CN110521733A - A kind of Co doping ZnO quantum dot/palygorskite nano complex antimicrobials and preparation method thereof - Google Patents
A kind of Co doping ZnO quantum dot/palygorskite nano complex antimicrobials and preparation method thereof Download PDFInfo
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- CN110521733A CN110521733A CN201910878468.3A CN201910878468A CN110521733A CN 110521733 A CN110521733 A CN 110521733A CN 201910878468 A CN201910878468 A CN 201910878468A CN 110521733 A CN110521733 A CN 110521733A
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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
- 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
- A01N59/16—Heavy metals; Compounds thereof
Abstract
The present invention discloses a kind of Co doping ZnO quantum dot/palygorskite nano complex antimicrobials and preparation method thereof, using APT as carrier, four acetate hydrate cobalts are dopant, novel photoelectric functional material ZnO quantum dot is major antibacterial components, using the size limitation of ZnO quantum dot itself and quantum confined effect, in conjunction with itself and Co2+Between coupling, effectively inhibit the compound of the surface ZnO light induced electron and hole；Co doping ZnO quantum dot is loaded into attapulgite surface, utilize the huge specific surface area of APT and high-absorbility, by bacterial adsorption to its surface, then collaboration is supported on cobalt (Co) the doping zinc-oxide quantum dot (ZnO QDs) between attapulgite surface and duct and plays high-efficiency antimicrobial effect, preparation method has many advantages, such as that safety and environmental protection, drug resistance are strong, and the composite nano germicide of preparation is to the bacteriostasis rate of Escherichia coli up to 85.71%.
Description
Technical field
The present invention relates to a kind of high-efficient antibacterial agents, and in particular to a kind of Co doping ZnO quantum dot/palygorskite nano is compound
Antibacterial agent and preparation method thereof.
Background technique
In recent years, not enough, it is unfavorable to prevent, and, which results in global, is expected to industrial negative effect due to people
Three big crises: shortage of resources, environmental pollution, ecological disruption.At the same time, the improper use of antibacterials leads to various cause a disease
The appearance of bacterium, fungi and virus more has the increase of drug-fast bacteria and the generation of super drug-resistant bacteria.The research and development of various antibacterial agents are
Through becoming current research hotspot, wherein inorganic antibacterial material, can be high-efficiency continuous because cheap, security performance is high, nontoxic
It sterilizes and receives more and more attention.
ZnO antibacterial agent is high because having many advantages, such as nontoxic, safe and reliable and thermal stability and chemical stability, rapidly becomes
The research hotspot of antibacterial agent at present.Correlative study shows: nano-ZnO size is smaller, and anti-microbial property is better, but small size
Nano-ZnO itself large specific surface area, easy to reunite, and its greater band gap, biocompatibility are poor, electron-hole is easily compound, no
High-efficiency antimicrobial performance is played conducive to it.
Attapulgite (APT) is a kind of hydration alumina magnesia silicate, has as a kind of natural porous material carrier
Unique layer chain crystal structure, and crystal has big specific surface area and macroion in very tiny rodlike and fibrous
The advantages that exchange capacity, makes it be widely used in terms of improving environment.Due in natural attapulgite tetrahedral si-o film
Silicon can be by a small amount of Al3+And Fe3+It is substituted, and the magnesium in octahedral sheet can also be by a small amount of Fe2+It is replaced, various ions replace
The result in generation makes attapulgite with a small amount of negative electrical charge, and negative electrical charge can attract electron hole pair, promote electron hole pair
Transfer.There is efficient antibacterial action as carrier.
Summary of the invention
Present invention aims at propose a kind of Co doping ZnO quantum dot/palygorskite nano complex antimicrobials and its system
Preparation Method, the present invention have easy to operate, preparation process mild condition, the composite nano germicide good biocompatibility of preparation,
The advantages that safety and environmental protection, excellent antibacterial effect.
To achieve the goals above, the present invention uses following technical scheme.
