CN110681364B - Loofah sponge based activated carbon hydrogel material and preparation method and application thereof - Google Patents
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Abstract
The invention provides a loofah sponge based activated carbon hydrogel material and a preparation method and application thereof. The preparation method of the loofah sponge based activated carbon hydrogel material comprises the following steps: (1) carbonizing retinervus Luffae fructus at high temperature to obtain retinervus Luffae fructus-based activated carbon LAC; (2) grinding the LAC into a powder; (3) adding PVA powder into distilled water, stirring, heating, preserving heat and cooling to obtain a PVA solution; (4) adding LAC powder into the PVA solution, and performing ultrasonic dispersion to obtain a mixed solution A; (5) adding sodium alginate into the mixed solution A, and stirring to obtain a mixed solution B; (6) dropping the mixed solution A into CaCl 2 And (5) dissolving in an aqueous solution to obtain the compound. Compared with the prior art, the preparation method has the advantages of simple preparation process, low equipment requirement and low cost, and the prepared loofah sponge-based activated carbon hydrogel material has complete appearance, can be used for adsorbing antibiotics in water, has excellent adsorption performance on the antibiotics, and has continuous adsorption capacity.
Description
Technical Field
The invention belongs to the field of preparation of green environment-friendly materials, and particularly relates to a loofah sponge based activated carbon hydrogel material and a preparation method and application thereof.
Background
The loofah sponge-based activated carbon has a large specific surface area, is low in loofah sponge cost, is harmless to the environment, and has ultrahigh antibiotic adsorption performance; particularly, the adsorption performance of the solution of three antibiotics of ofloxacin, norfloxacin and tetracycline is good, and the solution has very high super-hydrophilicity, telescopic performance and good biocompatibility; and the method has the advantages of environmental friendliness, no toxicity, no harm, low cost and the like, so that the method has excellent adsorption capacity when adsorbing the ultra-low concentration antibiotics. In addition, the surface structure of the loofah sponge-based active carbon material and the excellent adsorption capacity of the loofah sponge-based gel to the antibiotic solution are concerned by the majority of researchers.
In recent years, a great number of methods for preparing various antibiotic adsorbents have been reported, such as: activated carbon, polyacrylamide, and the like. However, the activated carbon is difficult to recycle due to the granular or powdery form, and the application range of the activated carbon is greatly limited. The research focuses on the unique structural characteristics of the natural loofah and the unique gelling capacity of the sodium alginate, and the loofah sponge-based activated carbon sodium alginate (LAC-SA) globule which can be recycled and massively prepared is prepared.
Disclosure of Invention
The invention aims to overcome the defects of the adsorbent and provide a loofah sponge based activated carbon hydrogel material and a preparation method and application thereof.
The invention is realized by the following technical scheme:
a preparation method of a loofah sponge based active carbon hydrogel material comprises the following steps:
(1) carbonizing retinervus Luffae fructus at high temperature to obtain retinervus Luffae fructus-based activated carbon LAC;
(2) grinding loofah sponge-based activated carbon LAC into powder to obtain LAC powder;
(3) adding polyvinyl alcohol (PVA) powder into distilled water, stirring at 2500-3500 rpm, heating to 80-100 ℃, keeping the temperature at 80-100 ℃ for 1-3 h, and cooling to room temperature to obtain a PVA solution;
(4) adding LAC powder into the PVA solution, and performing ultrasonic dispersion for 5-8 hours to obtain a mixed solution A;
(5) adding sodium alginate into the mixed solution A, and stirring at 2000-3000rpm for 1-6 h to obtain a mixed solution B;
(6) dripping the mixed solution B into CaCl with the mass fraction of 1-15wt% at the speed of 10-20mL/min 2 And (3) obtaining loofah sponge based activated carbon sodium alginate (LAC-SA) black hydrogel spheres, namely the loofah sponge based activated carbon hydrogel material, from the aqueous solution.
The high-temperature carbonization conditions are as follows: taking argon as a protective gas, heating to 700-1000 ℃ at a speed of 2-5 ℃/speed, and preserving heat for 6-8 hours at 700-1000 ℃.
