The iron-based ionic liquid is strongly acidic, and after a certain amount of organic solvent is added, the viscosity and acidity of a desulfurization system are simultaneously reduced, and H is promoted2The S gas is absorbed, the gas-liquid mass transfer process is strengthened, and the desulfurization efficiency is obviously improved. The patent CN201710505891.X discloses a compound ionic liquid desulfurizer and a preparation method thereof, and the compound ionic liquid desulfurizer comprises 4-25% of physical solvent and the balance Fe-IL liquid by mass percent, and can effectively improve the pH and viscosity of the compound desulfurizer and promote the absorption rate of Fe-IL in the desulfurizer to hydrogen sulfide by compounding the organic solvent and the Fe-IL liquid.
The regeneration process of the desulfurization solution is enhanced to a certain extent by introducing the organic solvent into the iron-based ionic liquid, but the required regeneration time is still longer and the regeneration effect is not ideal. In order to meet the green chemical requirements of sustainable development and realize the recycling of the iron-based ionic liquid in the desulfurization process, the research on the regeneration process of the iron-based ionic liquid is essential.
At present, the regeneration technology of the desulfurization solution mainly comprises a biological method, an electrolytic method and a chemical oxidation method. Because the temperature, the pH, the Fe (II) concentration and the like all influence the growth of strains, the requirement of the biological method regeneration desulfurization solution on the process condition is harsh, so that the investment cost is increased, and the industrial application range is narrowed; the viscosity, the conductivity, the apparent diffusion coefficient and other electrochemical properties of active particles of the iron-based ionic liquid are not ideal and are not suitable for direct electrolytic regeneration, the cost is greatly increased due to the selection of the platinum electrode, the platinum electrode is difficult to be applied to the actual industrial process in a large range, in addition, the research reports that the desulfurization-electrolysis process of the system is further promoted to industrialization by carefully discussing the electrode from the aspects of electrode type, optimization and the like and selecting a proper electrode are few, and the electrolytic regeneration process is not mature; the air/oxygen regeneration desulfurization solution is the earliest and most common method, and although no peroxidation side reaction occurs in the chemical oxidation regeneration process, the required cost is low, and the process is simple, the solubility of oxygen in a composite system is low, so that the regeneration time is long, and the regeneration efficiency is low.
Disclosure of Invention
One of the technical problems to be solved by the invention is that the existing iron-based ion desulfurization solution has poor regeneration effect, and the iron-based ion desulfurization solution is provided.
The invention solves the technical problems through the following technical means:
the invention provides an iron-based ion desulfurization solution which is mainly prepared from the following raw materials: the ionic liquid comprises an iron-based ionic liquid, an organic solvent and a copper-based ionic liquid, wherein the iron-based ionic liquid and the organic solvent are mixed to form a composite ionic liquid, the volume ratio of the iron-based ionic liquid to the organic solvent is 30:1-20, and the volume ratio of the composite ionic liquid to the copper-based ionic liquid is 8: 1;
the organic solvent is one of polyethylene glycol dimethyl ether, 1, 3-dimethyl-2-imidazolidinone, dimethylformamide and dimethylacetamide.
Has the advantages that: the desulfurization solution is compounded with the organic solvent, so that the acidity and viscosity of a desulfurization system are reduced, the gas-liquid mass transfer process is enhanced, and H is promoted2S and O2The gas absorption effectively improves the desulfurization effect and the regeneration effect.
The desulfurizing liquid of the present invention has transition metal Cu (II) introduced, and the Cu (II) may be reacted with S in the desulfurizing stage2+CuS precipitate is generated and undergoes redox reaction with active Fe (III) to promote desulfurization system to react with H2S is absorbed, so that the desulfurization efficiency is further improved;
the invention introduces transition metal Cu (II) into the desulfurization solution, produces CuS precipitate in the desulfurization process and promotes the desulfurization system to carry out H precipitation2The absorption of S is simultaneously beneficial to the conversion of the CuS oxidized by Fe (III) -IL into a sulfur product, and cuprous ions are generated in the reaction process to catalyze the conversion process from Fe (II) to Fe (III), so that the regeneration effect is improved. Further improving the regeneration effect and realizing the recycling of the iron-based ionic liquid.
