CN109876771B - Loofah activated carbon aerogel material, and preparation method and application thereof - Google Patents
Loofah activated carbon aerogel material, and preparation method and application thereof Download PDFInfo
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Abstract
本发明属于吸附材料领域，具体涉及一种丝瓜活性炭气凝胶材料、其制备方法和应用。该丝瓜活性炭气凝胶材料为以琼脂糖掺杂丝瓜络活性炭为孔壁，形成弹性变形的三维贯通的均匀海绵状结构，丝瓜络活性炭均匀分布在孔壁的表面和内部，附着在孔壁表面的丝瓜络活性炭表面包裹琼脂糖。其制备方法为将丝瓜络活性炭置于琼脂糖水溶液中恒温搅拌均匀，冷藏形成水凝胶后，冷冻干燥，制得丝瓜活性炭气凝胶材料。本发明制备工艺简单，设备要求低，成本低廉，环境友好，制得的丝瓜活性炭气凝胶材料外观完整，轻便易携带，超亲水性和高弹性变形性，抗生素的吸附性能优异，尤其适于超低浓度抗生素的吸附，且可重复回收使用。
The invention belongs to the field of adsorption materials, in particular to a loofah activated carbon aerogel material, a preparation method and application thereof. The loofah activated carbon aerogel material uses agarose doped loofah activated carbon as the pore wall to form an elastically deformed three-dimensional through uniform sponge-like structure. The loofah activated carbon is evenly distributed on the surface and inside of the pore wall, and is attached to the surface of the pore wall The surface of the loofah activated carbon is coated with agarose. The preparation method includes placing the loofah activated carbon in an aqueous agarose solution and stirring evenly at a constant temperature, refrigerating to form a hydrogel, and then freeze-drying to obtain the loofah activated carbon aerogel material. The preparation process of the invention is simple, the equipment requirement is low, the cost is low, and the environment is friendly. The prepared loofah activated carbon aerogel material has a complete appearance, is light and easy to carry, has super hydrophilicity and high elastic deformation, and has excellent adsorption performance of antibiotics, and is especially suitable for It is suitable for the adsorption of ultra-low concentration antibiotics and can be recycled and reused.
Description
Technical Field
The invention belongs to the field of adsorption materials, and particularly relates to a towel gourd activated carbon aerogel material, and a preparation method and application thereof.
Background
The loofah sponge activated carbon is light, porous, amorphous, high in specific surface area, super-hydrophilic, scalable, biocompatible and strong in adsorbability, environment-friendly, non-toxic and harmless, low in manufacturing cost, and has high antibiotic adsorbability, especially strong adsorbability on antibiotics such as ofloxacin, norfloxacin and tetracycline, so that the loofah sponge activated carbon is paid much attention by researchers.
In recent years, various types of antibiotic adsorbents have been reported in large numbers, such as: activated carbon, polyacrylamide, and the like. However, most of the currently reported adsorbents are granular, are not easy to carry, and have poor adsorption performance and recovery performance. The loofah activated carbon aerogel material prepared by the invention solves the problems of difficult carrying, poor adsorption, low recovery rate and easy loss of the existing granular adsorbent, and also has the advantages of light weight, easy carrying, batch production, low manufacturing cost, small environmental pollution and the like. In addition, experiments prove that the towel gourd activated carbon aerogel prepared by the invention has excellent adsorption performance on antibiotics with ultralow concentration.
Disclosure of Invention
The invention aims to provide a towel gourd activated carbon aerogel material which is light in weight, easy to carry and recycle, super-hydrophilic and high in elastic deformability, strong in antibiotic adsorption, particularly excellent in antibiotic adsorption performance at ultra-low concentration, recyclable and reusable, environment-friendly, low in manufacturing cost and easy in obtaining of raw materials.
The invention also provides a preparation method of the luffa activated carbon aerogel material, and the preparation method is simple, convenient, easy to control, easy to operate, low in cost, and non-toxic and pollution-free to the environment.
The invention also provides application of the luffa activated carbon aerogel material in the aspect of an adsorbent.
