CN114749164A - Preparation method of sulfur dioxide and hydrogen sulfide gas adsorbent - Google Patents

Preparation method of sulfur dioxide and hydrogen sulfide gas adsorbent Download PDF

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Publication number
CN114749164A
CN114749164A CN202210418362.7A CN202210418362A CN114749164A CN 114749164 A CN114749164 A CN 114749164A CN 202210418362 A CN202210418362 A CN 202210418362A CN 114749164 A CN114749164 A CN 114749164A
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China
Prior art keywords
precursor
hydrogen sulfide
sulfur dioxide
sulfide gas
treatment
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CN202210418362.7A
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施振亚
曾国治
曾敏
杨志
翟晓强
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Jiangsu Meiya Keze Filtration Technology Co ltd
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Jiangsu Meiya Keze Filtration Technology Co ltd
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    • 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
    • B01J20/3021—Milling, crushing or grinding
    • 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
    • B01J20/02—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
    • 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
    • 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
    • B01J20/3085—Chemical treatments not covered by groups B01J20/3007 - B01J20/3078
    • 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
    • B01J2220/00—Aspects relating to sorbent materials
    • B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
    • B01J2220/48—Sorbents characterised by the starting material used for their preparation
    • B01J2220/4812—Sorbents characterised by the starting material used for their preparation the starting material being of organic character
    • B01J2220/4825—Polysaccharides or cellulose materials, e.g. starch, chitin, sawdust, wood, straw, cotton
    • 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
    • B01J2220/00—Aspects relating to sorbent materials
    • B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
    • B01J2220/48—Sorbents characterised by the starting material used for their preparation
    • B01J2220/4875—Sorbents characterised by the starting material used for their preparation the starting material being a waste, residue or of undefined composition
    • B01J2220/4881—Residues from shells, e.g. eggshells, mollusk shells

Abstract

The invention discloses a preparation method of a sulfur dioxide and hydrogen sulfide gas adsorbent, which comprises the following steps: step S1, the precursor body is prepared: grinding, cleaning and drying the precursor body to obtain a clean precursor body; step S2, modified processing: carrying out dipping treatment and standing placement on the precursor body obtained in the step S1 by using a modifying agent; step S3, drying: placing the precursor subjected to the modification treatment in the step S2 into a vacuum drying oven for drying treatment to obtain a dried precursor; step S4, carbonization: under the protection of inert gas, the precursor obtained in the step S3 is subjected to heating carbonization treatment; step S5, calcination treatment: the carbonized precursor body in step S4 is calcined under the protection of an inert gas. The method of the invention not only can shorten the preparation process of the conventional adsorbent and improve the preparation efficiency, but also can achieve the effects of increasing the gaps of the adsorbent and attaching the catalyst, and improve the adsorption efficiency and the effect.