A kind of Co doping ZnO quantum dot/palygorskite nano complex antimicrobials preparation method, includes the following steps:
Step 1: being that 1:0.007 weighs acetic acid dihydrate zinc respectively and four acetate hydrate cobalts disperse by zinc and cobalt molar ratio
In dehydrated alcohol, be (0.4-0.6) by attapulgite and acetic acid dihydrate zinc mass ratio after mixing evenly: 1 is added concave convex rod
Stone, 70-90 DEG C of heating in water bath for reaction 1-2.5h is to get zinc, cobalt, attapulgite mixing precursor solution；
Step 2: by potassium hydroxide be added ethanol solution in magnetic agitation it is uniform aqueous slkali, by acetic acid dihydrate zinc with
Zn in potassium hydroxide2+:OH-Molar ratio be 1:1.4, by gained aqueous slkali be added drop-wise to step 1 preparation zinc, cobalt, attapulgite
It mixes in precursor solution, after mixing, magnetic agitation is fully dispersed, and 95 DEG C of heating in water bath for reaction 5h terminate；Then gradually
Deionized water is added until solution becomes milky, standing, cleaning are centrifuged and receive to get Co doping ZnO quantum dot/attapulgite
Rice complex antimicrobials.
Further, the magnetic agitation time is 30min in the step 2.
Further, centrifugal treating in the step 2, centrifugation rate 7000rpm/min.
Further, magnetic force stirs solution addition deionized water again at room temperature after solution becomes milky in the step 2
Mix 20min.
The invention has the following advantages:
Co prepared by the present invention adulterates ZnO quantum dot/palygorskite nano complex antimicrobials, using APT as carrier, four hydrations
Cobalt acetate is dopant, and novel photoelectric functional material ZnO quantum dot is major antibacterial components, utilizes the ruler of ZnO quantum dot itself
Very little limitation and quantum confined effect, in conjunction with itself and Co2+Between coupling, effectively inhibit answering for the surface ZnO light induced electron and hole
It closes；Co doping ZnO quantum dot is loaded into attapulgite surface, it, will be thin using the huge specific surface area of APT and high-absorbility
Bacterium is adsorbed to its surface, and then collaboration is supported on cobalt (Co) doping zinc-oxide quantum dot (ZnO between attapulgite surface and duct
QDs high-efficiency antimicrobial effect) is played, bacterium is killed, finally prepares the high novel nano of a kind of good biocompatibility, antibacterial activity
Complex antimicrobials.
Cobalt (Co) doping zinc-oxide quantum dot (ZnO QDs) with high antibacterial activity component is embedded into the duct APT
Between, on the one hand efficiently solve cobalt (Co) doping zinc-oxide quantum dot defect easy to reunite；On the other hand, in APT lattice
Si4+Ion is easy and isomorphous substitution occurs for other cations at a low price, and then adsorbs bacterium, improves its anti-microbial property, preparation side
Method has many advantages, such as that safety and environmental protection, drug resistance are strong, and the Co of preparation adulterates ZnO quantum dot/palygorskite nano complex antimicrobials pair
The bacteriostasis rate of Escherichia coli is up to 85.71%.
Detailed description of the invention
Fig. 1 is that Co prepared by the present invention adulterates ZnO quantum dot/palygorskite nano complex antimicrobials TEM photo；
Fig. 2 (a) is Escherichia coli blank master drawing；
Fig. 2 (b) is that Co prepared by the present invention adulterates ZnO quantum dot/palygorskite nano complex antimicrobials antibacterial effect
Fruit figure；
Specific embodiment
Present invention is further described in detail combined with specific embodiments below, but not as a limitation of the invention.