The technical scheme of the invention is that the loofah sponge activated carbon aerogel material is characterized in that agarose is doped with loofah sponge activated carbon to serve as a hole wall, an elastic deformation three-dimensional through uniform sponge-like structure is formed, the loofah sponge activated carbon is uniformly distributed on the surface and inside the hole wall, and the surface of the loofah sponge activated carbon attached to the surface of the hole wall is coated with the agarose. The luffa activated carbon aerogel material has good compressibility and recoverability, does not damage the structure of the luffa activated carbon aerogel material in the deformation and recovery process, and is an elastic deformation material with good performance.
The pore diameter of the sponge structure is 4-6 μm, preferably 5 μm; the porosity is 60% to 75%, preferably 70%.
The preparation method of the towel gourd activated carbon aerogel material comprises the following steps: adding powdered loofah sponge activated carbon into agarose aqueous solution, uniformly stirring at constant temperature, refrigerating to form hydrogel, and freeze-drying to obtain the loofah sponge activated carbon aerogel material. Specifically, under the state of constant-temperature stirring, adding powdered loofah sponge activated carbon into an agarose aqueous solution, and uniformly stirring, wherein the constant-temperature stirring temperature is 60-90 ℃, and preferably 80-90 ℃; the rotation speed of the constant-temperature stirring is 2000-3000 rpm/min, preferably 2500-3000 rpm/min.
Preparing a uniform mixed solution of the loofah sponge activated carbon and the agarose aqueous solution by a hydrothermal method, further uniformly distributing the loofah sponge activated carbon and the agarose by adjusting the rotating speed, and refining the particle size of the powdery loofah sponge activated carbon.
The concentration of the agarose aqueous solution is 2-10 g/L, preferably 4-9 g/L.
In a uniform mixing system of the loofah sponge activated carbon and the agarose aqueous solution, the mass ratio of the loofah sponge activated carbon to the agarose is 1: 0.5 to 2.5, preferably 1: 1 to 1.5, more preferably 1: 1.2 to 1.3.
The particle size of the powdery loofah sponge activated carbon is 1-75 μm, preferably 10-25 μm.
Stirring at constant temperature of 60-90 ℃ and at the rotating speed of 2000-3000 rpm/min, wherein the constant-temperature stirring temperature is preferably 80-90 ℃; the rotation speed of constant-temperature stirring is preferably 2500-3000 rpm/min.
Uniformly stirring powdered loofah sponge active carbon and agarose aqueous solution at constant temperature, and refrigerating to form hydrogel.
And (3) refrigerating at 10-15 ℃ for 5-10 h to form hydrogel, wherein the refrigerating temperature is preferably 10-13 ℃, the refrigerating time is preferably 8-10 h, and the optimal scheme is that the hydrogel is formed by refrigerating at 10 ℃ for 10 h.
Freeze-drying at-50 to-30 ℃ for 24 to 48 hours to prepare the luffa activated carbon aerogel material; the freeze drying temperature is preferably-50 ℃ to-40 ℃; the preferable freeze drying time is 30-48 h, and the preferable scheme is that the towel gourd activated carbon aerogel material is prepared by freeze drying for 48h at-45 ℃.
The preparation method of the loofah sponge activated carbon comprises the following steps: and carbonizing the loofah sponge at constant temperature in the protective gas atmosphere to form the loofah sponge activated carbon. Specifically, the loofah sponge is placed in a carbonization furnace, and is carbonized at constant temperature in a protective gas atmosphere to form the loofah sponge activated carbon. The carbonization furnace is a tubular furnace. The protective gas is at least one of argon, nitrogen or helium, and preferably argon; the purity of the protective gas is 95 to 99.9 percent, and the preferred purity is 99.9 percent.
Heating to 600-800 ℃ at the speed of 2-4 ℃/min and carbonizing for 6-10 h to form loofah sponge active carbon; the temperature rising speed is preferably 2-3 ℃/min, the carbonization temperature is preferably 750-800 ℃, the carbonization time is preferably 6-8 h, and as the preferred scheme, the temperature rising speed is 3 ℃/min to 800 ℃ for carbonization for 6h, so as to form the loofah sponge activated carbon.
