CN110652961A - Preparation method of magnesium oxide porous nano material loaded activated carbon fiber felt - Google Patents

Preparation method of magnesium oxide porous nano material loaded activated carbon fiber felt Download PDF

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CN110652961A
CN110652961A CN201910950183.6A CN201910950183A CN110652961A CN 110652961 A CN110652961 A CN 110652961A CN 201910950183 A CN201910950183 A CN 201910950183A CN 110652961 A CN110652961 A CN 110652961A
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activated carbon
carbon fiber
fiber felt
magnesium oxide
oxide porous
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金震
廖敏和
张勇
丁益
徐民达
张欢
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Anhui Jianzhu University
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/20Solid 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
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/28Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
    • B01J20/28014Solid 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
    • B01J20/28033Membrane, sheet, cloth, pad, lamellar or mat
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/28Treatment of water, waste water, or sewage by sorption
    • C02F1/281Treatment of water, waste water, or sewage by sorption using inorganic sorbents
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00Nature of the contaminant
    • C02F2101/10Inorganic compounds
    • C02F2101/12Halogens or halogen-containing compounds
    • C02F2101/14Fluorine or fluorine-containing compounds

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Abstract

The invention relates to the technical field of chemical preparation, in particular to a preparation method of a magnesium oxide porous nanomaterial loaded activated carbon fiber felt. The invention has the beneficial effects that: 1. compared with the conventional magnesium oxide material for water treatment, the invention provides the nano material for water treatment, which not only has the high adsorption property of the porous nano material of magnesium oxide, but also is convenient to recycle; 2. the morphology of the magnesium oxide porous material on the activated carbon fiber felt can be accurately controlled, the modification amount is large and exceeds 40%, and meanwhile, the preparation equipment investment is low, the process is simple, and the operation is easy; 3. the design idea and the preparation method of the water treatment material provided by the invention provide a new design idea and a new preparation method for the practical application of the magnesium oxide porous nano material.

Description

Preparation method of magnesium oxide porous nano material loaded activated carbon fiber felt
Technical Field
The invention relates to the technical field of chemical preparation, in particular to a preparation method of a magnesium oxide porous nano material loaded activated carbon fiber felt.
Background
The magnesium oxide is a common adsorption material, has good adsorption performance, and has very wide application in neutralizing acid waste gas and water, and removing arsenic, fluorine and heavy metal ions in water. With the improvement of environmental protection requirements, the national demand for high-efficiency magnesium oxide adsorbents is rapidly increased. Adsorption is the action of attaching and fixing an object to be adsorbed on the surface of an adsorbent, and the strength of the adsorption capacity of the adsorbent is often closely related to the specific surface area of the adsorbent. The porous nano material has the specific surface area which is greatly higher than that of the conventional powder material and excellent adsorption performance due to the nano size and nano holes. Therefore, in order to obtain a magnesium oxide adsorbent with better adsorption performance, scientists have prepared various magnesium oxide porous nano materials with different morphologies. The magnesium oxide porous nano material has very strong adsorption capacity, but the magnesium oxide porous nano material is directly used for water treatment and has the problems of difficult recovery, easy secondary pollution and the like, which seriously hinders the large-scale application process. Therefore, if the magnesium oxide nano material can be immobilized on the substrate, the magnesium oxide nano material can be easily recovered while ensuring the high adsorption capacity of the magnesium oxide nano material, and secondary pollution is not caused.
