CN113231036A - Supported adsorbent for removing ultralow-concentration hydrogen sulfide and preparation method thereof - Google Patents
Supported adsorbent for removing ultralow-concentration hydrogen sulfide and preparation method thereof Download PDFInfo
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- CN113231036A CN113231036A CN202110555689.4A CN202110555689A CN113231036A CN 113231036 A CN113231036 A CN 113231036A CN 202110555689 A CN202110555689 A CN 202110555689A CN 113231036 A CN113231036 A CN 113231036A
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
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- 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
- B01D53/02—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 adsorption, e.g. preparative gas chromatography
- B01D53/04—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 adsorption, e.g. preparative gas chromatography with stationary adsorbents
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
- B01J20/28057—Surface area, e.g. B.E.T specific surface area
- B01J20/28064—Surface area, e.g. B.E.T specific surface area being in the range 500-1000 m2/g
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
- B01J20/28057—Surface area, e.g. B.E.T specific surface area
- B01J20/28066—Surface area, e.g. B.E.T specific surface area being more than 1000 m2/g
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
- B01J20/28069—Pore volume, e.g. total pore volume, mesopore volume, micropore volume
- B01J20/28071—Pore volume, e.g. total pore volume, mesopore volume, micropore volume being less than 0.5 ml/g
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01D2257/00—Components to be removed
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- B01D2257/304—Hydrogen sulfide
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Abstract
The invention discloses a load type adsorbent for removing ultralow-concentration hydrogen sulfide and a preparation method thereof. Alkali treatment is carried out on the activated carbon through alkali solution, and then an impregnation method is adopted to load the active component on the activated carbon subjected to the alkali treatment. The active components of the supported adsorbent can be uniformly dispersed on the surface of the active carbon, and the supported adsorbent has strong capability of removing ultralow-concentration hydrogen sulfide from coal gas tail gas.
Description
Technical Field
The invention belongs to the technical field of hydrogen sulfide adsorption, and particularly relates to a supported adsorbent for removing ultralow-concentration hydrogen sulfide and a preparation method thereof.
Background
After the waste gas generated by coal gas is washed and purified by low-temperature methanol, more than 90 percent of the waste gas is carbon dioxide, and meanwhile, hydrogen sulfide with ultralow concentration exists. The hydrogen sulfide is a highly toxic gas with the odor of the rotten eggs and has strong irritation. Poisoning and even death can occur when humans come into contact with certain concentrations of hydrogen sulfide, which, in addition, can corrode piping and equipment, resulting in catalyst poisoning. The removal of the hydrogen sulfide with ultra-low concentration in the coal gas tail gas is beneficial to the health of human bodies and the safe production. Because the conventional normal-temperature desulfurization method is mostly based on acid-base reaction to remove hydrogen sulfide, and carbon dioxide and hydrogen sulfide are both acid gases, the inhibition effect of carbon dioxide in the desulfurization process cannot be avoided, and the desulfurization selectivity is poor. Therefore, the development of a high-selectivity desulfurizing agent for removing ultralow-concentration hydrogen sulfide in coal gas tail gas is needed.
At present, the common industrial normal temperature desulfurization methods are mainly classified into absorption methods and adsorption methods. The absorption process is mainly to absorb hydrogen sulfide into the liquid phase by using an alcohol amine solution. The absorption method has large treatment capacity, but has low desulfurization precision, and the treated gas has high content of hydrogen sulfide and can cause equipment corrosion. The adsorption method mainly utilizes molecular sieves (Steijns M, MarsP. Industrial & Engineering chemical Product Research & Development,2017,16(1):103-10.), activated carbon (Mochizuki T, Kubota M, Matsuda H, et al. Fuel Processing Technology,2016,144: 164. quadrature. 169.) and the like to adsorb hydrogen sulfide, overcomes the defect of low desulfurization precision of the absorption method, and is one of the common fine desulfurization technologies. Among them, the activated carbon adsorbent is widely used due to its advantages of low cost, easy regeneration, etc. However, the common activated carbon has poor adsorption selectivity, for example, patent CN202010648368.4 discloses a preparation method of activated carbon with basic functional groups, but it is only suitable for removing hydrogen sulfide in air environment, and cannot effectively remove ultralow concentration hydrogen sulfide in coal gas tail gas.