The preparation method of the agarose aqueous solution comprises the following steps: and dissolving agarose in deionized water, and stirring uniformly at constant temperature to obtain an agarose aqueous solution. Specifically, under the state of constant-temperature stirring, agarose is dissolved in deionized water and is uniformly stirred; the constant-temperature stirring temperature is 60-90 ℃, and preferably 70-80 ℃; the rotation speed of the constant-temperature stirring is 2000-3000 rpm/min, preferably 2500-3000 rpm/min. The centripetal force provided by the constant-temperature stirring rotating speed promotes the agarose to be quickly and uniformly dissolved in the solution, is beneficial to the quick and uniform distribution of the agarose in the solution, promotes the diffusion of substances, accelerates the dissolution process of the agarose, and prevents the generation of precipitates.
Stirring at constant temperature of 60-90 ℃ and at the rotating speed of 2000-3000 rpm/min, wherein the constant-temperature stirring temperature is preferably 70-80 ℃; the rotation speed of constant-temperature stirring is preferably 2500-3000 rpm/min.
The dosage ratio of the agarose to the deionized water is 2-10 g/L, preferably 4-9 g/L.
As a preferred embodiment of the present invention, a method for preparing a luffa activated carbon aerogel material comprises the steps of: adding powdered loofah sponge activated carbon into 5g/L agarose aqueous solution at 90 ℃ and 2500rpm/min, and uniformly mixing, wherein the mass ratio of the loofah sponge activated carbon to the agarose is 1: 1.2-1.3, refrigerating at 10 ℃ for 10h to form hydrogel, and freeze-drying at-45 ℃ for 48h to obtain the luffa activated carbon aerogel material.
The loofah activated carbon aerogel material prepared by the invention has high porosity, pore diameter and specific surface area, good elastic deformation performance, repeated recycling and good adsorption performance on antibiotics such as ofloxacin, norfloxacin, tetracycline and the like. Can be used for preparing adsorbent, especially antibiotic adsorbent.
An adsorbent comprises the loofah activated carbon aerogel material prepared by the invention. Preferably an antibiotic adsorbent which has antibiotic adsorption activity and can adsorb antibiotics in sewage, wastewater, air and the like, and the towel gourd activated carbon aerogel material prepared by the invention.
Compared with the prior art, the invention has the following advantages:
(1) according to the invention, a hydrothermal method is adopted to prepare a mixed solution of loofah sponge activated carbon and agarose, so that the loofah sponge activated carbon and the agarose in the mixed solution are uniformly distributed; and then freezing and coagulating the gel into hydrogel with complete shape, and then freezing and drying the hydrogel to obtain the luffa activated carbon aerogel material. The contact angle of the luffa activated carbon aerogel material is 0 degrees, and the luffa activated carbon aerogel material is a super-hydrophilic material; the material can be compressed from 1.7cm to 0.5cm and returns to the original appearance after being loosened; namely, the towel gourd activated carbon aerogel material has extremely high hydrophilicity and elastic deformability.
(2) The towel gourd activated carbon aerogel material prepared by the invention has a strong adsorption effect on an antibiotic solution with the concentration of less than 10ppm, and can be used for adsorption treatment of ultralow-concentration antibiotic water pollution.
(3) The preparation method has simple operation, does not need complex equipment, has lower manufacturing cost of the loofah sponge active carbon, can realize batch production, has low cost, and has no toxicity and no pollution to the environment.
(4) The loofah activated carbon aerogel material prepared by the invention has excellent adsorption performance, and can meet the adsorption requirements of antibiotic solutions (ofloxacin, norfloxacin and tetracycline) with different concentration grades.
Drawings
Fig. 1 is a scanning electron microscope picture of the loofah sponge activated carbon.
Fig. 2 is a scanning electron microscope picture of the luffa activated carbon aerogel according to the present invention.
Detailed Description
The invention is described in detail below with reference to the figures and specific embodiments.
