CN106719818A - The preparation method of one metal ion species/oxide composite antibacterial material - Google Patents
The preparation method of one metal ion species/oxide composite antibacterial material Download PDFInfo
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- CN106719818A CN106719818A CN201611031362.2A CN201611031362A CN106719818A CN 106719818 A CN106719818 A CN 106719818A CN 201611031362 A CN201611031362 A CN 201611031362A CN 106719818 A CN106719818 A CN 106719818A
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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
- A01N59/20—Copper
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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 relates to a kind of preparation method of anti-biotic material, more particularly, to the preparation method of one metal ion species/oxide composite antibacterial material, it is primary raw material that the method chooses 13X molecular sieves, zinc chloride, NaOH and copper nitrate, 13X molecular sieves are added after first mixing zinc chloride and NaOH according to a certain percentage, zinc oxide support type 13X molecular sieves are obtained by vibration, roasting, then made ZnO 13X are added in certain density copper nitrate solution, drying is obtained copper ion/zinc oxide composite antibiosis material after vibration；Made Cu2+Copper ion, the weight/mass percentage composition of zinc oxide are respectively 8%~10% and 10%~15% in/ZnO 13X anti-biotic materials；The present invention have it is simple to operate, using low raw-material cost, the advantages of institute's prepared material bactericidal effect is notable.
Description
Technical field
It is compound anti-more particularly, to one metal ion species/oxide the present invention relates to a kind of preparation method of anti-biotic material
The preparation method of bacterium material.
Background technology
Inorganic antiseptic is generally divided into two major classes.The first kind is the sterilized or antibacterial energy using metal ions such as silver, copper, zinc
Power, metal ion is loaded or combination is made metal ion support type antibacterial material in some inorganic material surfaces or its structure
Material.In the metal ion for being used, the antibacterial activity of silver ion is best.Zhang et al. is by the loaded Ag on A type molecular sieve+Prepare the anti-biotic material with very strong bacteriostatic activity；Han Lu et al. is with Ag+For antimicrobial component, 13X molecular sieves are carrier, it is prepared for
Ag-carried antibacterial material, the material has excellent anti-microbial property.But, silver-colored price is higher, and under the conditions of illumination, heating etc. easily
It is converted into elemental silver or silver oxide and causes discoloration, so as to loses antibacterial activity.These unfavorable factors all limit silver in antibacterial
Application in terms of material.Copper is only second to silver as a kind of typical inorganic antibacterial material, its bacteriostasis, compared to organic anti-bacterial material
Material have the advantages that antibacterial persistently, broad-spectrum antiseptic, non-secondary pollution.
Equations of The Second Kind inorganic antiseptic is the antiseptic with photocatalysis such as titanium dioxide and zinc oxide etc..With antibacterial gold
Category ionic material is compared, and photocatalysis antibacterial agent also has sterilizing ability by force, and sterilization of high efficiency, persistent is harmless
Advantage.The zinc oxide that Duan etc. is experimentally confirmed different-shape shows preferable antibacterial effect to Escherichia coli.ZnO
In Zn-ef ficiency be one of the essential trace elements of the human body, as the simple class inorganic, metal oxide of molecular composition, ZnO tools
Have the advantages that nontoxic, raw material is easy to get, preparation cost is low and biocompatibility is good, there is extremely strong chemism, can have with various
Machine thing includes that the organic matter in bacterium occurs oxidation reaction, so as to most germs and virus are killed.
Above-mentioned is the anti-biotic material prepared using single antimicrobial component.This antibacterial material prepared by single antimicrobial component
Expect that its bactericidal effect is less notable, it is difficult to be widely applied in daily life.There is presently no the method for overcoming drawbacks described above.
The content of the invention
The purpose of the present invention is the defect for overcoming prior art, there is provided one kind not only can overcome the disadvantages that using only metal ion or oxygen
The deficiency of the single bactericidal action of compound, and it is simple to operate, using low raw-material cost, and to Gram-negative bacteria Escherichia coli
With one metal ion species/oxide composite antibacterial that gram-positive bacteria staphylococcus aureus is respectively provided with good fungistatic effect
The preparation method of material.