Disclosure of Invention
Aiming at the defect of poor selectivity of the existing hydrogen sulfide adsorbent, the invention provides a method for removing a load type adsorbent. The adsorbent prepared by the invention has the synergistic effect of the tertiary amine ionic liquid, the tertiary amine and the activated carbon carrier, has higher hydrogen sulfide adsorption capacity and adsorption selectivity, is simple in preparation process, and does not corrode equipment. The invention also provides a preparation method of the supported adsorbent.
The technical scheme of the invention is as follows: a load type adsorbent for removing ultralow-concentration hydrogen sulfide is characterized in that activated carbon treated by alkali is used as a carrier, and tertiary amine ionic liquid and tertiary amine are used as active components; wherein the loading capacity of the tertiary amine ionic liquid is 1-10% of the mass of the activated carbon subjected to alkali treatment; the loading amount of the tertiary amine is 10-40% of the mass of the alkali-treated activated carbon; the specific surface area of the activated carbon after alkali treatment is 680-1010m2Per g, pore volume of 0.32-0.49cm3/g。
Preferably, the cation of the tertiary amine ionic liquid is any one of triethanolamine, N-methyldiethanolamine or N, N, N ', N' -tetramethylhexamethylenediamine in tertiary amine, and the anion is any one of formic acid, acetic acid or benzoic acid in organic acid; the tertiary amine is one of triethanolamine, N-methyldiethanolamine or N, N, N ', N' -tetramethyl hexanediamine.
The invention also provides a method for preparing the supported adsorbent, which comprises the following steps:
(1) preparation of tertiary amine ionic liquid: respectively dissolving tertiary amine and organic acid in water, adding the organic acid solution into the tertiary amine solution at 40-80 ℃, stirring for 12-24h, evaporating to remove water, and drying in vacuum to obtain tertiary amine ionic liquid;
(2) preparation of alkali-treated activated carbon: adding activated carbon into the alkali solution, stirring for alkali treatment, washing the stirred activated carbon until the filtrate is neutral, and drying to obtain alkali-treated activated carbon;
(3) preparation of the supported adsorbent: weighing a certain mass of tertiary amine and tertiary amine ionic liquid according to the loading capacity, dissolving the tertiary amine and tertiary amine ionic liquid in an organic solvent, adding the alkali-treated active carbon obtained in the step (2) into the solution, stirring, and drying to obtain the supported adsorbent.
Preferably, the molar ratio of the tertiary amine to the organic acid in the step (1) is (1-1.5): 1. Preferably, the evaporation temperature in the step (1) is 70-100 ℃; the vacuum drying temperature is 80-120 deg.C, and the drying time is 12-24 h.
Preferably, the alkali solution in the step (2) is NaOH solution or NaHCO solution3One of a solution or ammonia; the mass concentration of the alkali solution is 5-15%; the ratio of the volume of the alkali solution to the mass of the activated carbon is (10-50) mL/g. Preferably, the stirring temperature in the step (2) is 25-85 ℃, and the stirring time is 6-12 h; the drying temperature is 80-120 ℃, and the drying time is 8-12 h.
Preferably, the organic solvent in the step (3) is one of methanol, ethanol or ethylene glycol; the ratio of the volume of the organic solvent to the mass of the alkali-treated activated carbon carrier is (10-30) mL/g.
Preferably, the stirring time in the step (3) is 4-8h, and the stirring temperature is 20-70 ℃; the drying temperature is 70-100 deg.C, and the drying time is 3-9 h.
The invention provides a method for removing trace hydrogen sulfide in coal gas tail gas by using the adsorbent, which comprises the following steps: mixing carbon dioxide and hydrogen sulfide according to a certain proportion to prepare mixed gas, filling an adsorbent into an adsorption tube of a fixed bed device, introducing the mixed gas to carry out an adsorption experiment, and calculating the penetration adsorption amount when the concentration of a hydrogen sulfide outlet reaches a penetration point of 0.5 ppm; wherein the concentration of hydrogen sulfide in the mixed gas is 3-20 ppm; the adsorption temperature is 20-60 ℃; the space velocity is 8000-20000 mL/g.h.
