CN112400869A - Cl-modified GQD/ZnO/acidified attapulgite nano composite antibacterial agent and preparation method thereof - Google Patents
Cl-modified GQD/ZnO/acidified attapulgite nano composite antibacterial agent and preparation method thereof Download PDFInfo
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
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- A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
- A01N25/08—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests containing solids as carriers or diluents
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N59/00—Biocides, pest repellants or attractants, or plant growth regulators containing elements or inorganic compounds
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
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- A01N59/16—Heavy metals; Compounds thereof
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
Abstract
The invention discloses a Cl-modified GQD/ZnO/acidified attapulgite nano composite antibacterial agent and a preparation method thereof, wherein ATP is used as a carrier, HCl is used as a modifier, Cl-modified GQD and a novel photoelectric functional material ZnO quantum dot are used as main antibacterial components, the GQD is modified to increase the defect sites thereof, and is compounded with ZnO, so that the photoproduction-electron recombination on the surface of ZnO is effectively inhibited, and the generation of active oxygen is promoted; and finally, loading the Cl-modified GQD/ZnO quantum dots on the surface of the acidified attapulgite, adsorbing bacteria on the surface of the acidified attapulgite by utilizing the huge specific surface area and high absorptivity of ATP, and then cooperatively loading the Cl-modified GQD/ZnO quantum dots (GQD-Cl/ZnO) on the surface of the acidified attapulgite and among the pore channels to play a high-efficiency antibacterial role. The technical scheme has the advantages of safety, no pollution, high antibacterial efficiency and the like, and the antibacterial rate of the nano composite antibacterial agent prepared by the method at 3mg/ml to escherichia coli can reach 96.88%.
Description
Technical Field
The invention relates to a safe, environment-friendly and efficient antibacterial agent, and in particular relates to a Cl-modified GQD/ZnO/acidified attapulgite nano composite antibacterial agent and a preparation method thereof.
Background
In recent years, the rapid propagation of various pathogenic bacteria causes the deterioration of substances and the infection and illness of human bodies, which seriously affect normal lives and health safety, so that people begin to use a large amount of antibiotics, thereby generating a 'super bacteria' problem and seriously harming human health. Therefore, the research and development of novel efficient antibacterial materials which are green, environment-friendly and eco-friendly are urgent.
The nano ZnO has the characteristics of safety, no toxicity, high thermal stability, high chemical stability and the like, and is widely researched. Relevant studies have shown that: the antibacterial effect of nano ZnO is improved along with the reduction of the size. However, as a photocatalytic antibacterial agent, ZnO itself has disadvantages such as a large forbidden band width and easy recombination of photogenerated electron-hole pairs, and the application range thereof is severely restricted. The novel carbon quantum dot material is favored because of the advantages of low biological toxicity, good water solubility, good conductivity and the like. Relevant studies have shown that: carbon nanomaterials with defect or heteroatom sites can generate reactive oxygen species by surface reactions under illumination, the reactivity of which is generally dependent on the defect or heteroatom sites. As a novel quantum dot material, the graphene quantum dot has oxygen-containing functional groups on the surface, and the surface functional groups can be modified by reaction to obtain different performances. Chlorine atom doping is an effective method for modifying defect energy levels and adjusting physical and chemical properties, which results in a corresponding change in electron density and charge transfer capability of GQDs, and chlorine atoms have a larger atomic radius and a higher electronegativity than carbon atoms. The prepared Cl-GQD has better fluorescence and photocatalysis characteristics and biocompatibility. Therefore, the Cl-GQD and the ZnO are compounded to realize effective interface charge transfer and inhibit the recombination of electron hole pairs, thereby accelerating the generation of active oxygen and improving the antibacterial performance of the composite material. However, the small-sized quantum dots have large specific surface areas and are easy to agglomerate, and the antibacterial performance of the quantum dots is seriously influenced.