To achieve the above object, the technical scheme that the present invention takes comprises the following steps：
The preparation method of one metal ion species/oxide composite antibacterial material, it is characterised in that：The method is with 13X points
Son sieve is carrier, and 13X molecular sieves are added after first mixing zinc chloride and NaOH, zinc oxide is obtained and bears by vibration, roasting
Load type 13X molecular sieves are ZnO-13X, and then made ZnO-13X is added in copper nitrate solution, and drying is obtained copper after vibration
Ion/zinc oxide composite antibiosis material is Cu2+/ZnO-13X；
The preparation method of the ZnO-13X is that zinc chloride is added by the amount of 1~2 times of 13X molecular sieves ion exchange capacity
To in reactor, then NaOH is added with the amount of 1~2 times of zinc chloride quality successively in the reactor, 100~300ml is added
20~30h is vibrated after deionized water at 60~90 DEG C, 1~5g 13X molecular sieves are subsequently adding, continuation is shaken at 60~90 DEG C
20~30h is swung, centrifugation is dried at 70~90 DEG C after being washed with deionized 3~5 times, forged at 120~150 DEG C
2~5h is burnt, ZnO-13X is obtained；
The Cu2+The preparation method of/ZnO-13X is to prepare nitric acid with the amount of 1~2 times of 13X molecular sieves ion exchange capacity
Copper solution, then adds 1~5g ZnO-13X of above-mentioned preparation in copper nitrate solution, after 8~10h is stirred at 50~70 DEG C
6~8h of ageing, vacuum filtration is washed with deionized 3~5 times after being dried at 70~90 DEG C, and Cu is obtained2+/ZnO-13X；
The Cu2+The assay method of copper ion and zinc oxide content uses ultraviolet spectrophotometry in/ZnO-13X；
The Cu2+/ ZnO-13X is antibacterial and bactericidal activity determines the standard broth dilution recommended using US National laboratory
Method, minimal inhibitory concentration and MBC to Escherichia coli and staphylococcus aureus are respectively 0.1~0.4mg/ml
With 0.8~1.6mg/ml.
The present invention has following beneficial effect：
1) method is unique, simple to operate：Method the method that the present invention is provided is, with 13X molecular sieves as carrier, to make respectively
Standby ZnO-13X and Cu2+/ZnO-13X；The preparation method of the ZnO-13X is by 13X molecular sieve ion exchange capacities by zinc chloride
1~2 times of amount is added in reactor, then in the reactor successively with the amount of 1~2 times of zinc chloride quality add NaOH,
20~30h is vibrated at 60~90 DEG C after adding 100~300ml deionized waters, 1~5g 13X molecular sieves are subsequently adding, continued
20~30h is vibrated at 60~90 DEG C, centrifugation is dried after being washed with deionized 3~5 times at 70~90 DEG C, then at
2~5h is calcined at 120~150 DEG C, ZnO-13X is obtained；The Cu2+The preparation method of/ZnO-13X is with 13X molecular sieve ions
The amount that 1~2 times of exchange capacity prepares copper nitrate solution, and 1~5g ZnO- of above-mentioned preparation are then added in copper nitrate solution
13X, is aged 6~8h after 8~10h is stirred at 50~70 DEG C, and vacuum filtration is washed with deionized 3~5 times after 70~90
Dried at DEG C, Cu is obtained2+/ZnO-13X.The method with the 13X with stronger suction-operated be carrier, by load copper ion and
Zinc oxide prepares composite antibacterial material, and the fungistatic effect of material is improved using the synergic remove of copper ion and zinc oxide.
2) low raw-material cost is used：It is main that this method chooses 13X molecular sieves, zinc chloride, NaOH and copper nitrate
Raw material, adds 13X molecular sieves after first mixing zinc chloride and NaOH according to a certain percentage, oxygen is obtained by vibration, roasting
It is ZnO-13X to change zinc support type 13X molecular sieves, and then made ZnO-13X is added in certain density copper nitrate solution, is shaken
Drying is obtained copper ion/zinc oxide composite antibiosis material i.e. Cu after swinging2+/ZnO-13X.The raw material that the present invention is used is with 13X
Molecular sieve is carrier, and with zinc chloride, NaOH, deionized water etc. as raw material, these raw material sources are easy, low cost.
3) method that the present invention is provided not only makes up the deficiency using only metal ion or the single bactericidal action of oxide, and
Good fungistatic effect is respectively provided with to Gram-negative bacteria Escherichia coli and gram-positive bacteria staphylococcus aureus：The present invention
Simultaneously be carried on 13X carriers two kinds of sterilization components by the method for use, using two kinds of synergic removes of sterilization component, carries
A kind of preparation method of the anti-biotic material for having stronger adsorption capacity and killing action to bacterium is supplied.Experiment shows, uses we
Cu prepared by method2+/ ZnO-13X anti-biotic materials are sterilized to the minimal inhibitory concentration and minimum of Escherichia coli and staphylococcus aureus
Concentration is respectively 0.1~0.4mg/ml and 0.8~1.6mg/ml.