Preferably, the preparation method of the iron-based ionic liquid comprises the following steps:
(1) mixing and stirring 1-butyl-3-methylimidazole chloride and ferric chloride hexahydrate in a molar ratio of 1:2 for 24 hours;
(2) standing and layering the mixed product in the step (1), and taking the upper liquid by using a separating funnel;
(3) and (3) drying the liquid in the step (2) at 80 ℃ for 12h to obtain the iron-based ionic liquid.
Preferably, the organic solvent is polyethylene glycol dimethyl ether.
Preferably, the volume ratio of the iron-based ionic liquid to the polyethylene glycol dimethyl ether is 3: 1.
Preferably, the preparation method of the copper-based ionic liquid comprises the following steps:
(1) mixing and stirring 1-butyl-3-methylimidazole chloride and copper chloride dihydrate in a molar ratio of 1:0.01 for 12 hours;
(2) and (2) drying the mixed product in the step (1) to obtain the copper-based ionic liquid.
Preferably, the drying temperature is 80 ℃ and the drying time is 12 h.
Has the advantages that: the imidazole copper ionic liquid is directly added into the composite ionic liquid in the form of imidazole copper ionic liquid, which is equivalent to only introducing Cu (II) into the original system, and directly removing the influence of anions.
The second technical problem to be solved by the invention is that the existing iron-based ion desulfurization solution has poor regeneration effect, and provides a regeneration method of the iron-based ion desulfurization solution.
A regeneration method of an iron-based ion desulfurization solution comprises the following steps: the iron-based ion desulfurization solution absorbs H2And (S) introducing oxygen-containing gas.
Preferably, the oxygen-containing gas is oxygen.
Preferably, the oxygen flow rate is 50mL/min, and the reaction temperature is 30 ℃.
Preferably, said introduced H2The flow rate of S was 40 mL/min.
Preferably, the desulfurization time of the iron-based ionic desulfurization solution is 7 hours.
Has the advantages that: in the invention, transition metal Cu (II) is introduced into the desulfurization solution to catalyze Fe (II) to be oxidized into Fe (III), thereby shortening the regeneration time, improving the regeneration effect and realizing the recycling of the iron-based ionic liquid.
The invention has the advantages that:
(1) the desulfurization solution is compounded with the organic solvent, so that the acidity and viscosity of a desulfurization system are reduced, the gas-liquid mass transfer process is enhanced, and H is promoted2S and O2The gas absorption effectively improves the desulfurization effect and the regeneration effect;
(2) the desulfurizing liquid of the present invention has transition metal Cu (II) introduced, and the Cu (II) may be reacted with S in the desulfurizing stage2+CuS precipitate is generated and undergoes redox reaction with active Fe (III) to promote desulfurization system to react with H2S is absorbed, so that the desulfurization efficiency is further improved;
(3) the invention introduces transition metal Cu (II) into the desulfurization solution, produces CuS precipitate in the desulfurization process and promotes the desulfurization system to carry out H precipitation2S absorption, while facilitating the oxidative CuS conversion of Fe (III) -ILThe sulfur product simultaneously generates cuprous ions in the reaction process to catalyze the conversion process of Fe (II) to Fe (III), thereby improving the regeneration effect and realizing the recycling of the iron-based ionic liquid.
Drawings
FIG. 1 is a schematic structural diagram of a regeneration experimental apparatus in example 1 of the present invention;
FIG. 2 is a graph showing the results of the determination of the regeneration effect of the iron-based ionic liquid and the dimethyl glycol ether in the comparative example 1 according to the present invention under different mixing ratios;
FIG. 3 is a viscosity measurement result of the iron-based ionic liquid and the polyethylene glycol dimethyl ether in different proportions in comparative example 1;
FIG. 4 is a graph showing the results of measurement of the regeneration effect of the iron-based ion desulfurization solution in example 3 of the present invention;
FIG. 5 is a graph showing the results of measurement of the regeneration effect of the iron-based ion desulfurization solution in example 4 of the present invention;
in the figure: an oxygen cylinder 1; a gas flow meter 2; a reactor 3; a glass sand core 4; and an iron stand 5.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are some embodiments of the present invention, but not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
Regeneration experimental apparatus, as shown in fig. 1, including oxygen cylinder 1, gas flowmeter 2, reactor 3, glass psammitolite 4 and iron stand platform 5, reactor 3 places on iron stand platform 5, and reactor 3's lower extreme and oxygen cylinder 1 intercommunication, pipe connection reactor 3 and oxygen cylinder 1, and the centre connects gas flowmeter 2 to do the buffering, is equipped with glass psammitolite 4 in the reactor 3, and gas flowmeter 2 is located reactor 3 and oxygen cylinder 1 centre.