The activated carbon fiber is used as a multifunctional adsorption material and is mainly prepared by taking precursors such as viscose, phenolic fiber, Polyacrylonitrile (PAN), pitch, polyimide fiber and the like as the basis through carbonization and activation processes. Compared with the common activated carbon material, the activated carbon fiber has rich and developed pore structure and also has the excellent quality of a continuum material, is an ideal adsorbing material and a carrier of a catalyst, and meets the application requirements of a plurality of fields such as environmental protection, chemical industry, food, electronics, electrochemistry and the like. Therefore, in recent years, research and development of activated carbon fiber materials and surface modification thereof have received great attention from many researchers at home and abroad. However, no report is found about the modification of the activated carbon fiber by the magnesium oxide nano material at present. The abundant microporous structure and functional groups on the surface of the activated carbon fiber can provide favorable conditions for the nucleation and crystallization of magnesium oxide; thirdly, the continuous body material of the activated carbon fiber can be used as the matrix material for loading the magnesium oxide. The invention provides a method for preparing magnesium oxide nano material loaded active carbon fiber by loading magnesium oxide on the surface of a reticular active carbon fiber by using a chemical bath method, which can solve the problems of difficult loading of powder materials, difficult recycling and the like. Moreover, the method is simple and convenient, and can be used for large-scale batch production. The magnesium oxide nano material loaded activated carbon fiber has wide application prospect in the aspects of absorbing and removing arsenic, fluorine and heavy metal ions in water and the like.
Disclosure of Invention
The invention aims to overcome the problems in the prior art and provides a preparation method of a magnesium oxide porous nanomaterial loaded activated carbon fiber felt, which can overcome the defect that a nanomaterial is difficult to recycle and provides a magnesium oxide porous nanomaterial loaded activated carbon fiber material, wherein the magnesium oxide loading capacity exceeds 40%.
In order to achieve the technical purpose and achieve the technical effect, the invention is realized by the following technical scheme:
a preparation method of a magnesium oxide porous nano material loaded activated carbon fiber felt comprises the following steps:
A. activating the activated carbon fiber felt: firstly, washing an activated carbon fiber felt for a plurality of times by using clean water, then immersing the activated carbon fiber felt in a closed container filled with water, activating for a certain time at a certain temperature, taking out, and drying at a low temperature to obtain the activated carbon fiber felt;
B. loading of the magnesium oxide precursor on the activated carbon fiber felt: dissolving a hydroxyl slow-release agent and a magnesium salt in deionized water to form a transparent solution with a certain concentration, immersing the activated carbon fiber felt treated in the step A in the transparent solution for a certain time, taking out, putting the activated carbon fiber felt into a high-pressure kettle, reacting at a high temperature for a certain time, taking out, repeatedly washing with clear water for multiple times, and drying at a low temperature to obtain the activated carbon fiber felt loaded by the basic magnesium carbonate nanosheets;
C. preparing the activated carbon fiber felt loaded by the magnesium oxide porous nanosheets: and D, putting the activated carbon fiber felt processed in the step B into a muffle furnace, and annealing for a certain time in a protective gas or vacuum environment to obtain the activated carbon fiber felt loaded by the magnesium oxide porous nanosheet, wherein the loading capacity of the magnesium oxide is over 40%.
Further, the activation treatment in the step A is treatment at the temperature of 80-150 ℃ for 2-48H.
Further, the low-temperature drying in the step A and the step B is drying in an oven at the temperature of 40-80 ℃.
Further, the hydroxyl slow-release agent in the step B is a chemical product which is decomposed by urea and hexamethyleneimine at high temperature to generate hydroxyl.
Further, the magnesium salt in the step B is a soluble magnesium salt formed by a combination of any one or more of magnesium chloride, magnesium nitrate, magnesium sulfate, magnesium phosphate and magnesium oxalate.
Further, the transparent solution with a certain concentration in the step B is a mixed solution of urea with a concentration of 0.01-0.5% and magnesium salt with a concentration of 0.01-0.5%.
Further, in the step B, the activated carbon fiber felt treated in the step A is immersed in the transparent solution for 0.5-12H and then taken out.
Further, in the step B, the high-temperature reaction for a certain time refers to heat preservation for 6-24H in an autoclave with the temperature of 120-220 ℃.
Further, the protective gas in the step C is nitrogen or argon.
Further, in the step C, the annealing for a certain time refers to annealing for 2-12H in a muffle furnace at the temperature of 250-550 ℃.
