CN113893814A - Preparation method of renewable adsorbent for deeply removing hydrogen sulfide - Google Patents

Preparation method of renewable adsorbent for deeply removing hydrogen sulfide Download PDF

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CN113893814A
CN113893814A CN202111366656.1A CN202111366656A CN113893814A CN 113893814 A CN113893814 A CN 113893814A CN 202111366656 A CN202111366656 A CN 202111366656A CN 113893814 A CN113893814 A CN 113893814A
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hydrogen sulfide
powder
parts
adsorbent
renewable
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龚甍
黄伟
仵静
李梦婕
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Xi'an Origin Chemical Technologies Co ltd
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Xi'an Origin Chemical Technologies Co ltd
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    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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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
    • B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
    • B01J20/08—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04 comprising aluminium oxide or hydroxide; comprising bauxite
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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
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    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • 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
    • B01J20/04—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of alkali metals, alkaline earth metals or magnesium
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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
    • B01J20/28014—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 form
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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
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    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/30—Processes for preparing, regenerating, or reactivating
    • B01J20/3021—Milling, crushing or grinding
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    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/30—Processes for preparing, regenerating, or reactivating
    • B01J20/305—Addition of material, later completely removed, e.g. as result of heat treatment, leaching or washing, e.g. for forming pores
    • B01J20/3064—Addition of pore forming agents, e.g. pore inducing or porogenic agents
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/30—Processes for preparing, regenerating, or reactivating
    • B01J20/3071—Washing or leaching
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/30—Processes for preparing, regenerating, or reactivating
    • B01J20/3078—Thermal treatment, e.g. calcining or pyrolizing
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2253/00—Adsorbents used in seperation treatment of gases and vapours
    • B01D2253/10—Inorganic adsorbents
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2253/00—Adsorbents used in seperation treatment of gases and vapours
    • B01D2253/10—Inorganic adsorbents
    • B01D2253/104—Alumina
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2257/00—Components to be removed
    • B01D2257/30—Sulfur compounds
    • B01D2257/304—Hydrogen sulfide

Abstract

The invention discloses a preparation method of a renewable adsorbent for deeply removing hydrogen sulfide, which comprises the following steps: firstly, adding polyethylene glycol, tetraethoxysilane and hexamethylenetetramine into a nitric acid solution, heating, preserving heat, stirring, and then adding NH4OH stirring, cleaning and drying to obtain powder I; secondly, uniformly mixing sodium metaaluminate, sodium thiosulfate and anhydrous sodium carbonate, and roasting to obtain powder II; thirdly, uniformly mixing the powder I and the powder II, adding activated alumina for calcination, and cooling to obtain powder III; and fourthly, grinding the powder III to obtain the renewable adsorbent. The invention controls the roasting process of the powder after adding the activated alumina and combines the addition of the auxiliary agent, so that the renewable adsorbent is preparedThe pore structure and the density are changed, the specific surface area is increased, the selectivity of the renewable adsorbent to the hydrogen sulfide gas is improved, the combination of the hydrogen sulfide gas and the renewable adsorbent through a complexing action force is promoted, and the adsorption capacity and the renewable performance to the hydrogen sulfide gas are improved.

Description

Preparation method of renewable adsorbent for deeply removing hydrogen sulfide
Technical Field
The invention belongs to the technical field of environmental protection, and particularly relates to a preparation method of a renewable adsorbent for deeply removing hydrogen sulfide.
Background
The hydrogen sulfide is widely present in natural gas and methane, has pungent odor, is very toxic to human bodies, is inflammable and explosive, is very easy to corrode metal, blocks pipelines, causes great pollution to the environment even if tail gas and natural gas discharged by factories contain a small amount of hydrogen sulfide, and sometimes wastes a lot of resources even because of the presence of low-concentration hydrogen sulfide. The sulfur-containing compounds are likely to generate hydrogen sulfide through various reactions, and the hydrogen sulfide in the industrial waste gas mainly comes from oil refineries, natural gas purification plants, smelting plants, tanneries, nitrogen fertilizer plants, pesticide plants and the like, but mainly takes oil refineries, natural gas purification plants, gas purification plants and synthetic nitrogen fertilizer raw material gases as quantities. For many years, researchers at home and abroad have conducted a great deal of research on the problem of desulfurization of sulfur-containing gases such as natural gas, coal bed gas and methane.