Specific embodiment
The present invention is described in further details with reference to specific embodiment, to be better understood from the present invention.Should
Work as understanding, specific embodiment described herein is only used to explain the present invention, is not intended to limit the present invention.
Embodiment 1：
The preparation method of one metal ion species/oxide composite antibacterial material, the method for weigh 0.63g zinc chloride and
0.76g NaOH, adds 100ml deionized waters, and 2g 13X molecular sieves are added after vibrating 30h at 80 DEG C, then at 80 DEG C
Vibration 30h, centrifugation is dried after being washed with deionized 3 times at 80 DEG C, then in 2h is calcined at 140 DEG C, is obtained
ZnO-13X.1.16g copper nitrates are weighed again to be dissolved in 100ml deionized waters, 2g ZnO-13X are added, after 8h is stirred at 60 DEG C
Ageing 8h, vacuum filtration is washed with deionized 3 times and is dried after 80 DEG C, and Cu is obtained2+/ ZnO-13X composite antibacterial materials
Material.Cu2+Copper ion, the weight/mass percentage composition of zinc oxide are respectively 8.2% and 10.4% in/ZnO-13X.Using US National reality
The standard broth dilution method of room recommendation is tested, Cu is measured2+/ ZnO-13X is minimum antibacterial to Escherichia coli and staphylococcus aureus
Concentration and MBC are respectively 0.4mg/ml and 1.6mg/ml.
Embodiment 2：
The preparation method of one metal ion species/oxide composite antibacterial material, the method for weigh 0.95g zinc chloride and
1.43g NaOH, adds 150ml deionized waters, and 2g 13X molecular sieves are added after vibrating 24h at 70 DEG C, then at 70 DEG C
Vibration 24h, centrifugation is dried after being washed with deionized 4 times at 70 DEG C, then in 3h is calcined at 125 DEG C, is obtained
ZnO-13X.1.74g copper nitrates are weighed again to be dissolved in 150ml deionized waters, 3g ZnO-13X are added, after 10h is stirred at 50 DEG C
Ageing 6h, vacuum filtration is washed with deionized 4 times and is dried after 90 DEG C, and Cu is obtained2+/ ZnO-13X composite antibacterial materials
Material.Cu2+Copper ion, the weight/mass percentage composition of zinc oxide are respectively 8.9% and 11.6% in/ZnO-13X.Using US National reality
The standard broth dilution method of room recommendation is tested, Cu is measured2+/ ZnO-13X is dense to the minimal inhibitory concentration of Escherichia coli and minimum sterilization
Degree is respectively 0.2mg/ml and 0.8mg/ml, and the minimal inhibitory concentration and MBC to staphylococcus aureus are respectively
0.2mg/ml and 1.6mg/ml.
Embodiment 3：
The preparation method of one metal ion species/oxide composite antibacterial material, the method for weigh 1.27g zinc chloride and
2.53g NaOH, adds 200ml deionized waters, and 2g 13X molecular sieves are added after vibrating 20h at 90 DEG C, then at 90 DEG C
Vibration 20h, centrifugation is dried after being washed with deionized 5 times at 90 DEG C, then in 5h is calcined at 130 DEG C, is obtained
ZnO-13X.2.32g copper nitrates are weighed again to be dissolved in 200ml deionized waters, 4g ZnO-13X are added, under being stirred after 6h in 70 DEG C
Ageing 7h, vacuum filtration is washed with deionized 5 times and is dried after 70 DEG C, and Cu is obtained2+/ ZnO-13X composite antibacterial materials
Material.Cu2+Copper ion, the weight/mass percentage composition of zinc oxide are respectively 9.7% and 13.3% in/ZnO-13X.Using US National reality
The standard broth dilution method of room recommendation is tested, Cu is measured2+/ ZnO-13X is minimum antibacterial to Escherichia coli and staphylococcus aureus
Concentration and MBC are respectively 0.1mg/ml and 0.8mg/ml.
The above is only the preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, under the premise without departing from the principles of the invention, some improvements and modifications can also be made, these improvements and modifications also should
It is considered as protection scope of the present invention.
