CN112827480A - Preparation method and application of antibiotic rapid adsorbent - Google Patents
Preparation method and application of antibiotic rapid adsorbent Download PDFInfo
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- CN112827480A CN112827480A CN202110025476.0A CN202110025476A CN112827480A CN 112827480 A CN112827480 A CN 112827480A CN 202110025476 A CN202110025476 A CN 202110025476A CN 112827480 A CN112827480 A CN 112827480A
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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
- B01J20/3078—Thermal treatment, e.g. calcining or pyrolizing
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- 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
- B01J20/205—Carbon nanostructures, e.g. nanotubes, nanohorns, nanocones, nanoballs
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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
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
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- B01J20/28009—Magnetic properties
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/283—Treatment of water, waste water, or sewage by sorption using coal, charred products, or inorganic mixtures containing them
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/34—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32
- C02F2103/343—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32 from the pharmaceutical industry, e.g. containing antibiotics
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Abstract
The preparation method of the antibiotic fast adsorbent comprises the following steps: preparing 9-11% PAN spinning solution by adopting a stirring method; adding nickel chloride into 9-11% of PAN spinning solution to prepare 8-10% of Ni spinning solution; carrying out electrostatic spinning on 8-10% of Ni spinning solution under the conditions that the spinning voltage is 12-14kV, the distance between an electrostatic spinning head and a collecting roller is 5-9cm, the rotating speed of the collecting roller is 370-390rpm, and the advancing speed of the electrostatic spinning head is 0.5-0.7mL/h to prepare spinning sheets containing 8-10% of Ni; heating the prepared spinning piece with the Ni content of 8-10% to 270-290 ℃ at the heating rate of 0.5-1.5 ℃/min, and preserving the heat for 1.5-2.5 hours to obtain an intermediate; the prepared intermediate is heated to 690-710 ℃ at the heating rate of 4-6 ℃/min, and the calcination time is 1.5-2.5 hours. The antibiotic fast adsorbent can be used for rapidly removing antibiotics such as sulfadiazine, carbamazepine, coumarin, sulfamethoxazole, acetaminophen and p-hydroxybenzoic acid within 25min, and can be rapidly separated by a magnetic field.
Description
Technical Field
The disclosure relates to a preparation method and application of an antibiotic rapid adsorbent.
Background
The antibiotic medicine used in daily life of people, the antibiotic used in large amount in breeding industry for improving economic benefit and the production wastewater generated by various large pharmaceutical factories are continuously discharged into natural water, the drug resistance of bacteria is increased, the ecological structure is destroyed, and the human health is greatly threatened by the biological enrichment effect.
At present, the accepted antibiotic effective removal technology is an adsorption method and an advanced oxidation method. Although the advanced oxidation method has higher treatment efficiency, harmful intermediate products can be generated in the reaction process to form secondary pollution. On the contrary, the adsorption method does not need to input an additional oxidant, and does not have the possibility of generating an intermediate toxic product, so the adsorption method has been developed into a high-efficiency and environment-friendly method for removing antibiotics.
Although carbon nanofibers have a certain antibiotic adsorption capacity, water treatment pressure is increasing with the development of the current society and the increasing shortage of water resources. Meanwhile, along with the improvement of environmental protection and health consciousness of people, the content of antibiotic pollutants in water is concerned, and the antibiotic removal efficiency and the antibiotic removal standard of the national society are continuously improved. Thus, conventional carbon nanofibers have not been satisfactory. The preparation of the high-efficiency carbon nanofiber adsorbent becomes a research hotspot of current researchers.
Disclosure of Invention
The disclosure provides a preparation method of an antibiotic rapid adsorbent, which solves the technical problem that carbon nanofiber cannot meet the use requirement in the prior art.
Some embodiments adopted to solve the above technical problems include:
a preparation method of an antibiotic fast adsorbent comprises the following steps:
preparing 9-11% PAN spinning solution by adopting a stirring method;
adding nickel chloride into 9-11% of PAN spinning solution to prepare 8-10% of Ni spinning solution;
carrying out electrostatic spinning on 8-10% of Ni spinning solution under the conditions that the spinning voltage is 12-14kV, the distance between an electrostatic spinning head and a collecting roller is 5-9cm, the rotating speed of the collecting roller is 370-390rpm, and the advancing speed of the electrostatic spinning head is 0.5-0.7mL/h to prepare spinning sheets containing 8-10% of Ni;
heating the prepared spinning piece with the Ni content of 8-10% to 270-290 ℃ at the heating rate of 0.5-1.5 ℃/min, and preserving the heat for 1.5-2.5 hours to obtain an intermediate;
the prepared intermediate is heated to 690-710 ℃ at the heating rate of 4-6 ℃/min, and the calcination time is 1.5-2.5 hours.