The invention has the beneficial effects that: 1. compared with the conventional magnesium oxide material for water treatment, the invention provides the nano material for water treatment, which not only has the high adsorption property of the porous nano material of magnesium oxide, but also is convenient to recycle; 2. the morphology of the magnesium oxide porous material on the activated carbon fiber felt can be accurately controlled, the modification amount is large and exceeds 40%, and meanwhile, the preparation equipment investment is low, the process is simple, and the operation is easy; 3. the design idea and the preparation method of the water treatment material provided by the invention provide a new design idea and a new preparation method for the practical application of the magnesium oxide porous nano material.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings used in the description of the embodiments will be briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art that other drawings can be obtained according to the drawings without creative efforts.
FIG. 1a is a photograph of an activated carbon fiber mat before modification by a magnesium oxide porous nanosheet;
FIG. 1b is a photograph of an activated carbon fiber mat modified with a magnesium oxide porous nanosheet;
FIG. 2 is XRD spectra of activated carbon fiber felt, activated carbon fiber felt modified by magnesium oxide precursor, and activated carbon fiber felt modified by magnesium oxide porous nanosheet;
FIGS. 3a-3b are SEM images of activated carbon fiber mats at different magnifications;
3c-3e are SEM images of different magnifications of the activated carbon fiber felt modified by the magnesium oxide porous nanosheet;
FIG. 3f is a TEM image of the ultrasonically dispersed surface-modified magnesium oxide nanosheets of the activated carbon fibers;
FIG. 4 is a drawing showing isothermal adsorption of fluorine ions in water by an activated carbon fiber felt rusted by a magnesium oxide porous nanosheet;
FIG. 5 is a schematic flow chart of the method of the present invention.
Detailed Description
In order to make the technical means, the creation features, the achievement purposes and the effects of the invention easy to understand, 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 only a part of the embodiments of the present invention, not all of the 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
Referring to fig. 5, fig. 5 shows a preparation method of a magnesium oxide porous nanomaterial loaded activated carbon fiber felt, which includes the following steps:
(1) activation of the activated carbon fiber felt: firstly, washing the activated carbon fiber felt for 3 times by using clear water, then immersing the activated carbon fiber felt in a high-pressure kettle filled with water, preserving the heat for 48 hours at 80 ℃, then taking out the activated carbon fiber felt, and putting the activated carbon fiber felt into a drying oven at 40 ℃ for drying to obtain the activated carbon fiber felt.
(2) Loading of the magnesium oxide precursor on the activated carbon fiber felt: dissolving urea and magnesium chloride in deionized water to form a transparent solution with the concentration of 0.01%, and then soaking the activated carbon fiber felt treated in the step (1) in the transparent solution for 0.5H. Then, the mixture was placed in an autoclave and reacted at 120 ℃ for 6H. And after the reaction is finished, taking out, repeatedly cleaning the activated carbon fiber felt by using clear water for many times, and drying the activated carbon fiber felt in a drying oven at 40 ℃ to obtain the precursor basic magnesium carbonate nanosheet-loaded activated carbon fiber felt.
(3) Preparing the activated carbon fiber felt loaded by the magnesium oxide porous nanosheets: and (3) putting the sample in the step (2) into a muffle furnace, and annealing for 2H at 250 ℃ in a vacuum environment to obtain the magnesium oxide porous nanosheet loaded activated carbon fiber felt.
Example 2
Referring to fig. 5, fig. 5 shows a preparation method of a magnesium oxide porous nanomaterial loaded activated carbon fiber felt, which includes the following steps:
(1) activation of the activated carbon fiber felt: firstly, washing the activated carbon fiber felt for 3 times by using clear water, then immersing the activated carbon fiber felt in a high-pressure kettle filled with water, preserving the heat for 40 hours at 90 ℃, then taking out the activated carbon fiber felt, and putting the activated carbon fiber felt into a drying oven at 50 ℃ for drying to obtain the activated carbon fiber felt.