The regeneration method of the desulfurization solution comprises the following steps: and (3) placing the desulfurized liquid into a reactor, opening an oxygen cylinder valve, introducing oxygen, regulating and controlling the oxygen flow to be 50mL/min, and setting the reaction temperature to be 30 ℃ for reaction.
Example 2
Preparation method of iron-based ionic liquid
(1) Mixing and stirring 1-butyl-3-methylimidazole chloride and ferric chloride hexahydrate at a molar ratio of 1:2 at normal temperature for 24 hours;
(2) standing and layering the mixed product in the step (1), and taking the upper liquid by using a separating funnel;
(3) and (3) drying the liquid in the step (2) at 80 ℃ for 12h to obtain the iron-based ionic liquid.
Comparative example 1
Regeneration effect and viscosity measurement of composite ionic liquid
The compound volume ratio of the iron-based ionic liquid to the polyethylene glycol dimethyl ether is 1:0, 6:1, 3:1, 2:1, 1.5:1 and 1:1 respectively, and H with the concentration of 1% is introduced into the compound ionic liquid at the flow rate of 40mL/min at normal temperature2And S, continuously desulfurizing for 7h to obtain composite ionic liquid desulfurization rich liquid with different compound volume ratios, and measuring the regeneration effect of the composite ionic liquid desulfurization rich liquid by using the regeneration device in the embodiment 1, wherein the regeneration effect is not limited to the measurement by using the regeneration device in the embodiment 1, the total reaction time is 3h, the Fe (II) concentrations in different time periods are respectively measured, and the regeneration efficiency is calculated, wherein the regeneration efficiency is (1-the Fe (II) concentration after the reaction/the initial Fe (II) concentration) multiplied by 100%.
Measuring the viscosity of the composite ionic liquid desulfurization rich solution with different compound volumes by adopting an SNB-2 type digital viscometer
The experimental results are as follows: as shown in fig. 2, the regeneration effect of the pure iron-based ionic liquid desulfurization rich solution is the worst; the regeneration effect of the iron-based ionic liquid desulfurization rich solution with the volume ratio of the iron-based ionic liquid to the polyethylene glycol dimethyl ether being 3:1 is best, the regeneration efficiency is 31% when the solution is regenerated for 180min, the compounding ratio of the polyethylene glycol dimethyl ether is continuously increased, and the regeneration effect is reduced.
As shown in figure 3, with the increase of the compounding volume ratio of the polyethylene glycol dimethyl ether, the viscosity of the compounding system is gradually reduced, and O is2The absorption in the compound system belongs to the gas-liquid reaction process, and the reduction of the viscosity is beneficial to O2But at the same time the Fe (II) concentration in the system is reduced, with O2The contact chance of the iron-based ionic liquid/polyethylene glycol dimethyl ether is reduced, so that the content of the polyethylene glycol dimethyl ether in a compound system is not high enough, and the preferable compound volume ratio of the iron-based ionic liquid/the polyethylene glycol dimethyl ether is 3: 1.
Example 3
Preparation method of copper-based ionic liquid
(1) Mixing and stirring 1-butyl-3-methylimidazole chloride and copper chloride dihydrate at a molar ratio of 1:0.01 at normal temperature for 12 hours;
(2) and (2) drying the mixed product in the step (1) at 80 ℃ for 12h to obtain the copper-based ionic liquid.
Example 4
Determination of regeneration effect of iron-based ion desulfurization solution
Compounding the iron-based ionic liquid and the polyethylene glycol dimethyl ether at a volume ratio of 3:1, mixing to obtain a composite ionic liquid, mixing to obtain the iron-based ionic desulfurization liquid, wherein the volume ratio of the composite ionic liquid to the copper-based ionic liquid is 8:1, and introducing 1% H into the iron-based ionic desulfurization liquid at a flow rate of 40mL/min at normal temperature2S, continuously desulfurizing for 7h to obtain an iron-based ion desulfurization rich solution, and measuring the regeneration effect of the iron-based ion desulfurization solution by using the regeneration device in the embodiment 1, but the measurement is not limited to the regeneration device in the embodiment 1.