Preferably, the spinning solution of 9-11% PAN prepared by the stirring method is stirred by a mechanical stirring mode.
Preferably, the prepared spinning piece containing 8-10% of Ni is heated to 270-290 ℃ at the heating rate of 0.5-1.5 ℃/min, and is subjected to heat preservation for 1.5-2.5 hours to obtain an intermediate, and the intermediate is prepared by adopting a muffle furnace.
Preferably, the prepared intermediate is heated to 690-710 ℃ at a heating rate of 4-6 ℃/min, and the intermediate with the calcination time of 1.5-2.5 hours is heated and calcined in a tubular furnace under the protection of nitrogen.
Preferably, 2.6-2.8g PAN is dissolved in 25g DMF and mechanically stirred to complete dissolution to obtain 9% -11% PAN dope.
Preferably, 2.74g of nickel chloride is added to 9% -11% PAN dope and stirred to complete dissolution to obtain 8% -10% Ni dope.
Preferably, the collecting roller comprises a roller body, and the roller body is wrapped with tin foil paper.
Preferably, the collecting roller further comprises a frame, the cylinder is rotatably connected to the frame, the collecting roller further comprises a driving machine for driving the cylinder to rotate, and the driving machine drives the cylinder to rotate through a synchronous belt.
Preferably, the electrospinning head is a syringe needle having an inner diameter of 1.1mm to 1.3 mm.
An application of an antibiotic fast adsorbent, an application of the antibiotic fast adsorbent in water treatment.
Compared with the prior art, the preparation method of the antibiotic rapid adsorbent provided by the disclosure has the following advantages:
the preparation method of the antibiotic fast adsorbent comprises the following steps: preparing 9-11% PAN spinning solution by adopting a stirring method; adding nickel chloride into 9-11% of PAN spinning solution to prepare 8-10% of Ni spinning solution; carrying out electrostatic spinning on 8-10% of Ni spinning solution under the conditions that the spinning voltage is 12-14kV, the distance between an electrostatic spinning head and a collecting roller is 5-9cm, the rotating speed of the collecting roller is 370-390rpm, and the advancing speed of the electrostatic spinning head is 0.5-0.7mL/h to prepare spinning sheets containing 8-10% of Ni; heating the prepared spinning piece with the Ni content of 8-10% to 270-290 ℃ at the heating rate of 0.5-1.5 ℃/min, and preserving the heat for 1.5-2.5 hours to obtain an intermediate; the prepared intermediate is heated to 690-710 ℃ at the heating rate of 4-6 ℃/min, and the calcination time is 1.5-2.5 hours. The antibiotic fast adsorbent prepared by the process can quickly remove the antibiotics such as sulfadiazine, carbamazepine, coumarin, sulfamethoxazole, acetaminophen, p-hydroxybenzoic acid and the like within 25min, and the adsorbent can be quickly separated by a magnetic field.
Drawings
For purposes of explanation, several embodiments of the disclosed technology are set forth in the following figures. The following drawings are incorporated herein and constitute a part of the detailed description. In some instances, well-known structures and components are shown in block diagram form in order to avoid obscuring the concepts of the disclosed subject technology.
FIG. 1 is a transmission electron micrograph of the antibiotic fast adsorbent.
FIG. 2 is a graph comparing the effect of different Ni contents on sulfadiazine treatment of antibiotic fast adsorbents.
FIG. 3 is a graph comparing the removal of different contaminants by fast antibiotics adsorbents.
FIG. 4 is a diagram showing the effect of the antibiotic fast adsorbent before and after magnetic separation.
FIG. 5 is a schematic view of a first orientation of the collection roller.
FIG. 6 is a schematic view of the collection roller in a second orientation.
Detailed Description
The specific embodiments illustrated below are intended as descriptions of various configurations of the presently disclosed subject technology and are not intended to represent the only configurations in which the presently disclosed subject technology may be practiced. Specific embodiments include specific details for the purpose of providing a thorough understanding of the presently disclosed subject matter technology. It will be apparent, however, to one skilled in the art that the disclosed subject matter technology is not limited to the specific details shown herein and may be practiced without these specific details.