(2) Loading of the magnesium oxide precursor on the activated carbon fiber felt: dissolving urea and magnesium nitrate in deionized water to form a transparent solution with the concentration of 0.03%, and then soaking the activated carbon fiber felt treated in the step (1) in the transparent solution for 1H. Then, the mixture was placed in an autoclave and reacted at 140 ℃ for 8H. And after the reaction is finished, taking out, repeatedly cleaning the activated carbon fiber felt by using clear water for many times, and drying the activated carbon fiber felt in a drying oven at 50 ℃ to obtain the precursor basic magnesium carbonate nanosheet-loaded activated carbon fiber felt.
(3) Preparing the activated carbon fiber felt loaded by the magnesium oxide porous nanosheets: and (3) putting the sample in the step (2) into a muffle furnace, and annealing for 4H at 300 ℃ in a vacuum environment to obtain the magnesium oxide porous nanosheet loaded activated carbon fiber felt.
Example 3
Referring to fig. 5, fig. 5 shows a preparation method of a magnesium oxide porous nanomaterial loaded activated carbon fiber felt, which includes the following steps:
(1) activation of the activated carbon fiber felt: firstly, washing the activated carbon fiber felt with clear water for 4 times, then immersing the activated carbon fiber felt in a high-pressure kettle filled with water, preserving the heat for 35H at 100 ℃, then taking out the activated carbon fiber felt, and putting the activated carbon fiber felt into a drying oven at the temperature of 60 ℃ for drying to obtain the activated carbon fiber felt.
(2) Loading of the magnesium oxide precursor on the activated carbon fiber felt: dissolving hexamethyleneimine and magnesium sulfate in deionized water to form a transparent solution with the concentration of 0.06%, and then soaking the activated carbon fiber felt treated in the step (1) in the transparent solution for 2H. Then, the mixture was placed in an autoclave and reacted at 150 ℃ for 10H. And after the reaction is finished, taking out, repeatedly cleaning the activated carbon fiber felt by using clear water for many times, and drying the activated carbon fiber felt in a drying oven at the temperature of 60 ℃ to obtain the precursor basic magnesium carbonate nanosheet-loaded activated carbon fiber felt.
(3) Preparing the activated carbon fiber felt loaded by the magnesium oxide porous nanosheets: and (3) putting the sample in the step (2) into a muffle furnace, and annealing for 6H at 350 ℃ under the protection of nitrogen to obtain the magnesium oxide porous nanosheet loaded activated carbon fiber felt.
Example 4
Referring to fig. 5, fig. 5 shows a preparation method of a magnesium oxide porous nanomaterial loaded activated carbon fiber felt, which includes the following steps:
(1) activation of the activated carbon fiber felt: firstly, washing the activated carbon fiber felt for 30 times by using clear water, then immersing the activated carbon fiber felt in a high-pressure kettle filled with water, preserving the heat for 12 hours at 110 ℃, then taking out the activated carbon fiber felt, and putting the activated carbon fiber felt into a drying oven at 70 ℃ for drying to obtain the activated carbon fiber felt.
(2) Loading of the magnesium oxide precursor on the activated carbon fiber felt: dissolving hexamethyleneimine and magnesium phosphate in deionized water to form a transparent solution with the concentration of 0.08%, and then soaking the activated carbon fiber felt treated in the step (1) in the transparent solution for 4H. Then, the mixture was placed in an autoclave and reacted at 160 ℃ for 12H. And after the reaction is finished, taking out, repeatedly cleaning the activated carbon fiber felt by using clear water for many times, and drying the activated carbon fiber felt in a 70 ℃ drying oven to obtain the precursor basic magnesium carbonate nanosheet-loaded activated carbon fiber felt.
(3) Preparing the activated carbon fiber felt loaded by the magnesium oxide porous nanosheets: and (3) putting the sample in the step (2) into a tube furnace, and annealing for 8H at 400 ℃ under the protection of argon gas to obtain the activated carbon fiber felt loaded by the magnesium oxide porous nanosheet.