The supported adsorbent prepared by the invention has rich pore channel structures of the active carbon, is beneficial to the loading of active components, and can also reduce the mass transfer resistance of hydrogen sulfide. The alkali treated active carbon carrier increases the number of alkaline sites on the surface of the active carbon. The tertiary amine group does not have active hydrogen ions and does not react with carbon dioxide in a dry environment, so that the removal of ultralow-concentration hydrogen sulfide in the coal gas tail gas can be realized by introducing the tertiary amine group into the adsorbent. The tertiary amine and the tertiary amine ionic liquid are loaded into the pore channel of the activated carbon, so that the tertiary amine groups are uniformly dispersed, the contact probability of the tertiary amine groups and hydrogen sulfide is increased, and the adsorption capacity and selectivity of the adsorbent are improved. And the addition of the tertiary amine ionic liquid improves the thermal stability of the adsorbent. The active carbon is pretreated by the alkali solution, and the tertiary amine and tertiary amine ionic liquid are loaded into the active carbon pore channel by adopting an impregnation method, so that the adsorption capacity and the adsorption selectivity of the adsorbent are improved, and the adsorbent has the advantages of easiness in preparation, good stability and the like.
Has the advantages that:
(1) the adsorbent prepared by the invention has high tertiary amine group content, uniform dispersion, good desulfurization efficiency and high selectivity.
(2) The invention adopts alkali solution to modify the active carbon, and increases the number of surface alkaline functional groups.
(3) The tertiary amine ionic liquid is prepared and loaded into the pore channel of the alkali-treated active carbon, and the thermal stability of the adsorbent is favorably improved.
(4) The invention adopts an impregnation method to load the active components on the active carbon, and the preparation process is simple.
Detailed Description
In order that the objects and advantages of the invention will become more apparent, the invention is further illustrated by the following specific examples. The specific embodiments described herein are merely illustrative of the present invention and do not specifically limit the scope of the invention.
Example 1
(1) 11.916g of N-methyldiethanolamine (0.1mol) and 4.603g of formic acid (0.1mol) are weighed and respectively dissolved in 100mL of water, the formic acid solution is added into the N-methyldiethanolamine solution, the mixture is continuously stirred for 12h at 40 ℃, water is removed by evaporation at 70 ℃, and the tertiary amine ionic liquid is obtained by vacuum drying at 80 ℃ for 12 h.
(2) 4g of activated carbon was weighed into 200mL of 15 wt% ammonia water and stirred at 25 ℃ for 12 hours. And (4) filtering and washing the stirred activated carbon to be neutral, and drying at 120 ℃ for 8h to obtain the alkali-treated activated carbon. The specific surface area of the activated carbon after alkali treatment is 680m2G, pore volume 0.32cm3/g。
(3) 0.15g of the tertiary amine ionic liquid obtained in the step (1) and 0.45g of triethanolamine are weighed and dissolved in 15mL of ethanol, 1.5g of the solid obtained in the step (2) is weighed and added into the solution, stirred for 4h at 20 ℃, and dried for 3h at 100 ℃ to obtain the adsorbent 1.
(4) Weighing 1.114g of the adsorbent 1 for removing trace hydrogen sulfide in the coal gas tail gas, wherein the adsorption temperature is 30 ℃, the concentration of the hydrogen sulfide is 5ppm, and the space velocity is 14000 mL/g.h. When the outlet concentration reached 0.5ppm, the breakthrough adsorption capacity of finished adsorbent 1 was 2.233 mg/g.
Example 2
(1) 22.378g of triethanolamine (0.15mol) and 6.005g of acetic acid (0.1mol) are weighed and respectively dissolved in 100mL of water, the acetic acid solution is added into the triethanolamine solution, the stirring is continued for 24h at 80 ℃, the water is removed by evaporation at 80 ℃, and the tertiary amine ionic liquid is obtained after vacuum drying for 24h at 120 ℃.