Referring to fig. 1 to 4, a method for preparing an antibiotic fast adsorbent includes the following steps:
preparing 9-11% PAN spinning solution by adopting a stirring method;
adding nickel chloride into 9-11% of PAN spinning solution to prepare 8-10% of Ni spinning solution;
carrying out electrostatic spinning on 8-10% of Ni spinning solution under the conditions that the spinning voltage is 12-14kV, the distance between an electrostatic spinning head and a collecting roller is 5-9cm, the rotating speed of the collecting roller is 370-390rpm, and the advancing speed of the electrostatic spinning head is 0.5-0.7mL/h to prepare spinning sheets containing 8-10% of Ni;
heating the prepared spinning piece with the Ni content of 8-10% to 270-290 ℃ at the heating rate of 0.5-1.5 ℃/min, and preserving the heat for 1.5-2.5 hours to obtain an intermediate;
the prepared intermediate is heated to 690-710 ℃ at the heating rate of 4-6 ℃/min, and the calcination time is 1.5-2.5 hours.
The 9-11% PAN spinning solution prepared by the stirring method is stirred by a mechanical stirring mode.
The prepared spinning piece with the Ni content of 8-10% is heated to the temperature of 270-290 ℃ at the heating rate of 0.5-1.5 ℃/min, and is kept warm for 1.5-2.5 hours to obtain an intermediate, and the intermediate is prepared by adopting a muffle furnace.
The prepared intermediate is heated to 690-710 ℃ at the heating rate of 4-6 ℃/min, and the intermediate with the calcination time of 1.5-2.5 hours is heated and calcined in a tubular furnace under the protection of nitrogen.
Dissolving 2.6-2.8g of PAN into 25g of DMF, and mechanically stirring until the PAN spinning solution is completely dissolved to obtain 9-11% PAN spinning solution.
Adding 2.74g of nickel chloride into the spinning solution of 9% -11% of PAN, and stirring until the nickel chloride is completely dissolved to obtain 8% -10% of Ni spinning solution.
Referring to fig. 5-6, in some embodiments, the collecting drum 1 comprises a cylinder 2, and the cylinder 2 is wrapped with a foil.
The collecting roller 1 further comprises a rack 3, the barrel 2 is rotationally connected to the rack 3, the collecting roller 1 further comprises a driving machine 4 for driving the barrel 2 to rotate, and the driving machine 4 drives the barrel 2 to rotate through a synchronous belt 5.
The electrostatic spinning head is an injector needle with the inner diameter of 1.1mm-1.3 mm.
An application of an antibiotic fast adsorbent, an application of the antibiotic fast adsorbent in water treatment.
Practical application example:
s10, dissolving 2.7g of PAN into 25g of DMF, and mechanically stirring until the PAN is completely dissolved to obtain 10% PAN spinning solution;
s20, adding 2.74g of nickel chloride into the spinning solution obtained in the S10, and stirring until the nickel chloride is completely dissolved to obtain 9% Ni spinning solution;
s30, carrying out electrostatic spinning on the 9% Ni spinning solution under the conditions that the spinning voltage is 12kV, the distance between an electrostatic spinning head and a collecting roller is 9cm, the rotating speed of the collecting roller is 380rpm, and the advancing speed of the electrostatic spinning head is 0.6mL/h, wherein the spinning time is 6 hours, and thus obtaining 9% Ni spinning pieces;
s40, pressing the spinning sheet in a muffle furnace by using a high-temperature-resistant glass plate, heating to 280 ℃ at a heating rate of 1 ℃/min, and keeping the temperature for 2 hours;
s50, placing the material obtained after the pre-oxidation in a tube furnace, heating to 700 ℃ at a heating rate of 5 ℃/min under the protection of nitrogen, and calcining for 2.5 hours.
Referring to fig. 1-3, fig. 2 is a graph comparing the effect of sulfadiazine treatment with different Ni contents of the antibiotic fast adsorbent: 10mg of materials with different nickel contents react with 50mL of sulfadiazine with the concentration of 2.5mg/L for 25 minutes, wherein pure carbon fibers without nickel have no adsorption effect, the material containing 3 percent of Ni can adsorb 69 percent, the material containing 6 percent of Ni can adsorb 79 percent, and the material containing 8 to 10 percent of Ni can adsorb 99 percent. The adsorption effect is better with the increase of the elementary nickel.
FIG. 3 is a graph comparing the effect of 10mg of 9% Ni-containing material on the adsorption removal of 50mL, 2.5mg/L of different contaminants; 99% of sulfadiazine can be adsorbed, 89% of carbamazepine can be adsorbed and degraded, 97% of coumarin can be adsorbed and removed, 97% of sulfamethoxazole can be adsorbed and removed, 88% of acetaminophen can be adsorbed and 91% of p-hydroxybenzoic acid can be adsorbed and removed.