Example 5
Referring to fig. 5, fig. 5 shows a preparation method of a magnesium oxide porous nanomaterial loaded activated carbon fiber felt, which includes the following steps:
(1) activation of the activated carbon fiber felt: firstly, washing the activated carbon fiber felt with clear water for 5 times, then immersing the activated carbon fiber felt in a high-pressure kettle filled with water, preserving the heat for 24 hours at 120 ℃, then taking out the activated carbon fiber felt, and putting the activated carbon fiber felt into a drying oven at 80 ℃ for drying to obtain the activated carbon fiber felt.
(2) Loading of the magnesium oxide precursor on the activated carbon fiber felt: dissolving hexamethyleneimine and magnesium oxalate in deionized water to form a transparent solution with the concentration of 0.1%, and then soaking the activated carbon fiber felt treated in the step (1) in the transparent solution for 6H. Then, the mixture was placed in an autoclave and reacted at 180 ℃ for 14H. And after the reaction is finished, taking out, repeatedly cleaning the activated carbon fiber felt by using clear water for many times, and drying the activated carbon fiber felt in an oven at the temperature of 80 ℃ to obtain the precursor basic magnesium carbonate nanosheet-loaded activated carbon fiber felt.
(3) Preparing the activated carbon fiber felt loaded by the magnesium oxide porous nanosheets: and (3) putting the sample in the step (2) into a tube furnace, and annealing for 12H at 400 ℃ under the protection of argon gas to obtain the activated carbon fiber felt loaded by the magnesium oxide porous nanosheet.
Example 6
Referring to fig. 5, fig. 5 shows a preparation method of a magnesium oxide porous nanomaterial loaded activated carbon fiber felt, which includes the following steps:
(1) activation of the activated carbon fiber felt: firstly, washing the activated carbon fiber felt with clear water for 4 times, then immersing the activated carbon fiber felt in a high-pressure kettle filled with water, preserving the heat for 18 hours at 130 ℃, then taking out the activated carbon fiber felt, and putting the activated carbon fiber felt into a drying oven at 80 ℃ for drying to obtain the activated carbon fiber felt.
(2) Loading of the magnesium oxide precursor on the activated carbon fiber felt: dissolving urea and magnesium sulfate in deionized water to form a transparent solution with the concentration of 0.2%, and then soaking the activated carbon fiber felt treated in the step (1) in the solution for 8H. Then, the mixture was placed in an autoclave and reacted at 190 ℃ for 16H. And after the reaction is finished, taking out, repeatedly cleaning the activated carbon fiber felt by using clear water for many times, and drying the activated carbon fiber felt in a drying oven at the temperature of 60 ℃ to obtain the precursor basic magnesium carbonate nanosheet-loaded activated carbon fiber felt.
(3) Preparing the activated carbon fiber felt loaded by the magnesium oxide porous nanosheets: and (3) putting the sample in the step (2) into a tube furnace, and annealing for 10H at 450 ℃ under the protection of argon gas to obtain the activated carbon fiber felt loaded by the magnesium oxide porous nanosheet.
Example 7
Referring to fig. 5, fig. 5 shows a preparation method of a magnesium oxide porous nanomaterial loaded activated carbon fiber felt, which includes the following steps:
(1) activation of the activated carbon fiber felt: firstly, washing the activated carbon fiber felt with clear water for 4 times, then immersing the activated carbon fiber felt in a high-pressure kettle filled with water, preserving the heat for 8 hours at 140 ℃, then taking out the activated carbon fiber felt, and putting the activated carbon fiber felt into a drying oven at 60 ℃ for drying to obtain the activated carbon fiber felt.
(2) Loading of the magnesium oxide precursor on the activated carbon fiber felt: dissolving urea and magnesium nitrate in deionized water to form a transparent solution with the concentration of 0.3%, and then soaking the activated carbon fiber felt treated in the step (1) in the transparent solution for 10 hours. Then, the mixture was placed in an autoclave and reacted at 200 ℃ for 12H. And after the reaction is finished, taking out, repeatedly cleaning the activated carbon fiber felt by using clear water for many times, and drying the activated carbon fiber felt in a drying oven at the temperature of 60 ℃ to obtain the precursor basic magnesium carbonate nanosheet-loaded activated carbon fiber felt.