Currently, the commonly used desulfurization methods can be classified into dry desulfurization and wet desulfurization. The wet desulphurization such as a liquid phase catalysis method, a sodium carbonate or alcohol amine absorption method and the like is suitable for treating large-flow gas, has high desulphurization efficiency, can be continuously operated, but is easy to generate secondary pollution, has high investment and operation cost, and is difficult to bear by common manufacturers. The dry desulfurization is mainly applicable to fine desulfurization, and has the main disadvantage that the desulfurizing agent has relatively low adsorption capacity for hydrogen sulfide, resulting in relatively low desulfurization efficiency. The technical core of dry desulfurization is the development of an adsorbent or a catalyst. The desulfurization effect of the general metal oxide is good, but the utilization rate of the metal oxide is low, and the cost is higher; while the common activated carbon material mainly comprising micropores is widely used as an adsorbent, the blockage of pore channels is easy to occur in the adsorption process of hydrogen sulfide, so that the adsorption capacity is low. Therefore, the development of an adsorbing material with high hydrogen sulfide adsorption capacity is the key point of environmental material development.
Disclosure of Invention
The technical problem to be solved by the invention is to provide a preparation method of a renewable adsorbent for deeply removing hydrogen sulfide aiming at the defects of the prior art. According to the method, the roasting process of the powder after the active alumina is added is controlled, and the addition of the auxiliary agent is combined, so that the pore structure and the density of the renewable adsorbent are changed, the specific surface area is increased, the selectivity of the renewable adsorbent to the hydrogen sulfide gas is improved, the combination of the hydrogen sulfide gas and active components on the surface of the renewable adsorbent through complexing force is promoted, and the adsorption capacity and the renewable performance to the hydrogen sulfide gas are improved.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows: a preparation method of a regenerable adsorbent for deeply removing hydrogen sulfide is characterized by comprising the following steps:
step one, adding 5-9 parts by mass of polyethylene glycol, 2-6 parts by mass of ethyl orthosilicate and 1-4 parts by mass of hexamethylenetetramine into 10-20 parts by mass of nitric acid solution, heating, keeping the temperature and stirring, and then adding 2-9 parts by mass of NH4OH is stirred to obtain a solid product, and the solid product is washed by absolute ethyl alcohol and then dried to obtain powder I; the mass concentration of the nitric acid solution is 65 percent;
step two, uniformly mixing 2-7 parts of sodium metaaluminate, 1-4 parts of sodium thiosulfate and 2-8 parts of anhydrous sodium carbonate in parts by weight, and roasting to obtain powder II;
step three, uniformly mixing the powder I obtained in the step one and the powder II obtained in the step two, then adding 60-80 parts by mass of activated alumina, calcining, and cooling to room temperature to obtain powder III;
grinding the powder III obtained in the step three to obtain a renewable adsorbent; the average particle size of the regenerable adsorbent is 4-8 μm.
Aiming at the defects that in the prior art, hydrogen sulfide is removed through chemical adsorption or physical adsorption, the chemical adsorption generates new chemical bonds and is difficult to damage, so that the adsorbent cannot be regenerated, and the pure physical adsorption has weak binding force, so that the adsorption capacity of the adsorbent is too low, the method comprises the steps of firstly preparing powder I containing a pore-forming agent, a surfactant and an amine source, then preparing powder II containing a sodium source, mixing the powder I and the powder II, adding activated alumina, calcining to obtain powder III, and grinding to obtain the regenerated hydrogen sulfide gas adsorbent. According to the invention, through designing the compositions of the powder I and the powder II, in the roasting process after the mixture of the powder I and the powder II is added into the activated alumina, the carrier alumina is subjected to dehydration reaction, and the crystal structure is subjected to phase change, so that the pore structure and the density of the renewable adsorbent are changed, isomers are generated, the renewable adsorbent with narrow pore size distribution and concentrated to 3-5 nm is obtained, and the selectivity of the renewable adsorbent to hydrogen sulfide gas and the adsorption capacity of the hydrogen sulfide gas are improved. Meanwhile, the surface active agent and other additives are attached to the pore channel of the renewable adsorbent, so that the surface structure of the renewable adsorbent is changed, the specific surface area is increased, the combination of hydrogen sulfide gas and active components on the surface of the renewable adsorbent through a complexing force is promoted, and the adsorption capacity of the renewable adsorbent is further improved because the complexing force is greater than the Van der Waals force of physical adsorption. In addition, because the pore structure and the specific surface area of the regenerable adsorbent are changed, the hydrogen sulfide gas is easier to desorb and remove, so that the sulfur capacity, namely the adsorption quantity, of the regenerable adsorbent is increased, and the regenerability of the regenerable adsorbent is improved.