Attapulgite (ATP) is a natural porous material carrier, has a unique layer chain crystal structure, and the crystals of the ATP have a fine rod-like and fibrous shape, but the adsorption capacity of the natural attapulgite on antibacterial materials is low, so that the natural attapulgite needs to be subjected to activation modification to improve the adsorption performance. The acid activation treatment with proper concentration can play a role in dredging the inner pore canals of the attapulgite, removing impurities such as carbonate and the like in the attapulgite and increasing the specific surface area and the pore volume. In addition, the acidified attapulgite is more negatively charged than native attapulgite. Therefore, the acidified attapulgite becomes an ideal carrier of the antibacterial material.
The present invention is based on the above research background.
Disclosure of Invention
The invention aims to provide a Cl-modified GQD/ZnO/acidified attapulgite nano composite antibacterial agent and a preparation method thereof.
In order to achieve the above object, the present invention adopts the following technical solutions.
A preparation method of a Cl-modified GQD/ZnO/acidified attapulgite nano composite antibacterial agent comprises the following steps:
the method comprises the following steps: weighing 4-8g of attapulgite, placing into a hydrochloric acid solution, heating in water bath, washing the product with distilled water for 3 times, standing each time to remove supernatant, washing the attapulgite solution with water to neutrality, centrifuging, and drying the solid precipitate to obtain acidified attapulgite.
Step two: heating 2-5g of citric acid CA at 200 ℃ to become dark orange, adding NaOH aqueous solution to adjust the PH to be neutral to obtain GQDs aqueous solution, taking 110-140mg of GQDs in 50ml of HCl, and heating in water bath at 60-80 ℃ for 2h to obtain the chlorine modified graphene quantum dots.
Step three: respectively weighing zinc acetate dihydrate and chlorine modified graphene quantum dots (the mass ratio is 1 (0.01-0.06)) to be dispersed in absolute ethyl alcohol, uniformly stirring, adding acidified attapulgite prepared in the early stage (the mass ratio of the acidified attapulgite to the zinc acetate dihydrate is ((0.4-0.6): 1), heating in a water bath at 60-80 ℃ for 1.5-3 h, dropwise adding ethanol solution of potassium hydroxide (the molar ratio of the zinc acetate dihydrate to the potassium hydroxide is 1: 1.4), uniformly stirring and mixing, heating in an oil bath at 80-100 ℃ for 2-5h, finishing reaction, adding deionized water after the reaction is finished, standing, cleaning and centrifuging to obtain the Cl modified GZnO/acidified attapulgite nano composite antibacterial agent.
Further, the concentration of the hydrochloric acid in the step one is 5-8 mol/L.
Further, the temperature of the water bath in the step one is 50-70 ℃, and the reaction time is 10-25 h.
Further, the temperature of the water bath in the second step is 60-80 ℃, and the reaction time is 2 h.
Furthermore, the temperature of the oil bath in the third step is 80-100 ℃, and the reaction time is 2-5 h.
The invention has the following beneficial effects:
according to the Cl-modified GQD/ZnO/acidified attapulgite nano composite antibacterial agent prepared by the invention, ATP is used as a carrier, HCl is used as a modifier, Cl-modified GQD and a novel photoelectric functional material ZnO quantum dot are used as main antibacterial components, the GQD is modified to increase the defect sites, and the GQD is compounded with ZnO, so that the photoproduction-electron recombination on the surface of ZnO is effectively inhibited, and the generation of active oxygen is promoted; and finally, loading the Cl-modified GQD/ZnO quantum dots on the surface of the acidified attapulgite, adsorbing bacteria on the surface of the acidified attapulgite by utilizing the huge specific surface area and high absorptivity of ATP, and then utilizing Cl-modified GQD/ZnO quantum dots (GQD-Cl/ZnO) cooperatively loaded on the surface of the acidified attapulgite and among pore channels to play a high-efficiency antibacterial role to prepare the novel safe, environment-friendly and high-antibacterial-activity nano composite antibacterial agent.