Description

Preparation method of sulfur dioxide and hydrogen sulfide gas adsorbent
Technical Field
The invention belongs to the technical field of adsorbent preparation, and particularly relates to a preparation method of an adsorbent for sulfur dioxide and hydrogen sulfide gas.
Background
Sulfur dioxide, hydrogen sulfide and other sulfides are one of the important sources of air pollutants, which can stimulate the respiratory tract of the human body and damage the nervous system, liver, kidney and other important organs of the human body, and porous materials such as activated carbon, zeolite, metal organic frameworks, molecular sieves and the like benefit from the huge specific surface area and the complex pore structures and are widely applied to the field of air purification, including adsorption purification of sulfur dioxide, hydrogen sulfide and other sulfides. Among them, the activated carbon material is the most common adsorbing material because of its advantages such as better universality, certain mechanical strength, higher adsorption speed, etc.
The common activated carbon mainly depends on the interaction force among molecules when adsorbing gaseous molecular pollutants in the air, thereby aiming at the defects of difficult capture, small adsorption quantity, easy desorption and the like of low-concentration polluted gas. Therefore, in practical applications, it is necessary to perform modification treatment on the activated carbon, such as oxidation modification or alkaline compound solution impregnation modification. Currently, the preparation of the activated carbon adsorbent mainly comprises two steps: the first step is the preparation of active carbon, which is prepared by the processes of drying, carbonizing, activating and washing a precursor body; the second step is the modification of the activated carbon, and specifically comprises the steps of impregnation, drying, calcination and the like of the activated carbon. However, in the above-mentioned preparation process of the activated carbon adsorbent, the preparation of the activated carbon and the modification of the activated carbon are separated, so that the preparation process is complicated and is susceptible to environmental influences, such as air humidity and pollutant concentration, resulting in easy desorption or small adsorption capacity.
Disclosure of Invention
In view of the above problems, the present invention discloses a method for preparing an adsorbent for hydrogen sulfide gas and sulfur dioxide, so as to overcome the above problems or at least partially solve the above problems.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of a sulfur dioxide and hydrogen sulfide gas adsorbent comprises the following steps:
step S1, the precursor body is prepared: grinding, cleaning and drying the precursor body to obtain a clean precursor body;
step S2, modified processing: carrying out dipping treatment and standing placement on the precursor body obtained in the step S1 by using a modifying agent;
step S3, drying: placing the pre-material body subjected to the modification treatment in the step S2 in a vacuum drying oven for drying treatment to obtain a dried pre-material body;
step S4, carbonization: under the protection of inert gas, carrying out heating carbonization treatment on the precursor body obtained in the step S3;
step S5, calcination treatment: the carbonized precursor body in step S4 is calcined under the protection of an inert gas.
Preferably, in step S1, the precursor body is any one or more of coconut shells, nut shells, walnut shells, apricot pits, and wood chips.
Preferably, in step S1, the particle size of the precursor after grinding is 20 to 50 mesh.
Preferably, in step S1, the precursor is dried at 60 to 80 ℃ for 2 to 3 hours.
Preferably, in step S2, the modifying agent includes one or both of copper chloride and zinc chloride.
Preferably, the mass fraction of the copper chloride is 0-15 wt%, and the mass fraction of the zinc chloride is 0-15 wt%.
Preferably, in step S2, the immersion time is 10 to 12 hours, and the standing time is 2 to 3 hours.
Preferably, in step S2, the mass ratio of the precursor to the modifying agent is 1 (5-20).
Preferably, in step S3, the temperature of the vacuum drying oven is 60-80 ℃, and the drying time is 2-3 h.
Preferably, in step S4, the carbonization temperature is 800-900 ℃ and the carbonization time is 2-3 h.
Preferably, in step S5, the calcination temperature is 400 to 500 ℃, and the calcination time is 1 to 2 hours.
The invention has the advantages and beneficial effects that:
according to the preparation method of the adsorbent, activation treatment, drying treatment, carbonization treatment and calcination treatment are carried out on the ground, cleaned and dried precursor body in turn, so that the activation treatment and the modification treatment of the precursor body are completed at one time in the activation treatment stage, the preparation process of the conventional adsorbent can be shortened, the preparation efficiency of the adsorbent is improved, the effects of increasing the gaps of the adsorbent and attaching a catalyst can be achieved, and the adsorption efficiency and the adsorption effect on gas are improved.
Drawings