The experimental results are as follows: as shown in fig. 4, the introduction of Cu (ii) into the composite ionic liquid can improve the regeneration effect of the iron-based ionic liquid, and compared with the composite ionic liquid desulfurization rich liquid in the comparative example 1 in which the volume ratio of the iron-based ionic liquid to the polyethylene glycol dimethyl ether is 3:1, the regeneration efficiency of the iron-based ionic desulfurization liquid prepared in this embodiment can reach 35% when the regeneration time reaches 15min, and can reach 99% when the regeneration time reaches 180min, and the addition of Cu (ii) significantly improves the regeneration effect of the iron-based ionic liquid desulfurization liquid and greatly shortens the regeneration time.
Example 5
Prepared as in example 3Drying the obtained iron-based ion desulfurization solution until the iron-based ion desulfurization solution does not contain water; iron-based ionic liquid catalytic oxidation H2In the process of S, the S is2-Oxidation to elemental sulfur, hydrogen with H+Is present in the system. But in the oxygen regeneration process, there is O2-Generation of ions, so H+Finally with H2The form of O exists in the system. Therefore, the iron-based ionic liquid desulfurization pregnant solution is dried until the iron-based ionic liquid desulfurization pregnant solution does not contain water, and the influence of water on the regeneration of the iron-based ionic liquid desulfurization pregnant solution is examined; the regeneration effect of the dried iron-based ion desulfurization solution prepared in this example was measured.
The experimental results are as follows: as shown in fig. 5, in this example, compared with example 3, within 90min, the regeneration efficiency and the regeneration rate of the aqueous iron-based ionic liquid desulfurization solution are both better than those of the non-aqueous iron-based ionic liquid desulfurization solution, and within 90-180 min, the non-aqueous regeneration efficiency is slightly better than that of the aqueous iron-based ionic liquid desulfurization solution, and it can be seen that the iron-based ionic liquid desulfurization solution contains a small amount of water to promote the regeneration of the iron-based ionic liquid.
Example 6
The oxidation and regeneration reaction process of the iron-based ion desulfurization solution prepared by the invention
2Bmim[Fe(Ⅲ)xCly]+Η2S→2H<Bmim[Fe(Ⅱ)xCly]>+S↓……………………(1)
H2S+Cu(Ⅱ)→2H++CuS↓…………………………………………………(2)
Bmim[Fe(Ⅲ)xCly]+CuS→Bmim[Fe(Ⅱ)xCly]+S↓+Cu(Ⅱ)…………………(3)
Cu(Ⅱ)+CuS+4Cl-→S↓+2CuCl2 -…………………………………………………(4)
Bmim[Fe(Ⅲ)xCly]+CuCl2 -→Bmim[Fe(Ⅱ)xCly]+2Cl-+Cu(Ⅱ)………………(5)
4CuCl2 -+O2+4H+→4Cu(Ⅱ)+8Cl-+2H2O…………………………………(6)
4H<Bmim[Fe(Ⅱ)xCly]>+O2→4Bmim[Fe(Ⅲ)xCly]+2H2O…………………(7)
In the reaction formula, (1) is the iron-based ionic liquid catalytic oxidation H2S; (2) the formulas are Cu (II) and H2S reacts to form CuS precipitate, thereby promoting H2S is absorbed; (3) promoting the oxidation of Fe (III) -IL to CuS for Cu (II); (4) the formula is that Cu (II) promotes CuS to be converted into S, and Cu (I) is generated at the same time; (5) the formula (7) is the regeneration process of the copper-based ionic liquid and the iron-based ionic liquid.
The above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.

Claims (10)

1. An iron-based ionic desulfurization solution, which is characterized in that: the health-care food is mainly prepared from the following raw materials: the ionic liquid comprises an iron-based ionic liquid, an organic solvent and a copper-based ionic liquid, wherein the iron-based ionic liquid and the organic solvent are mixed to form a composite ionic liquid, the volume ratio of the iron-based ionic liquid to the organic solvent is 30:1-20, and the volume ratio of the composite ionic liquid to the copper-based ionic liquid is 8: 1;
the organic solvent is one of polyethylene glycol dimethyl ether, 1, 3-dimethyl-2-imidazolidinone, dimethylformamide and dimethylacetamide.