The preparation method of the regenerable adsorbent for deeply removing the hydrogen sulfide is characterized in that the heating temperature in the step one is 80-90 ℃, and the heat preservation and stirring time is 2-5 hours. The heating temperature and the heat preservation stirring time are favorable for promoting the reaction among polyethylene glycol, tetraethoxysilane, hexamethylenetetramine and nitric acid solution.
The preparation method of the regenerable adsorbent for deeply removing hydrogen sulfide is characterized in that the drying temperature in the first step is 90-110 ℃. The drying temperature of 90-110 ℃ is adopted to ensure the complete drying of the powder I, and the energy waste caused by overhigh drying temperature is avoided.
The preparation method of the regenerable adsorbent for deeply removing the hydrogen sulfide is characterized in that the roasting temperature in the second step is 200-300 ℃, and the roasting time is 20-60 min. The roasting temperature can effectively promote the raw materials in the powder II to fully react.
The preparation method of the regenerable adsorbent for deeply removing the hydrogen sulfide is characterized in that the calcining temperature in the third step is 400-600 ℃, and the calcining time is 300-360 min. Under the condition of the calcination process parameters, redundant nitrate can be completely decomposed, so that the adsorption performance of the renewable adsorbent is ensured, the sintering phenomenon caused by overhigh temperature is avoided, the pore structure of the renewable adsorbent is damaged, the specific surface area of the renewable adsorbent is reduced, the adsorption performance is reduced, meanwhile, Van der Waals force adsorption is caused to hydrogen sulfide by the renewable adsorbent, adsorption heat is generated, the overhigh calcination temperature is not beneficial to the diffusion of the adsorption heat, further, the desorption is serious, and the adsorption efficiency is influenced.
Compared with the prior art, the invention has the following advantages:
1. according to the invention, the roasting process after the activated alumina is added into the powder is controlled, so that the phase change of the crystal structure of the carrier is generated, the pore structure and the density of the renewable adsorbent are changed, isomers are generated, the renewable adsorbent with narrow pore size distribution and concentrated to 3-5 nm is obtained, and the selectivity of the renewable adsorbent to hydrogen sulfide gas and the adsorption capacity to the hydrogen sulfide gas are improved.
2. According to the invention, by adding the auxiliary agents such as the surfactant and the like, the surface structure of the renewable adsorbent is subjected to metamorphosis, the specific surface area is increased, the combination of hydrogen sulfide gas and active components on the surface of the renewable adsorbent through a complexing action force is promoted, the hydrogen sulfide is adsorbed through physical adsorption and a complexing action, and the adsorption capacity of the renewable adsorbent is further improved.
3. According to the invention, the pore structure and the specific surface area of the renewable adsorbent are changed by controlling the roasting process and adding the auxiliary agents such as the surfactant and the like, and the hydrogen sulfide gas is easier to desorb and remove, so that the sulfur capacity, namely the adsorption capacity, of the renewable adsorbent is increased, and the renewable performance of the renewable adsorbent is improved.
4. The regenerable adsorbent has a large specific surface area, is suitable for adsorbing low-concentration (concentration is 0-500 ppm) hydrogen sulfide, has good regenerability (adsorption is performed after regeneration, the sulfur capacity is not reduced), and has an obvious effect of purifying and treating the hydrogen sulfide.
The technical solution of the present invention is further described in detail by examples below.