GQD modified by Cl and a novel photoelectric functional material ZnO quantum dot (GQD-Cl/ZnO) with high antibacterial activity are embedded into ATP pore canals and surfaces, so that the defect that the quantum dots are easy to agglomerate is effectively overcome, and Si in attapulgite lattices4+ Ions are very easily isomorphously displaced with other low valent cations to adsorb and kill bacteria. The preparation method comprisesSafe, environment-friendly, high-efficiency and the like.
Drawings
FIG. 1 is a TEM photograph of the Cl-modified GQD/ZnO/acidified attapulgite nano composite antibacterial agent prepared in example 1 of the present invention;
FIG. 2 is a diagram showing the antibacterial effect of the Cl-modified GQD/ZnO/acidified attapulgite nano composite antibacterial agent prepared in example 1 of the present invention.
Detailed Description
The present invention will be described in further detail with reference to the following examples, which are not intended to limit the invention thereto.
Example 1
Weighing 4g of attapulgite, putting into 5mol/L hydrochloric acid solution, heating in 70 ℃ water bath for 10h, washing the product with distilled water for 3 times, and standing each time to remove supernatant so as to wash the attapulgite solution to neutrality. And finally, centrifuging, and drying the solid precipitate to obtain the acidified attapulgite.
After 3g of Citric Acid (CA) was heated at 200 ℃ for 30min to turn dark orange, an aqueous NaOH solution was added to adjust the pH to neutral, to obtain an aqueous GQDs solution. And (3) heating 130mg of GQD in 50ml of HCl in a water bath at 65 ℃ for 2h to obtain the chlorine modified graphene quantum dot.
Respectively weighing 1g of zinc acetate dihydrate and 0.05g of chlorine-modified graphene quantum dots, dispersing in 100 mL of absolute ethanol, uniformly stirring, adding 400 mg of AP, pouring into a three-neck flask, and heating in a water bath at 60 ℃ for reacting for 1.5h to obtain a mixed precursor solution of zinc, GQD-Cl and acidified attapulgite; adding 6.4 mmol of potassium hydroxide into 50mL of ethanol solution, magnetically stirring for 30min, dropwise adding the obtained alkali solution into the mixed precursor solution of zinc, GQD-Cl and attapulgite prepared at the earlier stage, magnetically stirring for 30min, heating in an oil bath at 80 ℃ for reaction for 5h, adding 100 mL of deionized water after the reaction is finished, magnetically stirring for 10 min at room temperature, standing, cleaning and centrifuging to obtain the Cl-modified GQD/ZnO/acidified attapulgite nano composite antibacterial agent.
As shown in figure 1, the Cl modified GQD and ZnO are distributed on the rod body of the attapulgite, which shows that the Cl modified GQD/ZnO/acidified attapulgite nano composite antibacterial agent is successfully prepared.
The Cl-modified GQD/ZnO/acidified attapulgite nano composite antibacterial agent (with the concentration of 3 mg/ml) prepared by the technical scheme has the bacteriostasis rate of 96.88% on escherichia coli. FIG. 2 a) and FIG. 2 b) are diagrams illustrating the antibacterial effect of the Cl-modified GQD/ZnO/acidified attapulgite nano composite antibacterial agent on Escherichia coli.
Example 2:
weighing 7g of attapulgite, putting the attapulgite into 8mol/L hydrochloric acid solution, heating in water bath at 50 ℃ for 25h, washing the product with distilled water for 3 times, and standing each time to remove supernatant so as to wash the attapulgite solution to neutrality. Finally, the mixture is centrifuged to obtain a mixture,
and drying the solid precipitate to obtain the acidified attapulgite.
2g of Citric Acid (CA) is heated at 200 ℃ for 30min to become dark orange, and then NaOH aqueous solution is added to adjust the pH to be neutral, so as to obtain GQDs aqueous solution. And (3) heating 120mg of GQD in 50ml of HCl in a water bath at 60 ℃ for 2h to obtain the chlorine modified graphene quantum dot.