Example 1
(1) Preparing loofah sponge active carbon: placing retinervus Luffae fructus in a tube furnace, heating to 800 deg.C at a heating rate of 2 deg.C/min with argon as protective gas, and keeping the temperature for 6h to obtain retinervus Luffae fructus activated carbon, as shown in figure 1.
(2) Preparation of an agarose solution: 200mg of agarose was dissolved in 100mL of deionized water at 70 ℃ at 2000rmp/min to form a homogeneous agarose solution.
(3) Preparing loofah activated carbon agarose gel: grinding the loofah sponge activated carbon prepared in the step (1) into powder, adding the powder into the uniform agarose solution prepared in the step (2) under a continuous stirring state, and stirring at the temperature of 90 ℃ and the rotating speed of 2000rmp/min to form uniform loofah sponge activated carbon and agarose mixed solution, wherein the mass of the loofah sponge activated carbon is 45% of the total mass of the loofah sponge activated carbon and the agarose; placing the loofah sponge activated carbon and agarose mixed solution in a refrigerator at 15 ℃ for refrigeration for 10 hours to obtain loofah sponge activated carbon and agarose hydrogel; transferring the loofah sponge activated carbon and the agarose hydrogel into a vacuum freeze dryer at-50 ℃ for freeze-drying for 48h to obtain the loofah sponge activated carbon aerogel adsorbent, as shown in figure 2.
The loofah sponge activated carbon aerogel prepared in the embodiment is a three-dimensional through uniform sponge-like structure formed by loofah sponge activated carbon and agarose, the loofah sponge activated carbon is attached to a sponge-like hole wall formed by the agarose, and the surface of the loofah sponge activated carbon is coated with the agarose. The aperture of the spongy structure is 4-6 microns, and the apertures are mostly distributed at 5 microns; the porosity is 60-75%, and the porosity is more distributed at 70%, so that the three-dimensional through uniform sponge-like structure formed by the loofah sponge activated carbon and the agarose has good compressibility. Respectively has a concentration of 5 mg.L to the antibiotic solution-1，10mg·L-1，15mg·L-1，20mg·L-1，25mg·L-1，30mg·L-1，35mg·L-1，40mg·L-1Adsorbing the contaminants (b) to obtain raw data, fitting with Langmuir (Langmuir) formula, and fitting the adsorption results of antibiotics of 10ppm or less to 275mg g-1(Tetracycline), 300 mg. g-1(norfloxacin), 400mg g-1(Ofloxacin).
The loofah activated carbon aerogel prepared in the embodiment can be recycled for three times of adsorption of antibiotics (norfloxacin, ofloxacin and tetracycline), and the adsorption amount of each cycle is more than 100 mg/g.
Example 2
(1) Preparing towel gourd activated carbon: placing retinervus Luffae fructus in a tube furnace, taking argon as protective gas, heating to 750 deg.C at a heating rate of 4 deg.C/min, and keeping the temperature for 8h to obtain retinervus Luffae fructus activated carbon with structure shown in figure 1.
(2) Preparation of an agarose solution: 396mg of agarose was dissolved in 100mL of deionized water at 60 ℃ at 3000rmp/min to form a homogeneous agarose solution.
(3) Preparing loofah activated carbon agarose gel: grinding the loofah activated carbon prepared in the step (1) into powder, adding the powder into the uniform agarose solution prepared in the step (2) under a continuous stirring state, and stirring at 85 ℃ and 3000rmp/min to form uniform loofah sponge activated carbon and agarose mixed solution, wherein the mass of the loofah sponge activated carbon is 45% of the total mass of the loofah sponge activated carbon and the agarose; placing the loofah sponge activated carbon and agarose mixed solution in a refrigerator at 10 ℃ for cold storage for 5 hours to obtain loofah sponge activated carbon and agarose hydrogel; transferring the loofah sponge activated carbon and the agarose hydrogel into a vacuum freeze dryer at the temperature of-45 ℃, and freeze-drying for 36 hours to obtain the loofah sponge activated carbon aerogel adsorbent.