Detailed Description
Example 1
The embodiment comprises the following steps:
step one, adding 5 parts of polyethylene glycol, 2 parts of ethyl orthosilicate and 1 part of hexamethylenetetramine into 10 parts of nitric acid solution by mass, heating to 80 ℃, keeping the temperature and stirring for 2 hours, and then adding 2 parts of NH4OH is stirred to obtain a solid product, and the solid product is washed by absolute ethyl alcohol and dried at the temperature of 90 ℃ to obtain powder I; the mass concentration of the nitric acid solution is 65 percent;
step two, uniformly mixing 2 parts of sodium metaaluminate, 1 part of sodium thiosulfate and 2 parts of anhydrous sodium carbonate in parts by weight, roasting for 20min at the temperature of 200 ℃, quenching the obtained melt in water, and then crushing to obtain powder II;
step three, uniformly mixing the powder I obtained in the step one and the powder II obtained in the step two, then adding 60 parts by mass of activated alumina, placing the mixture in a muffle furnace to calcine the mixture for 300min at the temperature of 400 ℃, cooling the mixture to room temperature to obtain powder III, and carrying out BET test on the powder III, wherein the specific surface area of the powder III is 220m2/g；
Grinding the powder III obtained in the step three to obtain a renewable adsorbent; the regenerable adsorbent had an average particle size of 4 μm.
The method for detecting the hydrogen sulfide adsorption of the renewable adsorbent prepared by the embodiment comprises the following specific processes: before an adsorption test is carried out, activating treatment is carried out on a renewable adsorbent, the activating process is the same as that of the regeneration process, the renewable adsorbent is firstly filled into a fixed reaction bed, nitrogen is introduced into the fixed reaction bed at the temperature of 100 ℃ and the temperature is raised, the temperature is raised to 280 ℃ at the speed of 3 ℃/min and kept for 4 hours, then the temperature is lowered to the room temperature, finally, the introduction of the nitrogen is stopped, and the activating process is finished; filling 10mL of adsorbent into a U-shaped pipe with a branch, introducing 100ppm of hydrogen sulfide standard gas to start timing, wherein the flow rate of the hydrogen sulfide standard gas is 0.6L/min, detecting the concentration of the hydrogen sulfide at an outlet by a TYBX31C pump-suction type gas detector produced by Shanghai Tang apparatus electronic technology Co., Ltd, and recording the time from the start of timing to the stop of timing as the penetration time when the concentration of the hydrogen sulfide at the outlet reaches 0.01ppm and the timing is stopped; and detecting the concentration of hydrogen sulfide in the airflow at the outlet of the U-shaped pipe by adopting a handheld hydrogen sulfide detector. The results show that: the penetration time of the regenerable adsorbent prepared by the embodiment to hydrogen sulfide at 45 ℃ is 65min, and the capacity of absorbing hydrogen sulfide can reach 39%.
Regenerating the regenerable adsorbent after hydrogen sulfide adsorption detection, wherein the regeneration comprises the following specific processes: introducing nitrogen into the fixed reaction bed at 100 ℃, heating to 280 ℃ at 3 ℃/min, keeping for 4 hours, then cooling to room temperature, and finally stopping introducing the nitrogen. The regenerated adsorbent is subjected to the hydrogen sulfide adsorption detection process, and the result shows that the penetration time of the regenerated adsorbent is still 65min, which indicates that the adsorption performance of the regenerated hydrogen sulfide gas adsorbent prepared in the embodiment is not affected and has stable adsorption performance.
Example 2
The embodiment comprises the following steps:
step one, adding 7 parts of polyethylene glycol, 4 parts of ethyl orthosilicate and 2 parts of hexamethylenetetramine into 15 parts of nitric acid solution by mass, heating to 85 ℃, keeping the temperature and stirring for 4 hours, and then adding 5 parts of NH4OH is stirred to obtain a solid product, and the solid product is washed by absolute ethyl alcohol and dried at the temperature of 100 ℃ to obtain powder I; the mass concentration of the nitric acid solution is 65 percent;
step two, uniformly mixing 5 parts of sodium metaaluminate, 2 parts of sodium thiosulfate and 5 parts of anhydrous sodium carbonate in parts by weight, roasting for 40min at the temperature of 240 ℃, quenching the obtained melt in water, and then crushing to obtain powder II;
step three, uniformly mixing the powder I obtained in the step one and the powder II obtained in the step two, adding 70 parts by mass of activated alumina, and calcining 330 in a muffle furnace at the temperature of 500 DEG Cmin, cooling to room temperature to obtain powder III, and performing BET test on the powder III to obtain powder III with specific surface area of 259m2/g；
Grinding the powder III obtained in the step three to obtain a renewable adsorbent; the regenerable adsorbent had an average particle size of 6 μm.