FIG. 4 is a diagram showing the effect of the antibiotic fast adsorbent before and after magnetic separation, and it can be seen from FIG. 4 that the antibiotic fast adsorbent can be rapidly and completely separated from the solution, which shows that the material has good recoverability. In fig. 4, the left bottle is the effect before separation, the middle bottle is the effect after separation, and the rightmost bottle is made of magnetic material.
While the subject matter of the present disclosure and its corresponding details have been described above, it is to be understood that the above description is only illustrative of some embodiments of the subject matter of the present disclosure and that some of the details may be omitted from the detailed description.
In addition, in some of the embodiments disclosed above, there is a possibility that a plurality of embodiments may be combined and implemented, and various combinations are not listed at length. The implementation embodiments can be freely combined according to the requirements when the technical personnel in the field carry out the implementation so as to obtain better application experience.
Other configurations of details or figures may be derived by those skilled in the art in practicing the presently disclosed subject matter, as well as figures, and it will be apparent that such details are within the scope of the presently disclosed subject matter and are covered by the presently disclosed subject matter without departing from the presently disclosed subject matter.
Claims (10)
1. The preparation method of the antibiotic rapid adsorbent is characterized by comprising the following steps:
preparing 9-11% PAN spinning solution by adopting a stirring method;
adding nickel chloride into 9-11% of PAN spinning solution to prepare 8-10% of Ni spinning solution;
carrying out electrostatic spinning on 8-10% of Ni spinning solution under the conditions that the spinning voltage is 12-14kV, the distance between an electrostatic spinning head and a collecting roller is 5-9cm, the rotating speed of the collecting roller is 370-390rpm, and the advancing speed of the electrostatic spinning head is 0.5-0.7mL/h to prepare spinning sheets containing 8-10% of Ni;
heating the prepared spinning piece with the Ni content of 8-10% to 270-290 ℃ at the heating rate of 0.5-1.5 ℃/min, and preserving the heat for 1.5-2.5 hours to obtain an intermediate;
the prepared intermediate is heated to 690-710 ℃ at the heating rate of 4-6 ℃/min, and the calcination time is 1.5-2.5 hours.
2. The method for preparing the antibiotic fast adsorbent according to claim 1, characterized in that: the 9-11% PAN spinning solution prepared by the stirring method is stirred by a mechanical stirring mode.
3. The method for preparing the antibiotic fast adsorbent according to claim 2, characterized in that: the prepared spinning piece with the Ni content of 8-10% is heated to the temperature of 270-290 ℃ at the heating rate of 0.5-1.5 ℃/min, and is kept warm for 1.5-2.5 hours to obtain an intermediate, and the intermediate is prepared by adopting a muffle furnace.
4. The method for preparing the antibiotic fast adsorbent according to claim 3, characterized in that: the prepared intermediate is heated to 690-710 ℃ at the heating rate of 4-6 ℃/min, and the intermediate with the calcination time of 1.5-2.5 hours is heated and calcined in a tubular furnace under the protection of nitrogen.
5. The method for preparing antibiotic fast adsorbent according to claim 1 or 2, characterized in that: dissolving 2.6-2.8g of PAN into 25g of DMF, and mechanically stirring until the PAN spinning solution is completely dissolved to obtain 9-11% PAN spinning solution.
6. The method for preparing the antibiotic fast adsorbent according to claim 1, characterized in that: adding 2.74g of nickel chloride into the spinning solution of 9% -11% of PAN, and stirring until the nickel chloride is completely dissolved to obtain 8% -10% of Ni spinning solution.
7. The method for preparing the antibiotic fast adsorbent according to claim 1, characterized in that: the collecting roller comprises a roller body, and tin foil paper is wrapped on the roller body.
8. The method for preparing the antibiotic fast adsorbent according to claim 1, characterized in that: the collecting roller further comprises a rack, the cylinder body is rotationally connected to the rack, the collecting roller further comprises a driving machine for driving the cylinder body to rotate, and the driving machine drives the cylinder body to rotate through a synchronous belt.
9. The method for preparing the antibiotic fast adsorbent according to claim 1, characterized in that: the electrostatic spinning head is an injector needle with the inner diameter of 1.1mm-1.3 mm.
10. The application of the antibiotic fast adsorbent is characterized in that the antibiotic fast adsorbent is applied to water treatment.
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