The structure of the luffa activated carbon aerogel prepared in this example is similar to that of example 1, and the antibiotic adsorption effect (norfloxacin, ofloxacin, tetracycline) is close to that of example 1.
Example 3
(1) Preparing loofah sponge active carbon: placing retinervus Luffae fructus in a tube furnace, heating to 700 deg.C at a heating rate of 3 deg.C/min with argon as protective gas, and maintaining for 10h to obtain retinervus Luffae fructus activated carbon with structure shown in figure 1.
(2) Preparation of an agarose solution: 500mg of agarose was dissolved in 100mL of deionized water at 80 ℃ and 2500rmp/min to form a homogeneous agarose solution.
(3) Preparing loofah activated carbon agarose gel: grinding the loofah sponge activated carbon prepared in the step (1) into powder, adding the powder into the uniform agarose solution prepared in the step (2) under a continuous stirring state, and stirring at the temperature of 80 ℃ and the rotating speed of 2500rmp/min to form uniform loofah sponge activated carbon and agarose mixed solution, wherein the mass of the loofah sponge activated carbon is 60% of the total mass of the loofah sponge activated carbon and the agarose; placing the loofah sponge activated carbon and agarose mixed solution in a refrigerator at 13 ℃ for cold storage for 8 hours to obtain loofah sponge activated carbon and agarose hydrogel; transferring the loofah sponge activated carbon and the agarose hydrogel into a vacuum freeze dryer at the temperature of-30 ℃, and freeze-drying for 48 hours to obtain the loofah sponge activated carbon aerogel adsorbent.
The structure of the luffa activated carbon aerogel prepared in this example is similar to that of example 1, and the antibiotic adsorption effect (norfloxacin, ofloxacin, tetracycline) is close to that of example 1.
Example 4
(1) Preparing loofah sponge active carbon: placing retinervus Luffae fructus in a tube furnace, heating to 760 deg.C at a heating rate of 3 deg.C/min with argon as protective gas, and maintaining for 10h to obtain retinervus Luffae fructus activated carbon with structure shown in figure 1.
(2) Preparation of an agarose solution: 900mg of agarose was dissolved in 100mL of deionized water at 90 ℃ and 2500rmp/min to form a homogeneous agarose solution.
(3) Preparing loofah activated carbon agarose gel: grinding the loofah sponge activated carbon prepared in the step (1) into powder, adding the powder into the uniform agarose solution prepared in the step (2) under a continuous stirring state, and stirring at the temperature of 90 ℃ and the rotating speed of 3000rmp/min to form uniform loofah sponge activated carbon and agarose mixed solution, wherein the mass of the loofah sponge activated carbon is 55% of the total mass of the loofah sponge activated carbon and the agarose; placing the mixed solution of the loofah sponge activated carbon and the agarose in a refrigerator at 15 ℃ for refrigeration for 6 hours to obtain loofah sponge activated carbon and agarose hydrogel; transferring the loofah sponge activated carbon and the agarose hydrogel into a vacuum freeze dryer at the temperature of-50 ℃, and freeze-drying for 24 hours to obtain the loofah sponge activated carbon aerogel adsorbent.
The structure of the luffa activated carbon aerogel prepared in this example is similar to that of example 1, and the antibiotic adsorption effect (norfloxacin, ofloxacin, tetracycline) is close to that of example 1.
Example 5
(1) Preparing loofah sponge active carbon: placing retinervus Luffae fructus in a tube furnace, taking argon as protective gas, heating to 780 deg.C at a heating rate of 2 deg.C/min, and keeping the temperature for 7h to obtain retinervus Luffae fructus activated carbon with structure shown in figure 1.
(2) Preparation of an agarose solution: 710mg of agarose was dissolved in 100mL of deionized water at 75 ℃ and 2500rmp/min to form a homogeneous agarose solution.