Various other advantages and benefits will become apparent to those of ordinary skill in the art upon reading the following detailed description of the preferred embodiments. The drawings are only for purposes of illustrating the preferred embodiments and are not to be construed as limiting the invention. Also, like reference numerals are used to refer to like parts throughout the drawings. In the drawings:
fig. 1 is a schematic flow chart of a method for preparing the absorbent for absorbing sulfur dioxide and hydrogen sulfide gas in this embodiment.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the technical solutions of the present invention will be described in detail and fully with reference to the accompanying drawings. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. 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.
With reference to fig. 1, the invention discloses a preparation method of a sulfur dioxide and hydrogen sulfide gas adsorbent, which specifically comprises the following steps:
in step S1, the precursor body is prepared. The precursor body, for example coconut shells, is subjected to grinding, washing and drying processes, so that a clean precursor body is obtained.
Preferably, the particle size of the ground precursor is controlled to be 20-50 meshes, so that the proper size of the finally obtained adsorbent is ensured, and the efficient adsorption effect on sulfur dioxide and hydrogen sulfide gas is achieved. Meanwhile, the ground and cleaned precursor body is dried for 2-3 hours at the temperature of 60-80 ℃ to achieve effective fruit drying treatment on the precursor body.
Of course, other materials such as nut shells, walnut shells, apricot seeds and wood chips can be used, and even mixed materials including the above materials can be used. At this time, according to the structural difference between different materials, the grinding particle size of the precursor body, the drying temperature and the drying time can be adjusted, and finally the clean and dry precursor body with proper gaps can be obtained.
Step S2, live change processing. The activating and modifying agent is used for carrying out dipping treatment and standing placement on the precursor body obtained in the step S1, so that the effect of completing activating treatment and modifying treatment on the precursor body at one time is achieved.
Wherein the mass ratio of the precursor to the modifying agent is 1 (5-20), and the modifying treatment is carried out on the precursor so as to ensure the effective activating treatment and modifying treatment on the precursor.
Preferably, the selected modifying agent at least comprises one of copper chloride and zinc chloride. At the moment, the pretreatment agent containing copper chloride and/or zinc chloride is used for carrying out impregnation and standing pretreatment on the precursor, so that the precursor can be subjected to the pretreatment to increase the pores, the specific surface area of the final adsorbent is increased, the adsorption efficiency of the gas is improved, the precursor can be simultaneously subjected to the modification treatment, the copper and/or the zinc are attached to the final adsorbent, the catalytic treatment of sulfur dioxide and hydrogen sulfide gas is further formed, the sulfur dioxide and hydrogen sulfide gas react with oxygen in the air to form salt substances, and the adsorption treatment effect of the sulfur dioxide and the hydrogen sulfide gas is achieved.
Preferably, the mass fraction of copper chloride in the modifying agent is controlled to be 0-15 wt%, the mass fraction of zinc chloride is controlled to be 0-15 wt%, the soaking time is controlled to be 10-12 h, and the standing time is controlled to be 2-3 h.
Step S3, drying process. And (5) placing the pre-material body subjected to the modification treatment in the step S2 in a vacuum drying oven for drying treatment to obtain a dried pre-material body. In the embodiment, the temperature of the vacuum drying oven is controlled to be 60-80 ℃, and the drying time is controlled to be 2-3 hours, so as to achieve effective drying treatment of the precursor.
Step S4, carbonization. Under the protection of inert gas, the precursor body obtained in step S3 is subjected to a heat carbonization treatment. Wherein the carbonization temperature is 800-900 ℃, and the carbonization time is 2-3 h.
Step S5, calcination process. The carbonized precursor body in step S4 is calcined under the protection of an inert gas. Wherein the calcining temperature is 400-500 ℃, and the calcining time is 1-2 h.
Next, the adsorbent is prepared by the above-described method for preparing an adsorbent for sulfur dioxide and hydrogen sulfide gases.
Example 1:
the coconut shell is selected as a precursor, firstly, 10g of coconut shell is ground and screened to 20-50 meshes, and then the coconut shell is dried for 2 hours at 80 ℃ after being washed by deionized water. Subsequently, the washed precursor was added to 100g of a 15 wt% cupric chloride solution, immersed for 12 hours, filtered, and left to stand for 3 hours. Then, the coconut shell is put into a vacuum drying oven and dried for 2 hours at 80 ℃. And then, under the protection of nitrogen, heating the activated coconut shell to 800 ℃ for carbonization treatment for 3 h. And finally, calcining for 2 hours at 400 ℃ under the protection of nitrogen, thereby preparing the target adsorbent.