(3) Preparing the activated carbon fiber felt loaded by the magnesium oxide porous nanosheets: and (3) putting the sample in the step (2) into a muffle furnace, and annealing for 10H at 500 ℃ under the protection of argon gas to obtain the activated carbon fiber felt loaded by the magnesium oxide porous nanosheet.
Example 8
Referring to fig. 5, fig. 5 shows a preparation method of a magnesium oxide porous nanomaterial loaded activated carbon fiber felt, which includes the following steps:
(1) activation of the activated carbon fiber felt: firstly, washing the activated carbon fiber felt with clear water for 4 times, then immersing the activated carbon fiber felt in a high-pressure kettle filled with water, preserving the heat for 4 hours at the temperature of 150 ℃, then taking out the activated carbon fiber felt, and putting the activated carbon fiber felt into a drying oven at the temperature of 70 ℃ for drying to obtain the activated carbon fiber felt.
(2) Loading of the magnesium oxide precursor on the activated carbon fiber felt: dissolving urea and magnesium nitrate in deionized water to form a transparent solution with the concentration of 0.4%, and then soaking the activated carbon fiber felt treated in the step (1) in the transparent solution for 12H. Then, the mixture was placed in an autoclave and reacted at 210 ℃ for 16H. And after the reaction is finished, taking out, repeatedly cleaning the activated carbon fiber felt by using clear water for many times, and drying the activated carbon fiber felt in a 70 ℃ drying oven to obtain the precursor basic magnesium carbonate nanosheet-loaded activated carbon fiber felt.
(3) Preparing the activated carbon fiber felt loaded by the magnesium oxide porous nanosheets: and (3) putting the sample in the step (2) into a muffle furnace, and annealing for 12H at 550 ℃ under the protection of argon gas to obtain the activated carbon fiber felt loaded by the magnesium oxide porous nanosheet.
Example 9
Referring to fig. 5, fig. 5 shows a preparation method of a magnesium oxide porous nanomaterial loaded activated carbon fiber felt, which includes the following steps:
(1) activation of the activated carbon fiber felt: firstly, washing the activated carbon fiber for 3 times by using clear water, then immersing the activated carbon fiber in a high-pressure kettle filled with water, preserving heat for 2H at 150 ℃, then taking out the activated carbon fiber, and putting the activated carbon fiber into a drying oven at 70 ℃ for drying to obtain the activated carbon fiber.
(2) Loading on the magnesium oxide precursor re-activated carbon fiber: dissolving urea and magnesium nitrate in deionized water to form a transparent solution with the concentration of 0.5%, and then soaking the activated carbon fiber treated in the step (1) in the solution for 4H. Then, the mixture was placed in an autoclave and reacted at 220 ℃ for 8H. And after the reaction is finished, taking out, repeatedly cleaning the activated carbon fiber by using clear water for many times, and drying the activated carbon fiber in a 70 ℃ drying oven to obtain the precursor basic magnesium carbonate nanosheet-loaded activated carbon fiber.
(3) Preparing the activated carbon fiber loaded by the magnesium oxide porous nanosheet: and (3) putting the sample in the step (2) into a muffle furnace, and annealing for 6H at 500 ℃ under the protection of argon gas to obtain the activated carbon fiber loaded by the magnesium oxide porous nanosheet.
Example 10
Referring to fig. 5, fig. 5 shows a preparation method of a magnesium oxide porous nanomaterial loaded activated carbon fiber felt, which includes the following steps:
(1) activation of the activated carbon fiber felt: firstly, washing the activated carbon fiber with clear water for 5 times, then immersing the activated carbon fiber in a high-pressure kettle filled with water, preserving the heat for 10 hours at 100 ℃, then taking out the activated carbon fiber, and putting the activated carbon fiber into a drying oven at 70 ℃ for drying to obtain the activated carbon fiber.