Respectively weighing 1g of zinc acetate dihydrate and 0.01g of chlorine-modified graphene quantum dots, dispersing in 100 mL of absolute ethanol, uniformly stirring, adding 600 mg of AP, pouring into a three-neck flask, and heating in a water bath at 80 ℃ for reaction for 3h to obtain a mixed precursor solution of zinc, GQD-Cl and acidified attapulgite; adding 6.4 mmol of potassium hydroxide into 50mL of ethanol solution, magnetically stirring for 30min, dropwise adding the obtained alkali solution into the mixed precursor solution of zinc, GQD-Cl and attapulgite prepared at the earlier stage, magnetically stirring for 30min, heating in an oil bath at 90 ℃ for reaction for 3h, adding 100 mL of deionized water after the reaction is finished, magnetically stirring for 10 min at room temperature, standing, cleaning and centrifuging to obtain the Cl-modified GQD/ZnO/acidified attapulgite nano composite antibacterial agent.
Example 3:
weighing 6g of attapulgite, putting into 7mol/L hydrochloric acid solution, heating in water bath at 60 ℃ for 20h, washing the product with distilled water for 3 times, and standing each time to remove supernatant so as to wash the attapulgite solution to neutrality. And finally, centrifuging, and drying the solid precipitate to obtain the acidified attapulgite.
After 5g of Citric Acid (CA) was heated at 200 ℃ for 30min to turn dark orange, an aqueous NaOH solution was added to adjust the pH to neutral, to obtain an aqueous GQDs solution. And (3) heating 140mg of GQD in 50ml of HCl in water bath at 80 ℃ for 2h to obtain the chlorine modified graphene quantum dot.
Respectively weighing 1g of zinc acetate dihydrate and 0.04g of chlorine-modified graphene quantum dots, dispersing in 100 mL of absolute ethanol, uniformly stirring, adding 500 mg of AP, pouring into a three-neck flask, and heating in a water bath at 70 ℃ for 2.5 hours to react to obtain a mixed precursor solution of zinc, GQD-Cl and acidified attapulgite; adding 6.4 mmol of potassium hydroxide into 50mL of ethanol solution, magnetically stirring for 30min, dropwise adding the obtained alkali solution into the mixed precursor solution of zinc, GQD-Cl and attapulgite prepared at the earlier stage, magnetically stirring for 30min, heating in an oil bath at 100 ℃ for reaction for 4h, adding 100 mL of deionized water after the reaction is finished, magnetically stirring for 10 min at room temperature, standing, cleaning and centrifuging to obtain the Cl-modified GQD/ZnO/acidified attapulgite nano composite antibacterial agent.
Example 4:
weighing 8g of attapulgite, putting into 6mol/L hydrochloric acid solution, heating in water bath at 65 ℃ for 15h, washing the product with distilled water for 3 times, and standing each time to remove supernatant so as to wash the attapulgite solution to neutrality. And finally, centrifuging, and drying the solid precipitate to obtain the acidified attapulgite.
After 4g of Citric Acid (CA) is heated at 200 ℃ for 30min to become dark orange, NaOH aqueous solution is added to adjust the pH to be neutral, and GQDs aqueous solution is obtained. And (3) heating 110mg of GQD in 50ml of HCl in a water bath at 70 ℃ for 2h to obtain the chlorine modified graphene quantum dot.
Respectively weighing 1g of zinc acetate dihydrate and 0.06g of chlorine-modified graphene quantum dots, dispersing in 100 mL of absolute ethanol, uniformly stirring, adding 400 mg of AP, pouring into a three-neck flask, and heating in a water bath at 75 ℃ for 2h to react to obtain a mixed precursor solution of zinc, GQD-Cl and acidified attapulgite; adding 6.4 mmol of potassium hydroxide into 50mL of ethanol solution, magnetically stirring for 30min, dropwise adding the obtained alkali solution into the mixed precursor solution of zinc, GQD-Cl and attapulgite prepared at the earlier stage, magnetically stirring for 30min, heating in an oil bath at 85 ℃ for reaction for 2h, adding 100 mL of deionized water after the reaction is finished, magnetically stirring for 10 min at room temperature, standing, cleaning and centrifuging to obtain the Cl-modified GQD/ZnO/acidified attapulgite nano composite antibacterial agent.