(2) 4g of activated carbon were weighed into 40mL of 10 wt% NaOH solution and stirred at 85 ℃ for 6 h. And (4) filtering and washing the stirred activated carbon to be neutral, and drying at 80 ℃ for 12h to obtain the alkali-treated activated carbon. The specific surface area of the activated carbon after alkali treatment is 1010m2Per g, pore volume 0.49cm3/g。
(3) 0.015g of the tertiary amine ionic liquid obtained in the step (1) and 0.6g of N, N, N ', N' -tetramethylhexamethylenediamine are weighed and dissolved in 45mL of methanol, 1.5g of the solid obtained in the step (2) is weighed and added into the solution, the mixture is stirred for 8h at 70 ℃, and the mixture is dried for 9h at 70 ℃ to obtain the adsorbent 2.
(4) 0.78g of adsorbent 2 is weighed to remove trace hydrogen sulfide in the coal gas tail gas, the adsorption temperature is 20 ℃, the concentration of the hydrogen sulfide is 3ppm, and the space velocity is 20000 mL/g.h. When the exit concentration reached 0.5ppm, the breakthrough adsorption capacity of finished adsorbent 2 was 3.429 mg/g.
Example 3
(1) 17.231g of N, N, N ', N' -tetramethylhexanediamine (0.1mol) and 12.212g of benzoic acid (0.1mol) are weighed and respectively dissolved in 100mL, the benzoic acid solution is added into the N, N, N ', N' -tetramethylhexanediamine solution, the mixture is continuously stirred for 18h at the temperature of 60 ℃, water is removed by evaporation at the temperature of 90 ℃, and the tertiary amine ionic liquid is obtained by vacuum drying for 20h at the temperature of 100 ℃.
(2) 4g of activated charcoal was weighed into 100mL of 5 wt% NaHCO3Stirring the solution at 65 ℃ for 9h, filtering and washing the stirred activated carbon to be neutral, and drying the activated carbon at 100 ℃ for 10h to obtain the alkali-treated activated carbon. The specific surface area of the activated carbon after alkali treatment is 769m2G, pore volume 0.36cm3/g。
(3) 0.1g of the tertiary amine ionic liquid obtained in the step (1) and 0.2g of methyldiethanolamine are weighed and dissolved in 30mL of ethylene glycol, 2g of the solid obtained in the step (2) is weighed and added into the solution, the mixture is stirred for 6h at 40 ℃, and the mixture is dried for 6h at 90 ℃ to obtain the adsorbent 3.
(4) Weighing 1.95g of the adsorbent 3 for removing trace hydrogen sulfide in the coal gas tail gas, wherein the adsorption temperature is 40 ℃, the concentration of the hydrogen sulfide is 20ppm, and the space velocity is 8000 mL/g.h. When the outlet concentration reached 0.5ppm, the breakthrough adsorption capacity of finished adsorbent 3 was 1.840 mg/g.
Example 4
(1) 17.874g of N-methyldiethanolamine (0.15mol) and 6.005g of acetic acid (0.1mol) are weighed and respectively dissolved in 100mL of water, the acetic acid solution is added into the N-methyldiethanolamine solution, the mixture is continuously stirred for 15h at 70 ℃, water is removed by evaporation at 100 ℃, and the tertiary amine ionic liquid is obtained by vacuum drying at 90 ℃ for 18 h.
(2) Weighing 4g of activated carbon, adding the activated carbon into 50mL of 10 wt% ammonia water, stirring at 45 ℃ for 12h, filtering and washing the stirred activated carbon to be neutral, and drying at 90 ℃ for 12h to obtain the alkali-treated activated carbon. The specific surface area of the activated carbon after alkali treatment is 835m2Per g, pore volume 0.43cm3/g。
(3) 0.075g of the tertiary amine ionic liquid obtained in the step (1) and 0.3g of triethanolamine are weighed and dissolved in 25mL of ethanol, 1.5g of the solid obtained in the step (2) is weighed and added into the solution, stirred for 7h at 40 ℃, and dried for 5h at 80 ℃ to obtain the adsorbent 4.
(4) Weighing 1.3g of adsorbent 4 for removing trace hydrogen sulfide in the coal gas tail gas, wherein the adsorption temperature is 50 ℃, the concentration of the hydrogen sulfide is 15ppm, the space velocity is 12000 mL/g.h, and when the outlet concentration reaches 0.5ppm, the penetrating adsorption capacity of the finished adsorbent 4 is 2.804 mg/g.
Claims (9)
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