Example 2:
the coconut shell is selected as a precursor, firstly, 10g of coconut shell is ground and screened to 20-50 meshes, and then the coconut shell is dried for 2 hours at 80 ℃ after being washed by deionized water. Then, the cleaned precursor was added to a mixed solution of 100g of 10 wt% copper chloride and 5 wt% zinc chloride, and the mixture was immersed for 12 hours, filtered, and left to stand for 3 hours. Then, the coconut shell was put into a vacuum oven and dried at 80 ℃ for 2 hours. And then, under the protection of nitrogen, heating the activated coconut shell to 800 ℃ for carbonization treatment for 3 h. And finally, calcining for 2 hours at 400 ℃ under the protection of nitrogen, thereby preparing the target adsorbent.
Example 3:
the coconut shell is selected as a precursor, firstly, 10g of coconut shell is ground and screened to 20-50 meshes, and then the coconut shell is dried for 2 hours at 80 ℃ after being washed by deionized water. Then, the cleaned precursor was added to a mixed solution of 100g of 5 wt% copper chloride and 10 wt% zinc chloride, and the mixture was immersed for 12 hours, filtered, and left to stand for 3 hours. Then, the coconut shell was put into a vacuum oven and dried at 80 ℃ for 2 hours. And then, under the protection of nitrogen, heating the activated coconut shell to 800 ℃ for carbonization treatment for 3 h. And finally, calcining for 2 hours at 400 ℃ under the protection of nitrogen, thereby preparing the target adsorbent.
Example 4:
the method comprises the steps of selecting coconut shells as a precursor material body, firstly, grinding 10g of coconut shells, screening to 20-50 meshes, washing with deionized water, and drying at 80 ℃ for 2 hours. Subsequently, the washed precursor was added to 100g of a 15 wt% zinc chloride solution, immersed for 12 hours, filtered, and left to stand for 3 hours. Then, the coconut shell was put into a vacuum oven and dried at 80 ℃ for 2 hours. And then, under the protection of nitrogen, heating the activated coconut shell to 800 ℃ for carbonization treatment for 3 h. And finally, calcining for 2 hours at 400 ℃ under the protection of nitrogen, thereby preparing the target adsorbent.
Example 5:
the method comprises the steps of selecting walnut shells as a precursor material, grinding 10g of walnut shells, screening to 20-50 meshes, washing with deionized water, and drying at 80 ℃ for 2 hours. Then, the cleaned precursor was added to a mixed solution of 100g of 5 wt% copper chloride and 10 wt% zinc chloride, and the mixture was immersed for 12 hours, filtered, and left to stand for 3 hours. Then, the walnut shells are put into a vacuum drying oven and dried for 2 hours at the temperature of 80 ℃. And then, under the protection of nitrogen, heating the activated walnut shells to 800 ℃ for carbonization for 3 hours. And finally, calcining for 2 hours at 400 ℃ under the protection of nitrogen, thereby preparing the target adsorbent.
Example 6:
the coconut shell is selected as a precursor, 10g of coconut shell is ground and screened to 20-50 meshes, and the coconut shell is washed by deionized water and dried for 2 hours at 80 ℃. Then, the cleaned precursor was added to a mixed solution of 100g of 5 wt% copper chloride and 10 wt% zinc chloride, and the mixture was immersed for 10 hours, filtered, and left to stand for 3 hours. Then, the coconut shell was put into a vacuum oven and dried at 80 ℃ for 2 hours. And then, under the protection of nitrogen, heating the activated coconut shell to 800 ℃ for carbonization treatment for 3 h. And finally, calcining for 2 hours at 400 ℃ under the protection of nitrogen, thereby preparing the target adsorbent.
Example 7:
the coconut shell is selected as a precursor, 10g of coconut shell is ground and screened to 20-50 meshes, and the coconut shell is washed by deionized water and dried for 2 hours at 80 ℃. Next, the washed precursor was added to a mixed solution of 100g of 5 wt% copper chloride and 10 wt% zinc chloride, and the mixture was immersed for 12 hours, filtered, and left to stand for 3 hours. Then, the coconut shell was put into a vacuum oven and dried at 80 ℃ for 2 hours. And then, under the protection of nitrogen, heating the activated coconut shell to 900 ℃ for carbonization treatment for 3 h. And finally, calcining for 2 hours at 400 ℃ under the protection of nitrogen, thereby preparing the target adsorbent.
The target adsorbents obtained in the above examples 1 to 7 were subjected to a gas adsorption test, and the adsorption effect was better than that of a common adsorbent, and therefore, an adsorbent having a better adsorption effect could be prepared by the adsorbent preparation method provided by the present invention.
While the foregoing is directed to embodiments of the present invention, other modifications and variations of the present invention may be devised by those skilled in the art in light of the foregoing teachings. It should be understood by those skilled in the art that the foregoing detailed description is for the purpose of better explaining the present invention, and the scope of the present invention should be determined by the scope of the appended claims.