(2) Loading of the magnesium oxide precursor on the activated carbon fiber: dissolving urea and magnesium nitrate in deionized water to form a transparent solution with the concentration of 0.3%, and then soaking the activated carbon fiber treated in the step (1) in the solution for 2H. Then, the mixture was placed in an autoclave and reacted at 180 ℃ for 12H. And after the reaction is finished, taking out, repeatedly cleaning the activated carbon fiber by using clear water for many times, and drying the activated carbon fiber in a 70 ℃ drying oven to obtain the precursor basic magnesium carbonate nanosheet-loaded activated carbon fiber.
(3) Preparing the activated carbon fiber loaded by the magnesium oxide porous nanosheet: and (3) putting the sample in the step (2) into a tube furnace, and annealing for 3H at 500 ℃ under the protection of nitrogen to obtain the activated carbon fiber loaded by the magnesium oxide porous nanosheet.
In order to more intuitively explain the technical effect of the present invention, please refer to fig. 1 a-1 b, fig. 1a is a photograph of an activated carbon fiber felt before modification, fig. 1b is a photograph of an activated carbon fiber felt after modification, as can be seen from the figures, the activated carbon fiber felt before modification is pure black, however, after the magnesium oxide porous nanosheet is modified, the surface of the activated carbon fiber felt is covered with a layer of white substance, which proves the modification of magnesium oxide on the surface thereof;
referring to fig. 2, it can be seen that the XRD spectrum of the activated carbon fiber mat has no obvious diffraction peak, only two steamed bread peaks; the XRD of the precursor modified magnesium oxide activated carbon fiber felt shows a plurality of small peaks which can be identified as the diffraction peak (Mg) of basic magnesium carbonate5(CO3)4(OH)2·(H2O)4That is, the diffraction peak of the magnesium oxide precursor also proves that the precursor is modified on the activated carbon fiber felt, and the XRD pattern of the activated carbon fiber felt modified by the magnesium oxide porous nanosheet is very obvious, so that all peak values can correspond to (200), (220), (311) and (222) planes of a magnesium oxide hexagonal structure (JCPDS89-4248), and the magnesium oxide porous nanosheet is also proved to be successfully modified on the activated carbon fiber felt;
referring to fig. 3a-3b, fig. 3a-3b are SEM images of activated carbon fiber mat with different magnifications, and it can be seen that the activated carbon fiber mat is irregular strip-shaped, has a smooth surface, and has no other substances attached to the surface;
referring to fig. 3c-3e, SEM images of different magnifications of the activated carbon fiber felt modified by the magnesium oxide porous nanosheets show that the activated carbon fiber surface is modified with a large amount of flaky magnesium oxide materials, and the magnesium oxide sheets are arranged closely and distributed uniformly. Gaps exist among the sheets, so that the magnesium oxide nano sheet can maintain the specific advantages of the nano material in the application of removing pollutants in water through subsequent adsorption;
referring to fig. 3f, fig. 3f is a TEM image of the ultrasonically dispersed magnesium oxide nanosheet modified on the surface of the activated carbon fiber, from which it can be found that the magnesium oxide material has a lamellar structure and a large number of nanopores exist across the magnesium oxide nanosheet. These nanopores are difficult to observe clearly from SEM images due to their small size. The characterization results of SEM and TEM show that the activated carbon fiber felt modified by the magnesium oxide porous nanosheet is successfully synthesized.
Referring to fig. 4, fig. 4 is a drawing showing isothermal adsorption of fluorine ions in water by the activated carbon fiber felt modified by the magnesium oxide porous nanosheet. As can be seen from the figure, the adsorption capacity of the activated carbon fiber felt modified by the magnesium oxide porous nanosheet is stronger as the concentration of the fluorine ions in the water increases, and the saturated adsorption capacity of the activated carbon fiber felt on the fluorine ions in the water can exceed 46.5mg/g at most. In conclusion, the experimental results show that the prepared defluorination composite material has a large effect on removing low-fluorine water and a high removal rate, and is an extremely high-efficiency defluorination material.