The method for detecting the hydrogen sulfide adsorption of the renewable adsorbent prepared by the embodiment comprises the following specific processes: before an adsorption test is carried out, activating treatment is carried out on a renewable adsorbent, the activating process is the same as that of the regeneration process, the renewable adsorbent is firstly filled into a fixed reaction bed, nitrogen is introduced into the fixed reaction bed at the temperature of 100 ℃ and the temperature is raised, the temperature is raised to 280 ℃ at the speed of 3 ℃/min and kept for 4 hours, then the temperature is lowered to the room temperature, finally, the introduction of the nitrogen is stopped, and the activating process is finished; filling 10mL of adsorbent into a U-shaped pipe with a branch, introducing 100ppm of hydrogen sulfide standard gas to start timing, wherein the flow rate of the hydrogen sulfide standard gas is 0.6L/min, detecting the concentration of the hydrogen sulfide at an outlet by a TYBX31C pump-suction type gas detector produced by Shanghai Tang apparatus electronic technology Co., Ltd, and recording the time from the start of timing to the stop of timing as the penetration time when the concentration of the hydrogen sulfide at the outlet reaches 0.01ppm and the timing is stopped; and detecting the concentration of hydrogen sulfide in the airflow at the outlet of the U-shaped pipe by adopting a handheld hydrogen sulfide detector. The results show that: the penetration time of the regenerable adsorbent prepared by the embodiment to hydrogen sulfide at 45 ℃ is 70min, and the capacity of absorbing hydrogen sulfide can reach 42%.
Regenerating the regenerable adsorbent after hydrogen sulfide adsorption detection, wherein the regeneration comprises the following specific processes: introducing nitrogen into the fixed reaction bed at 100 ℃, heating to 280 ℃ at 3 ℃/min, keeping for 4 hours, then cooling to room temperature, and finally stopping introducing the nitrogen. The regenerated adsorbent is subjected to the hydrogen sulfide adsorption detection process, and the result shows that the penetration time of the regenerated adsorbent is still 70min, which indicates that the adsorption performance of the regenerated hydrogen sulfide gas adsorbent prepared in the embodiment is not affected and has stable adsorption performance.
Example 3
The embodiment comprises the following steps:
step oneAdding 9 parts of polyethylene glycol, 6 parts of ethyl orthosilicate and 4 parts of hexamethylenetetramine into 20 parts of nitric acid solution by weight, heating to 90 ℃, keeping the temperature and stirring for 5 hours, and then adding 9 parts of NH4OH is stirred to obtain a solid product, and the solid product is washed by absolute ethyl alcohol and dried at the temperature of 110 ℃ to obtain powder I; the mass concentration of the nitric acid solution is 65 percent;
step two, uniformly mixing 7 parts of sodium metaaluminate, 4 parts of sodium thiosulfate and 8 parts of anhydrous sodium carbonate in parts by weight, roasting for 60min at the temperature of 300 ℃, quenching the obtained melt in water, and then crushing to obtain powder II;
step three, uniformly mixing the powder I obtained in the step one and the powder II obtained in the step two, adding 80 parts by mass of activated alumina, placing the mixture in a muffle furnace, calcining the mixture for 360min at the temperature of 600 ℃, cooling the mixture to room temperature to obtain powder III, and carrying out BET test on the powder III, wherein the specific surface area of the powder III is 237m2/g；
Grinding the powder III obtained in the step three to obtain a renewable adsorbent; the regenerable adsorbent had an average particle size of 8 μm.