The concentration of the PVA solution is 1-10 g/L.
The concentration of the cucurbituril-based activated carbon in the mixed solution A is 1-10 g/L. In the ultrasonic dispersion process, mixing and stirring a PVA solution and loofah sponge-based active carbon particles to form a uniform mixed solution; the ultrasonic time of several hours makes the particles of the loofah sponge based active carbon smaller and more uniform to mix with the PVA solution.
Preferably, the sodium alginate in the step (5) is added in batches under the condition that the stirring speed is 2000-3000rpm, so that the sodium alginate is fully and uniformly mixed.
Preferably, the concentration of the sodium alginate in the mixed solution B is 8-21 g/L.
The invention also provides a loofah sponge based activated carbon hydrogel material prepared by any one of the methods.
Preferably, the diameters of the loofah sponge based activated carbon hydrogel materials are uniformly distributed at 2-10 mm.
The loofah sponge based activated carbon hydrogel material has good recycling adsorbability.
The invention successfully prepares loofah sponge based activated carbon sodium alginate (LAC-SA) pellets with the diameter of 2-10 mm by using an external emulsification method, uniformly distributes the loofah sponge based activated carbon sodium alginate (LAC-SA) pellets by stirring a sodium alginate solution with a certain concentration and a loofah activated carbon mixed solution, and slowly drops CaCl 2 And (4) obtaining the loofah sponge based active carbon hydrogel material in the solution.
The loofah sponge-based activated carbon hydrogel material can be used for adsorbing antibiotics in water. The antibiotics include ofloxacin (OFO), Norfloxacin (NFO) and Tetracycline (TC).
An antibiotic adsorbent contains the loofah sponge based active carbon hydrogel material.
Compared with the prior art, the invention has the following advantages:
(1) the invention adopts an external emulsification method to successfully prepare a large amount of loofah sponge based activated carbon sodium alginate (LAC-SA) beads with the diameter of 2-10 mm. The loofah sponge-based activated carbon (LAC) is loaded in the Sodium Alginate (SA) gel pellets, is uniformly distributed and has an integral structure.
(2) The experiment researches the adsorption mechanism, adsorption capacity and cyclic adsorption performance of LAC-SA pellets for adsorbing Ofloxacin (OFL), Norfloxacin (NOR) and Tetracycline (TC). The cyclic adsorption data further prove that the LAC-SA adsorbent has continuous adsorption capacity, can be recycled for multiple times, keeps the adsorption capacity above 90% of the initial adsorption all the time, and is an effective adsorbent for adsorbing antibiotics in water, wherein the accumulated total adsorption amount exceeds 700mg/g after ten times of circulation.
(3) The preparation method has the advantages of simple operation, no need of complex equipment, low cost, no toxicity or harm to the environment and no pollution.
Drawings
In fig. 1, (a) is a photograph of a sample of the loofah activated carbon sodium alginate microsphere of the present invention, and (b) is a low-power scanning electron microscope picture of the loofah activated carbon of the present invention.
Detailed Description
Example 1
The preparation method of the loofah sponge based activated carbon (LAC) comprises the following steps: placing retinervus Luffae fructus in the middle of a tubular furnace under the action of argon gas as shielding gas, heating to 900 deg.C at a speed of 4 deg.C/min, maintaining for 6 hr, naturally cooling to room temperature to obtain retinervus Luffae fructus-based activated carbon (LAC), placing retinervus Luffae fructus-based activated carbon (LAC) in an agate mortar, and grinding into powder to obtain LAC powder, which is used as shown in figure 1 (b).