Finally, it is to be noted that: the above embodiments are only for illustrating the technical solutions of the present invention and not for limiting the same, and although the present invention is described in detail with reference to the above embodiments, those of ordinary skill in the art should understand that: modifications and equivalents may be made to the embodiments of the invention without departing from the spirit and scope of the invention, which is to be covered by the claims.
Claims (6)
1. A preparation method of a Cl-modified GQD/ZnO/acidified attapulgite nano composite antibacterial agent is characterized by comprising the following steps:
the method comprises the following steps: weighing 4-8g of attapulgite, placing into a hydrochloric acid solution, heating in water bath, washing the product with distilled water for 3 times, standing each time to remove supernatant, and washing the attapulgite solution to neutrality;
finally centrifuging, and drying the solid precipitate to obtain acidified attapulgite;
step two: heating 2-5g of citric acid CA at 200 ℃ to become dark orange, adding NaOH aqueous solution to adjust the PH to be neutral to obtain graphene quantum dot GQDs aqueous solution, taking 110-140mg of GQDs in 50ml of HCl, and heating in a water bath at 60-80 ℃ for 2h to obtain chlorine modified graphene quantum dots;
step three: respectively weighing the components in a mass ratio of 1: 0.01-0.06 of zinc acetate dihydrate and chlorine modified graphene quantum dots are dispersed in absolute ethyl alcohol, uniformly stirred, added with the acidified attapulgite prepared in the early stage, the mass ratio of the acidified attapulgite to the zinc acetate dihydrate is 0.4-0.6: 1, heated and reacted in a water bath at 60-80 ℃ for 1.5-3 h, then dropwise added with an ethanol solution of potassium hydroxide, the molar ratio of the zinc acetate dihydrate to the potassium hydroxide is 1:1.4, uniformly stirred and mixed, and heated and reacted in an oil bath at 80-100 ℃ for 2-5 h; and adding deionized water after the reaction is finished, standing, cleaning and centrifuging to obtain the Cl-modified GQD/ZnO/acidified attapulgite nano composite antibacterial agent.
2. The method for preparing the Cl-modified GQD/ZnO/acidified attapulgite nano composite antibacterial agent according to claim 1, wherein the method comprises the following steps: the concentration of the hydrochloric acid in the first step is 5-8 mol/L.
3. The method for preparing the Cl-modified GQD/ZnO/acidified attapulgite nano composite antibacterial agent according to claim 2, wherein the method comprises the following steps: in the first step, the water bath temperature is 50-70 ℃, and the reaction time is 10-25 h.
4. The method for preparing the Cl-modified GQD/ZnO/acidified attapulgite nano composite antibacterial agent according to claim 3, wherein the method comprises the following steps: in the second step, the temperature of the water bath is 60-80 ℃, and the reaction time is 2 h.
5. The method for preparing the Cl-modified GQD/ZnO/acidified attapulgite nano composite antibacterial agent according to claim 4, wherein the method comprises the following steps: in the third step, the oil bath temperature is 80-100 ℃, and the reaction time is 2-5 h.
6. The GQD/ZnO/acidified attapulgite nano composite antibacterial agent modified by Cl and prepared by the preparation method of claims 1-5.
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| CN113841708A (en) * | 2021-11-08 | 2021-12-28 | 陕西科技大学 | Silver sulfide/molybdenum disulfide/acidified attapulgite nano composite light-driven antibacterial material and preparation method and application thereof |
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| CN113841708A (en) * | 2021-11-08 | 2021-12-28 | 陕西科技大学 | Silver sulfide/molybdenum disulfide/acidified attapulgite nano composite light-driven antibacterial material and preparation method and application thereof |
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