(3) Preparing loofah activated carbon agarose gel: grinding the loofah sponge activated carbon prepared in the step (1) into powder, adding the powder into the uniform agarose solution prepared in the step (2) under a continuous stirring state, and stirring at 85 ℃ and 3000rmp/min to form uniform loofah sponge activated carbon and agarose mixed solution, wherein the mass of the loofah sponge activated carbon is 40% of the total mass of the loofah sponge activated carbon and the agarose; placing the loofah sponge activated carbon and agarose mixed solution in a refrigerator at 10 ℃ for cold storage for 10 hours to obtain loofah sponge activated carbon and agarose hydrogel; transferring the loofah sponge activated carbon and the agarose hydrogel into a vacuum freeze dryer at the temperature of-45 ℃, and freeze-drying for 30h to obtain the loofah sponge activated carbon aerogel adsorbent.
The structure of the luffa activated carbon aerogel prepared in this example is similar to that of example 1, and the antibiotic adsorption effect (norfloxacin, ofloxacin, tetracycline) is close to that of example 1.
The above embodiments are described to facilitate understanding and use by those of ordinary skill in the art. It will be readily apparent to those skilled in the art that various modifications to these embodiments may be made, and the generic principles described herein may be applied to other embodiments without the use of the inventive faculty. Therefore, the present invention is not limited to the above embodiments, and those skilled in the art can make improvements and modifications within the scope of the present invention based on the disclosure of the present invention.
Claims (5)
1. A loofah sponge activated carbon aerogel material is characterized in that agarose is doped with loofah sponge activated carbon to serve as a hole wall, an elastic deformation three-dimensional through uniform sponge-like structure is formed, the loofah sponge activated carbon is uniformly distributed on the surface and inside the hole wall, and the surface of the loofah sponge activated carbon attached to the surface of the hole wall is wrapped with the agarose;
the aperture of the spongy structure is 4-6 mu m, and the porosity is 60-75%;
the preparation method comprises the following steps: adding powdery loofah sponge activated carbon into an agarose aqueous solution, uniformly stirring at a constant temperature, stirring at a constant temperature of 60-90 ℃ and a rotation speed of 2000-3000 rpm/min, refrigerating at 10-15 ℃ for 5-10 h to form hydrogel, and freeze-drying at-50-30 ℃ for 24-48 h to obtain a loofah sponge activated carbon aerogel material; the concentration of the agarose aqueous solution is 2-10 g/L; in a uniform mixing system of the loofah sponge activated carbon and the agarose aqueous solution, the mass ratio of the loofah sponge activated carbon to the agarose is 1: 0.5 to 2.5;
the preparation method of the loofah sponge activated carbon comprises the following steps: under the protective gas atmosphere, the temperature of the loofah sponge is raised to 600-800 ℃ at the speed of 2-4 ℃/min, and the loofah sponge is carbonized at constant temperature for 6-10 hours to form loofah sponge active carbon, wherein the protective gas is at least one of argon, nitrogen or helium.
2. The luffa activated carbon aerogel material according to claim 1, wherein the preparation method of the agarose aqueous solution comprises: and dissolving agarose in deionized water, and stirring uniformly at constant temperature to obtain an agarose aqueous solution.
3. The luffa activated carbon aerogel material of claim 2, wherein the luffa activated carbon aerogel material is stirred at a constant temperature of 60-90 ℃ and a rotation speed of 2000-3000 rpm/min, and a dosage ratio of agarose to deionized water is 2-10 g/L.
4. Use of the loofah sponge activated carbon aerogel material according to any one of claims 1 to 3 for preparing an antibiotic adsorbent.
5. An antibiotic adsorbent comprising the luffa activated carbon aerogel material according to any one of claims 1 to 3.
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| CN111644158A (en) * | 2020-05-19 | 2020-09-11 | 浙江省农业科学院 | Carbon-based adsorbent for removing phosphate in solution |
| CN113077994B (en) * | 2021-02-24 | 2022-11-08 | 辽宁博艾格电子科技有限公司 | Electrode plate for super capacitor and preparation method thereof |
| CN114507361B (en) * | 2022-02-28 | 2024-01-19 | 新疆农业大学 | Agar activated carbon hydrogel for soilless culture seeds and preparation method thereof |
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