Embodiment 1:
Weighing the four acetate hydrate cobalts of 4.5mmol acetic acid dihydrate zinc and 0.032mmol respectively, to be scattered in 100mL anhydrous
In ethyl alcohol, after mixing evenly, the APT of 395mg is added, pours into three-necked flask, 70 DEG C of heating in water bath for reaction 1h to get zinc, cobalt,
Attapulgite mixing precursor solution；6.3mmol potassium hydroxide is added in 50mL ethanol solution, it, will after magnetic agitation 20min
Gained aqueous slkali is added drop-wise to zinc prepared by early period, cobalt, in attapulgite mixing precursor solution, and after mixing, magnetic force stirs
30min, 95 DEG C of heating in water bath for reaction 5h are mixed, 100mL deionized water is added after reaction until solution becomes milky, room temperature
Lower magnetic agitation 20min stands, cleaning, is centrifuged to get attapulgite load Co-doped ZnO quantum dot nano composite antibacterial
Agent.
As shown in Figure 1, it can be seen from the figure that Co-doped ZnO quantum dot is evenly distributed on the stick on attapulgite
Body shows that Co doping ZnO quantum dot/palygorskite nano complex antimicrobials are successfully prepared.Fig. 2 (a) and Fig. 2 (b) is the present invention
Prepared Co doping ZnO quantum dot/palygorskite nano complex antimicrobials pass through comparison to the antibacterial effect figure of Escherichia coli
Fig. 2 (a) and Fig. 2 (b) discovery complex antimicrobials are high to Escherichia coli antibacterial activity, excellent effect, nanometer prepared by the present invention
Antibacterial agent is to the bacteriostasis rate of Escherichia coli up to 85.71%.
Embodiment 2:
Weighing the four acetate hydrate cobalts of 4.5mmol acetic acid dihydrate zinc and 0.032mmol respectively, to be scattered in 100mL anhydrous
In ethyl alcohol, after mixing evenly, the APT of 593mg is added, pours into three-necked flask, 90 DEG C of heating in water bath for reaction 2h to get zinc, cobalt,
Attapulgite mixing precursor solution；6.3mmol potassium hydroxide is added in 50mL ethanol solution, it, will after magnetic agitation 20min
Gained aqueous slkali is added drop-wise to zinc prepared by early period, cobalt, in attapulgite mixing precursor solution, and after mixing, magnetic force stirs
30min, 95 DEG C of heating in water bath for reaction 5h are mixed, 100mL deionized water is added after reaction until solution becomes milky, room temperature
Lower magnetic agitation 20min stands, cleaning, is centrifuged and adulterates ZnO quantum dot/palygorskite nano complex antimicrobials to get recessed Co.
Embodiment 3:
Weighing the four acetate hydrate cobalts of 4.5mmol acetic acid dihydrate zinc and 0.032mmol respectively, to be scattered in 100mL anhydrous
In ethyl alcohol, after mixing evenly, the APT of 494mg is added, pours into three-necked flask, 85 DEG C of heating in water bath for reaction 2.5h to get zinc,
Cobalt, attapulgite mixing precursor solution；6.3mmol potassium hydroxide is added in 50mL ethanol solution, magnetic agitation 20min
Afterwards, gained aqueous slkali is added drop-wise to zinc prepared by early period, cobalt, in attapulgite mixing precursor solution, after mixing, magnetic
Power stirs 30min, 95 DEG C of heating in water bath for reaction 5h, and 100mL deionized water is added after reaction until solution and becomes milky,
Magnetic agitation 20min at room temperature stands, cleaning, is centrifuged and adulterates ZnO quantum dot/palygorskite nano composite antibacterial to get Co
Agent.
Embodiment 4:
Weighing the four acetate hydrate cobalts of 4.5mmol acetic acid dihydrate zinc and 0.032mmol respectively, to be scattered in 100mL anhydrous
In ethyl alcohol, after mixing evenly, the APT of 395mg is added, pours into three-necked flask, 80 DEG C of heating in water bath for reaction 1.5h to get zinc,
Cobalt, attapulgite mixing precursor solution；6.3mmol potassium hydroxide is added in 50mL ethanol solution, magnetic agitation 20min
Afterwards, gained aqueous slkali is added drop-wise to zinc prepared by early period, cobalt, in attapulgite mixing precursor solution, after mixing, magnetic
Power stirs 30min, 95 DEG C of heating in water bath for reaction 5h, and 100mL deionized water is added after reaction until solution and becomes milky,
Magnetic agitation 20min at room temperature stands, cleaning, is centrifuged and adulterates ZnO quantum dot/palygorskite nano composite antibacterial to get Co
Agent.