Claims (11)

1. A preparation method of a sulfur dioxide and hydrogen sulfide gas adsorbent is characterized by comprising the following steps:
step S1, preparing a precursor: grinding, cleaning and drying the precursor body to obtain a clean precursor body;
step S2, change processing: carrying out dipping treatment and standing placement on the precursor body obtained in the step S1 by using a modifying agent;
step S3, drying: placing the pre-material body subjected to the modification treatment in the step S2 in a vacuum drying oven for drying treatment to obtain a dried pre-material body;
step S4, carbonization: under the protection of inert gas, carrying out heating carbonization treatment on the precursor body obtained in the step S3;
step S5, calcination treatment: the carbonized precursor body in step S4 is calcined under the protection of an inert gas.
2. The method for producing the adsorbent for sulfur dioxide and hydrogen sulfide gas as claimed in claim 1, wherein the precursor body is any one or more of coconut shell, nut shell, walnut shell, apricot kernel and wood chip in step S1.
3. The method for producing an adsorbent for sulfur dioxide and hydrogen sulfide gas as claimed in claim 1, wherein in step S1, the particle size of the precursor after grinding is 20 to 50 mesh.
4. The method for producing the sulfur dioxide/hydrogen sulfide gas adsorbent as claimed in claim 1, wherein the drying treatment is performed on the precursor at 60 to 80 ℃ for 2 to 3 hours in step S1.
5. The method for preparing the absorbent for sulfur dioxide and hydrogen sulfide gas as claimed in claim 1, wherein in step S2, the modifying agent comprises one or both of copper chloride and zinc chloride.
6. The method for preparing the sulfur dioxide and hydrogen sulfide gas adsorbent as claimed in claim 5, wherein the mass fraction of copper chloride is 0 to 15 wt%, and the mass fraction of zinc chloride is 0 to 15 wt%.
7. The method for preparing the sulfur dioxide and hydrogen sulfide gas adsorbent as claimed in claim 1, wherein in step S2, the soaking time is 10-12 hours, and the standing time is 2-3 hours.
8. The method for preparing the sulfur dioxide and hydrogen sulfide gas adsorbent according to claim 1, wherein in step S2, the mass ratio of the precursor to the modifying agent is 1 (5-20).
9. The method for preparing the sulfur dioxide and hydrogen sulfide gas adsorbent according to claim 1, wherein in step S3, the temperature of the vacuum drying oven is 60-80 ℃, and the drying time is 2-3 h.
10. The method for preparing the sulfur dioxide and hydrogen sulfide gas adsorbent as claimed in claim 1, wherein in step S4, the carbonization temperature is 800-900 ℃ and the carbonization time is 2-3 h.
11. The method for preparing the sulfur dioxide and hydrogen sulfide gas adsorbent as claimed in claim 1, wherein in step S5, the calcination temperature is 400-500 ℃ and the calcination time is 1-2 h.
CN202210418362.7A 2022-04-20 2022-04-20 Preparation method of sulfur dioxide and hydrogen sulfide gas adsorbent Pending CN114749164A (en)

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