Adding 200mg of PVA powder (60 mesh, model 1750, Shandong Youyxue chemical technology Co., Ltd.) into a beaker containing 100mL of distilled water, stirring at 2500rpm, and heating to room temperatureKeeping the temperature at 90 ℃ for 1h, and cooling to room temperature to obtain a PVA solution. 200mg of LAC powder was added to the PVA solution and ultrasonically dispersed for 5 hours to obtain a mixed solution A. 1g of Sodium Alginate (SA) was added to the mixed solution A, and stirred at 3000rpm for 5 hours to obtain a mixed solution B. CaCl with the mass fraction of 5wt% is prepared 2 Adding mixed solution B into the CaCl at a rate of 12mL/min with a needle tube 2 Obtaining loofah sponge based activated carbon sodium alginate (LAC-SA) black hydrogel spheres, namely loofah sponge based activated carbon hydrogel materials, from the aqueous solution, as shown in figure 1 (a). The sample is subjected to an antibiotic adsorption experiment, and has excellent adsorption capacity for antibiotic solutions with different concentrations, so that the sample can effectively adsorb antibiotic pollutants in an aqueous solution.
Antibiotic adsorption experiments were as follows:
respectively preparing ofloxacin (OFO), Norfloxacin (NFO) and Tetracycline (TC) solutions with the concentrations of 5mg/L,10mg/L,15mg/L,20mg/L,25mg/L,30mg/L,35mg/L and 40mg/L, and adding LAC-SA to perform adsorption at 25 ℃, wherein the concentration of the LAC-SA is 20 g/L. After 5h, the obtained data are fitted by a Langmuir formula to obtain the following adsorption results: OFO (91.2564mg g) -1 )>TC(32.5832mg·g -1 )>NFO(25.6186mg·g -1 ). The LAC-SA pellet can be recycled for 10 times, and has total adsorption amount of OFO over 700mg g -1 。
The regeneration method of the loofah sponge based active carbon hydrogel material comprises the following steps: mixing the loofah sponge based active carbon hydrogel material adsorbed with the antibiotics and ethanol according to a solid-to-liquid ratio of 1 g: 15mL of the mixture was mixed, stirred at 200rpm for 24 hours, filtered, and washed with deionized water.
Example 2
The preparation method of the loofah sponge based activated carbon (LAC) comprises the following steps: under the condition of taking argon as protective gas, the loofah sponge is placed in the middle of a tube furnace, the temperature is increased to 850 ℃ at the speed of 3 ℃/min and kept for 6.5 hours, the loofah sponge is naturally cooled to the room temperature to obtain loofah sponge-based activated carbon (LAC), and the loofah sponge-based activated carbon (LAC) is placed in an agate mortar and ground into powder to obtain LAC powder for later use.
Mixing 250mgPVA powder (60 mesh, type 1750 PVA powder)Shandong Youye chemical science and technology Co., Ltd.) was added to a beaker containing 100mL of distilled water, stirred at 3000rpm, warmed to 95 ℃ and stirred and kept warm for 1h, and cooled to room temperature to obtain a PVA solution. 230mg of LAC powder was added to the above PVA solution and ultrasonically dispersed for 7 hours to obtain a mixed solution A, and 1g of Sodium Alginate (SA) was added to the mixed solution A and stirred at 3000rpm for 5.5 hours to obtain a mixed solution B. Preparing CaCl with the mass fraction of 6 wt% 2 Adding the mixed solution B into CaCl at a rate of 13mL/min with a needle tube 2 And (3) obtaining black hydrogel of loofah sponge based activated carbon sodium alginate (LAC-SA), namely the loofah sponge based activated carbon hydrogel material, in the aqueous solution. The sample is subjected to an antibiotic adsorption experiment, and has excellent adsorption capacity for antibiotic solutions with different concentrations, so that the sample can effectively adsorb antibiotic pollutants in an aqueous solution.
Antibiotic adsorption experiments were as follows:
respectively preparing ofloxacin (OFO), Norfloxacin (NFO) and Tetracycline (TC) solutions with the concentrations of 5mg/L,10mg/L,15mg/L,20mg/L,25mg/L,30mg/L,35mg/L and 40mg/L, and adding LAC-SA to perform adsorption at 25 ℃, wherein the concentration of the LAC-SA is 20 g/L. After 5h, the obtained data are fitted by a Langmuir formula to obtain the following adsorption results: OFO (94.8263mg g) -1 )>TC(34.4376mg·g -1 )>NFO(27.4125mg·g -1 ). The LAC-SA pellet can be recycled for 10 times, and has total adsorption amount of OFO over 700mg g -1 。
The regeneration method of the loofah sponge based active carbon hydrogel material comprises the following steps: mixing the loofah sponge based active carbon hydrogel material adsorbed with the antibiotics and ethanol according to a solid-to-liquid ratio of 1 g: 15mL of the mixture was mixed, stirred at 200rpm for 24 hours, filtered, and washed with deionized water.