Finally it should be noted that: the above examples are only used to illustrate the technical scheme of the present invention rather than its limitations, to the greatest extent
Pipe is described the invention in detail referring to above-described embodiment, it should be understood by those ordinary skilled in the art that: still may be used
With modifications or equivalent substitutions are made to specific embodiments of the invention, and repaired without departing from any of spirit and scope of the invention
Change or equivalent replacement, should all cover in present claims range.
Claims (5)
1. a kind of Co adulterates ZnO quantum dot/palygorskite nano complex antimicrobials preparation method, it is characterised in that including as follows
Step:
Step 1: being that 1:0.007 weighs acetic acid dihydrate zinc respectively and four acetate hydrate cobalts are scattered in nothing by zinc and cobalt molar ratio
In water-ethanol, be (0.4-0.6) by attapulgite and acetic acid dihydrate zinc mass ratio after mixing evenly: 1 is added attapulgite,
70-90 DEG C of heating in water bath for reaction 1-2.5h is to get zinc, cobalt, attapulgite mixing precursor solution；
Step 2: by potassium hydroxide be added ethanol solution in magnetic agitation it is uniform aqueous slkali, by acetic acid dihydrate zinc and hydrogen-oxygen
Change Zn in potassium2+:OH-Molar ratio be 1:1.4, by gained aqueous slkali be added drop-wise to step 1 preparation zinc, cobalt, attapulgite mix
In precursor solution, after mixing, magnetic agitation is fully dispersed, and 95 DEG C of heating in water bath for reaction 5h terminate；Then it is gradually added into
Deionized water becomes milky until solution, and standing, cleaning, centrifugation are multiple to get Co doping ZnO quantum dot/palygorskite nano
Close antibacterial agent.
2. Co as described in claim 1 adulterates ZnO quantum dot/palygorskite nano complex antimicrobials preparation method, special
Sign is: the magnetic agitation time is 30min in the step 2.
3. Co as described in claim 1 adulterates ZnO quantum dot/palygorskite nano complex antimicrobials preparation method, special
Sign is: centrifugal treating in the step 2, centrifugation rate 7000rpm/min.
4. Co as described in claim 1 adulterates ZnO quantum dot/palygorskite nano complex antimicrobials preparation method, special
Sign is: deionized water magnetic agitation 20min again at room temperature after solution becomes milky is added in solution in the step 2.
5. a kind of Co doping ZnO quantum dot/palygorskite nano such as any one of claim 1-4 the method preparation is compound anti-
Microbial inoculum.
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Cited By (3)
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|---|---|---|---|---|
| CN111838148A (en) * | 2020-07-14 | 2020-10-30 | 陕西科技大学 | Preparation method of cobalt-doped zinc oxide/molybdenum disulfide nano composite antibacterial agent |
| 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 |
| CN114532332A (en) * | 2022-01-26 | 2022-05-27 | 中国科学院兰州化学物理研究所 | Method for constructing zinc oxide/attapulgite nano composite antibacterial material by utilizing ginkgo leaf extract |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111838148A (en) * | 2020-07-14 | 2020-10-30 | 陕西科技大学 | Preparation method of cobalt-doped zinc oxide/molybdenum disulfide nano composite antibacterial agent |
| 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 |
| CN114532332A (en) * | 2022-01-26 | 2022-05-27 | 中国科学院兰州化学物理研究所 | Method for constructing zinc oxide/attapulgite nano composite antibacterial material by utilizing ginkgo leaf extract |
| CN114532332B (en) * | 2022-01-26 | 2023-03-28 | 中国科学院兰州化学物理研究所 | Method for constructing zinc oxide/attapulgite nano composite antibacterial material by utilizing ginkgo leaf extract |
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