The method for detecting the hydrogen sulfide adsorption of the renewable adsorbent prepared by the embodiment comprises the following specific processes: before an adsorption test is carried out, activating treatment is carried out on a renewable adsorbent, the activating process is the same as that of the regeneration process, the renewable adsorbent is firstly filled into a fixed reaction bed, nitrogen is introduced into the fixed reaction bed at the temperature of 100 ℃ and the temperature is raised, the temperature is raised to 280 ℃ at the speed of 3 ℃/min and kept for 4 hours, then the temperature is lowered to the room temperature, finally, the introduction of the nitrogen is stopped, and the activating process is finished; filling 10mL of adsorbent into a U-shaped pipe with a branch, introducing 100ppm of hydrogen sulfide standard gas to start timing, wherein the flow rate of the hydrogen sulfide standard gas is 0.6L/min, detecting the concentration of the hydrogen sulfide at an outlet by a TYBX31C pump-suction type gas detector produced by Shanghai Tang apparatus electronic technology Co., Ltd, and recording the time from the start of timing to the stop of timing as the penetration time when the concentration of the hydrogen sulfide at the outlet reaches 0.01ppm and the timing is stopped; and detecting the concentration of hydrogen sulfide in the airflow at the outlet of the U-shaped pipe by adopting a handheld hydrogen sulfide detector. The results show that: the penetration time of the regenerable adsorbent prepared by the embodiment to hydrogen sulfide at 45 ℃ is 67min, and the capacity of absorbing hydrogen sulfide can reach 40%.
Regenerating the regenerable adsorbent after hydrogen sulfide adsorption detection, wherein the regeneration comprises the following specific processes: introducing nitrogen into the fixed reaction bed at 100 ℃, heating to 280 ℃ at 3 ℃/min, keeping for 4 hours, then cooling to room temperature, and finally stopping introducing the nitrogen. The regenerated adsorbent is subjected to the hydrogen sulfide adsorption detection process, and the result shows that the penetration time of the regenerated adsorbent is still 67min, which indicates that the adsorption performance of the regenerated hydrogen sulfide gas adsorbent prepared in the embodiment is not affected and has stable adsorption performance.
The above description is only for the preferred embodiment of the present invention, and is not intended to limit the present invention in any way. Any simple modification, change and equivalent changes of the above embodiments according to the technical essence of the invention are still within the protection scope of the technical solution of the invention.

Claims (5)

1. A preparation method of a regenerable adsorbent for deeply removing hydrogen sulfide is characterized by comprising the following steps:
step one, adding 5-9 parts by mass of polyethylene glycol, 2-6 parts by mass of ethyl orthosilicate and 1-4 parts by mass of hexamethylenetetramine into 10-20 parts by mass of nitric acid solution, heating, keeping the temperature and stirring, and then adding 2-9 parts by mass of NH4OH is stirred to obtain a solid product, and the solid product is washed by absolute ethyl alcohol and then dried to obtain powder I; the mass concentration of the nitric acid solution is 65 percent;
step two, uniformly mixing 2-7 parts of sodium metaaluminate, 1-4 parts of sodium thiosulfate and 2-8 parts of anhydrous sodium carbonate in parts by weight, and roasting to obtain powder II;
step three, uniformly mixing the powder I obtained in the step one and the powder II obtained in the step two, then adding 60-80 parts by mass of activated alumina, calcining, and cooling to room temperature to obtain powder III;
grinding the powder III obtained in the step three to obtain a renewable adsorbent; the average particle size of the regenerable adsorbent is 4-8 μm.
2. The method for preparing the regenerable adsorbent capable of deeply removing hydrogen sulfide as claimed in claim 1, wherein the heating temperature in step one is 80-90 ℃, and the heat preservation stirring time is 2-5 h.
3. The method for preparing the regenerable adsorbent with deep removal of hydrogen sulfide as claimed in claim 1, wherein the drying temperature in the first step is 90-110 ℃.
4. The method for preparing the regenerable adsorbent capable of deeply removing hydrogen sulfide as claimed in claim 1, wherein the calcination temperature in step two is 200-300 ℃ and the calcination time is 20-60 min.
5. The method for preparing the regenerable adsorbent capable of deeply removing hydrogen sulfide as claimed in claim 1, wherein the calcination temperature in step three is 400-600 ℃ and the calcination time is 300-360 min.
CN202111366656.1A 2021-11-18 2021-11-18 Preparation method of renewable adsorbent for deeply removing hydrogen sulfide Pending CN113893814A (en)

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