Example 3
The preparation method of the loofah sponge based activated carbon (LAC) comprises the following steps: under the condition of taking argon as protective gas, the loofah sponge is placed in the middle of a tubular furnace, the temperature is raised to 830 ℃ at the heating rate of 4 ℃/min, then the temperature is kept for 7h, the loofah sponge-based activated carbon (LAC) is obtained by naturally cooling to the room temperature, and then the loofah sponge-based activated carbon (LAC) is placed into an agate mortar and ground into powder, so that LAC powder is obtained for later use.
220mg of PVA powder (namely polyvinyl alcohol powder, 60 meshes, model of 1750, Shandong Youyxue chemical science and technology Co., Ltd.) is added into 100mL of distilled water, stirred at 3000rpm, heated to 93 ℃, kept for 1.5h, and cooled to room temperature to obtain a PVA solution. 200mg of LAC powder was added to the above PVA solution and ultrasonically dispersed for 6 hours to obtain a mixed solution A, and 1g of Sodium Alginate (SA) was added to the mixed solution A and stirred at 3000rpm for 5 hours to obtain a mixed solution B. Preparing CaCl with the mass fraction of 7 wt% 2 Adding the mixed solution B into CaCl at a rate of 14mL/min with a needle tube 2 And (3) obtaining loofah sponge based activated carbon sodium alginate (LAC-SA) black hydrogel spheres, namely the loofah sponge based activated carbon hydrogel material, from the aqueous solution. The sample is subjected to an antibiotic adsorption experiment, and has excellent adsorption capacity for antibiotic solutions with different concentrations, so that the sample can effectively adsorb antibiotic pollutants in an aqueous solution.
Antibiotic adsorption experiments were as follows:
respectively preparing ofloxacin (OFO), Norfloxacin (NFO) and Tetracycline (TC) solutions with the concentrations of 5mg/L,10mg/L,15mg/L,20mg/L,25mg/L,30mg/L,35mg/L and 40mg/L, and adding LAC-SA to perform adsorption at 25 ℃, wherein the concentration of the LAC-SA is 20 g/L. After 5h, the obtained data are fitted by a Langmuir formula to obtain the following adsorption results: OFO (92.6814mg g) -1 >TC(33.6731mg·g -1 )>NFO(26.3217mg·g -1 ). The LAC-SA pellet can be recycled for 10 times, and has total adsorption amount of OFO over 700mg g -1 。
The regeneration method of the loofah sponge based active carbon hydrogel material comprises the following steps: mixing the loofah sponge based active carbon hydrogel material adsorbed with the antibiotics and ethanol according to a solid-to-liquid ratio of 1 g: 15mL of the mixture was mixed, stirred at 200rpm for 24 hours, filtered, and washed with deionized water.
Example 4
The preparation method of the loofah sponge based activated carbon (LAC) comprises the following steps: under the condition of taking argon as protective gas, the loofah sponge is placed in the middle of a tube furnace, the temperature is increased to 830 ℃ at the heating rate of 4 ℃/min, and then the temperature is kept for 8 h. Naturally cooling to room temperature to obtain loofah sponge-based activated carbon (LAC), and then putting the loofah sponge-based activated carbon (LAC) into an agate mortar and grinding into powder to obtain LAC powder for later use.