2. The iron-based ionic doctor solution as claimed in claim 1, wherein: the preparation method of the iron-based ionic liquid comprises the following steps:
(1) mixing and stirring 1-butyl-3-methylimidazole chloride and ferric chloride hexahydrate in a molar ratio of 1:2 for 24 hours;
(2) standing and layering the mixed product in the step (1), and taking the upper liquid by using a separating funnel;
(3) and (3) drying the liquid in the step (2) at 80 ℃ for 12h to obtain the iron-based ionic liquid.
3. The iron-based ionic doctor solution as claimed in claim 1, wherein: the organic solvent is polyethylene glycol dimethyl ether.
4. The iron-based ionic doctor solution as claimed in claim 2, wherein: the volume ratio of the iron-based ionic liquid to the polyethylene glycol dimethyl ether is 3: 1.
5. The iron-based ionic doctor solution as claimed in claim 1, wherein: the preparation method of the copper-based ionic liquid comprises the following steps:
(1) mixing and stirring 1-butyl-3-methylimidazole chloride and copper chloride dihydrate in a molar ratio of 1:0.01 for 12 hours;
(2) and (2) drying the mixed product in the step (1) to obtain the copper-based ionic liquid.
6. The iron-based ionic doctor solution as claimed in claim 5, wherein: the drying temperature is 80 ℃, and the drying time is 12 h.
7. A method for regenerating the iron-based ionic desulfurization solution according to claim 1, characterized in that: the method comprises the following steps: h is introduced into the iron-based ion desulfurization solution2And after S is desulfurized, introducing oxygen-containing gas.
8. The method for regenerating an iron-based ionic desulfurization solution according to claim 7, wherein: the oxygen-containing gas is oxygen.
9. The method for regenerating an iron-based ionic desulfurization solution according to claim 7, wherein: the oxygen flow was 50mL/min and the reaction temperature was 30 ℃.
10. The method for regenerating an iron-based ionic desulfurization solution according to claim 7, wherein: the introduced H2The flow rate of S was 40 mL/min.
CN201910730764.9A 2019-08-08 2019-08-08 Iron-based ion desulfurization solution and regeneration method thereof Pending CN112337285A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113019091A (en) * 2021-03-03 2021-06-25 山东理工大学 Preparation method and application of nonaqueous liquid phase complexing iron-nanofluid
CN113041791A (en) * 2021-03-18 2021-06-29 重庆科技学院 Iron-copper ionic liquid desulfurizing agent, preparation method and desulfurization method

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5705135A (en) * 1993-11-04 1998-01-06 Gas Research Institute Composition and process for the removal of hydrogen sulfide from gaseous streams
CN104117274A (en) * 2013-04-26 2014-10-29 北京化工大学 Combined desulfuration dephosphorization method
CN109045957A (en) * 2018-09-19 2018-12-21 重庆科技学院 A kind of method of transition metal salt reinforcing desulfuration performance
CN109550367A (en) * 2018-12-05 2019-04-02 齐鲁工业大学 A kind of ionic liquid desulphurization system and method

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5705135A (en) * 1993-11-04 1998-01-06 Gas Research Institute Composition and process for the removal of hydrogen sulfide from gaseous streams
CN104117274A (en) * 2013-04-26 2014-10-29 北京化工大学 Combined desulfuration dephosphorization method
CN109045957A (en) * 2018-09-19 2018-12-21 重庆科技学院 A kind of method of transition metal salt reinforcing desulfuration performance
CN109550367A (en) * 2018-12-05 2019-04-02 齐鲁工业大学 A kind of ionic liquid desulphurization system and method

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
张俊丰等: "Fe/Cu体系湿式催化氧化一步高效脱除H2S新方法研究", 《环境科学学报》 *
胡锦超: "基于铁基离子液体的脱硫液组成优化及氧化脱硫性能的研究", 《中国优秀博硕士学位论文全文数据库(硕士) 工程科技I辑》 *

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113019091A (en) * 2021-03-03 2021-06-25 山东理工大学 Preparation method and application of nonaqueous liquid phase complexing iron-nanofluid
CN113041791A (en) * 2021-03-18 2021-06-29 重庆科技学院 Iron-copper ionic liquid desulfurizing agent, preparation method and desulfurization method

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Application publication date: 20210209