The preferred embodiments of the invention disclosed above are intended to be illustrative only. The preferred embodiments are not intended to be exhaustive or to limit the invention to the precise embodiments disclosed. Obviously, many modifications and variations are possible in light of the above teaching. The embodiments were chosen and described in order to best explain the principles of the invention and the practical application, to thereby enable others skilled in the art to best utilize the invention. The invention is limited only by the claims and their full scope and equivalents.

Claims (10)

1. A preparation method of a magnesium oxide porous nano material loaded activated carbon fiber felt is characterized by comprising the following steps:
A. activating the activated carbon fiber felt: firstly, washing an activated carbon fiber felt for a plurality of times by using clean water, then immersing the activated carbon fiber felt in a closed container filled with water, activating for a certain time at a certain temperature, taking out, and drying at a low temperature to obtain the activated carbon fiber felt;
B. loading of the magnesium oxide precursor on the activated carbon fiber felt: dissolving a hydroxyl slow-release agent and a magnesium salt in deionized water to form a transparent solution with a certain concentration, immersing the activated carbon fiber felt treated in the step A in the transparent solution for a certain time, taking out, putting the activated carbon fiber felt into a high-pressure kettle, reacting at a high temperature for a certain time, taking out, repeatedly washing with clear water for multiple times, and drying at a low temperature to obtain the activated carbon fiber felt loaded by the basic magnesium carbonate nanosheets;
C. preparing the activated carbon fiber felt loaded by the magnesium oxide porous nanosheets: and D, putting the activated carbon fiber felt processed in the step B into a muffle furnace, and annealing for a certain time in a protective gas or vacuum environment to obtain the activated carbon fiber felt loaded by the magnesium oxide porous nanosheet, wherein the loading capacity of the magnesium oxide is over 40%.
2. The preparation method of the magnesium oxide porous nanomaterial-supported activated carbon fiber felt according to claim 1, wherein the activation treatment in the step A is a treatment at a temperature of 80-150 ℃ for 2-48H.
3. The preparation method of the magnesium oxide porous nanomaterial loaded activated carbon fiber felt according to claim 1, wherein the low-temperature drying in the step A and the step B is drying in an oven at 40-80 ℃.
4. The preparation method of the magnesium oxide porous nanomaterial-supported activated carbon fiber felt according to claim 1, wherein the hydroxide release agent in the step B is a chemical that is decomposed by urea and hexamethyleneimine at a high temperature to generate hydroxide.
5. The method for preparing the magnesium oxide porous nanomaterial-supported activated carbon fiber mat according to claim 1, wherein the magnesium salt in the step B is a soluble magnesium salt formed by a combination of one or more of magnesium chloride, magnesium nitrate, magnesium sulfate, magnesium phosphate and magnesium oxalate.
6. The method for preparing the magnesium oxide porous nanomaterial-supported activated carbon fiber felt according to claim 1, wherein the transparent solution with a certain concentration in the step B is a mixed solution of urea with a concentration of 0.01-0.5% and magnesium salt with a concentration of 0.01-0.5%.
7. The method for preparing the magnesium oxide porous nanomaterial loaded activated carbon fiber felt according to claim 1, wherein in the step B, the activated carbon fiber felt treated in the step A is immersed in a transparent solution for 0.5-12H and then taken out.
8. The method for preparing the magnesium oxide porous nanomaterial-supported activated carbon fiber felt according to claim 1, wherein in the step B, the high-temperature reaction for a certain time is performed by keeping the temperature of 6-24H in an autoclave at 120-220 ℃.
9. The preparation method of the magnesium oxide porous nanomaterial-supported activated carbon fiber mat according to claim 1, wherein the shielding gas in the step C is nitrogen or argon.
10. The method for preparing the magnesia porous nanomaterial-supported activated carbon fiber felt according to claim 1, wherein in the step C, the annealing for a certain time is performed in a muffle furnace at a temperature of 250-550 ℃ for 2-12H.
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