220mg of PVA powder (namely polyvinyl alcohol powder, 60 meshes, model of 1750, Shandong Youyxue chemical science and technology Co., Ltd.) is added into 100mL of distilled water, stirred at 2500rpm, heated to 93 ℃, kept for 2 hours, and cooled to room temperature to obtain a PVA solution. 200mg of LAC powder was added to the above PVA solution and ultrasonically dispersed for 8 hours to obtain a mixed solution A, and 1g of Sodium Alginate (SA) was added to the mixed solution A and stirred at 3000rpm for 5 hours to obtain a mixed solution B. Preparing CaCl with the mass fraction of 7 wt% 2 Adding the mixed solution B into the CaCl at 15mL/min with a needle tube 2 And (3) obtaining loofah sponge based activated carbon sodium alginate (LAC-SA) black hydrogel spheres, namely the loofah sponge based activated carbon hydrogel material, from the aqueous solution. The sample is subjected to an antibiotic adsorption experiment, and has excellent adsorption capacity for antibiotic solutions with different concentrations, so that the sample can effectively adsorb antibiotic pollutants in an aqueous solution.
Antibiotic adsorption experiments were as follows:
respectively preparing ofloxacin (OFO), Norfloxacin (NFO) and Tetracycline (TC) solutions with the concentrations of 5mg/L,10mg/L,15mg/L,20mg/L,25mg/L,30mg/L,35mg/L and 40mg/L, and adding LAC-SA to perform adsorption at 25 ℃, wherein the concentration of the LAC-SA is 20 g/L. After 5h, the obtained data are fitted by a Langmuir formula to obtain the following adsorption results: OFO (89.9281mg g) -1 )>TC(31.2695mg·g -1 )>NFO(24.2013mg·g -1 ). The LAC-SA pellet can be recycled for 10 times, and has total adsorption amount of OFO over 700mg g -1 。
The regeneration method of the loofah sponge based active carbon hydrogel material comprises the following steps: mixing the loofah sponge based active carbon hydrogel material adsorbed with the antibiotics and ethanol according to a solid-to-liquid ratio of 1 g: 15mL of the mixture was mixed, stirred at 200rpm for 24 hours, filtered, and washed with deionized water.
The embodiments described above are described to facilitate an understanding and use of the invention by those skilled 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 should make improvements and modifications within the scope of the present invention based on the disclosure of the present invention.
Claims (2)
1. The application of the loofah sponge based activated carbon hydrogel material in adsorbing antibiotics containing ofloxacin, norfloxacin and tetracycline in water is characterized in that the diameter of the loofah sponge based activated carbon hydrogel material is 2-
10mm, and the preparation method of the loofah sponge based activated carbon hydrogel material comprises the following steps:
(1) carbonizing retinervus Luffae fructus at high temperature to obtain retinervus Luffae fructus-based activated carbon LAC;
(2) grinding loofah sponge-based activated carbon LAC into powder to obtain LAC powder;
(3) adding polyvinyl alcohol (PVA) powder into distilled water, stirring at the stirring speed of 2500-3500 rpm, heating to 80-100 ℃, preserving heat at 80-100 ℃ for 1-3 hours, and cooling to obtain a PVA solution with the concentration of 1-10 g/L;
(4) adding LAC powder into a PVA solution, and performing ultrasonic dispersion to obtain a mixed solution A, wherein the concentration of LAC in the mixed solution A is 1-10 g/L;
(5) adding sodium alginate into the mixed solution A in batches under the condition that the stirring speed is 2000-3000rpm, and stirring for 1-6 h at 2000-3000rpm to obtain a mixed solution B, wherein the concentration of the sodium alginate in the mixed solution B is 8-21 g/L;
(6) dropping the mixed solution B into 1-15wt% of CaCl at a dropping speed of 10-20mL/min 2 And obtaining the loofah sponge based active carbon hydrogel material in the water solution.
2. The use according to claim 1, wherein in the preparation method of the loofah sponge-based activated carbon gel material, the conditions of high-temperature carbonization are as follows: taking argon as protective gas, heating to 700-1000 ℃ at the speed of 2-5 ℃/min, and preserving heat for 6-8 hours at the temperature of 700-1000 ℃.
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| CN110681364A (en) | 2020-01-14 |
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