Cu described in this method2+The assay method of copper ion and zinc oxide weight/mass percentage composition uses ultraviolet point in/ZnO-13X
Light photometry.According to test philosophy, Cu in eluent is measured after ion exchange2+、Zn2+Quality, be actually added into copper nitrate,
Cu in the gross mass and eluent of zinc chloride2+、Zn2+The difference of quality try to achieve Cu in modified molecular screen2+, ZnO actual matter
Amount.
The antibacterial and sterilization of the standard broth Dilution material that the US National laboratory described in this method is recommended is lived
Property, it is concretely comprised the following steps：By 13X molecular sieves, ZnO-13X and Cu2+/ ZnO-13X carries out doubling dilution, is subsequently adding test strain
Initial bacterial concentration is set to be l~2 × 106CFU/mL, is mixed, and 24h is cultivated in 37 DEG C of shaking tables.Each concentration does three repetitions,
In three parallel test tubes, have that two or more has no bacterial growth is the minimal inhibitory concentration of material；Bacterial growth will be had no
Test tube be forwarded in the agar plates without antiseptic, then through 37 DEG C culture 24h.Each concentration do three it is parallel, its
In to have have no bacterial growth on two agar plates be the MBC of material.
The test strain Escherichia coli (ATCC 25922) and staphylococcus aureus (ATCC 6538) are from country
Culture Collection.The initial concentration of the test strain is l~2 × 106CFU/ml。
Claims (5)
1. the preparation method of one metal ion species/oxide composite antibacterial material, it is characterised in that：The method is with 13X molecules
It is carrier to sieve, and 13X molecular sieves are added after first mixing zinc chloride and NaOH, zinc oxide is obtained and loads by vibration, roasting
Type 13X molecular sieves are ZnO-13X, and then made ZnO-13X is added in copper nitrate solution, after vibration drying i.e. be obtained copper from
Son/zinc oxide composite antibiosis material is Cu2+/ZnO-13X。
2. the preparation method of one metal ion species as claimed in claim 1/oxide composite antibacterial material, it is characterised in that：
The preparation method of the ZnO-13X is that zinc chloride is added into reactor by the amount of 1 ~ 2 times of 13X molecular sieves ion exchange capacity
In, then after adding NaOH, add 100 ~ 300ml deionized waters with the amount of 1 ~ 2 times of zinc chloride quality successively in the reactor
20 ~ 30h is vibrated at 60 ~ 90 DEG C, 1 ~ 5g 13X molecular sieves are subsequently adding, continues to vibrate 20 ~ 30h at 60 ~ 90 DEG C, centrifugation point
From, dried at 70 ~ 90 DEG C after being washed with deionized 3 ~ 5 times, 2 ~ 5h is calcined at 120 ~ 150 DEG C, ZnO-13X is obtained.
3. the preparation method of one metal ion species as claimed in claim 1/oxide composite antibacterial material, it is characterised in that：
The Cu2+The preparation method of/ZnO-13X is to prepare copper nitrate solution with the amount of 1 ~ 2 times of 13X molecular sieves ion exchange capacity, so
1 ~ 5g ZnO-13X of above-mentioned preparation are added in copper nitrate solution afterwards, 6 ~ 8h is aged after 8 ~ 10h is stirred at 50 ~ 70 DEG C, very
Empty suction filtration, is washed with deionized 3 ~ 5 times after being dried at 70 ~ 90 DEG C, and Cu is obtained2+/ZnO-13X。
4. the preparation method of one metal ion species as claimed in claim 1/oxide composite antibacterial material, it is characterised in that：
The Cu2+The assay method of copper ion and zinc oxide content uses ultraviolet spectrophotometry in/ZnO-13X.
5. the preparation method of one metal ion species as claimed in claim 1/oxide composite antibacterial material, it is characterised in that：
The Cu2+/ ZnO-13X is antibacterial and bactericidal activity determines the standard broth dilution method recommended using US National laboratory, to big
The minimal inhibitory concentration and MBC of enterobacteria and staphylococcus aureus be respectively 0.1 ~ 0.4mg/ml and 0.8 ~
1.6mg/m。
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108892149A (en) * | 2018-06-27 | 2018-11-27 | 沈阳理工大学 | A kind of preparation method of 13X type molecular sieve water purifying material |
| CN111296483A (en) * | 2020-03-05 | 2020-06-19 | 浙江大学 | Preparation method of zinc-containing molecular sieve antibacterial material |
| WO2021102746A1 (en) * | 2019-11-27 | 2021-06-03 | 惠州学院 | Dry powder paint with long-lasting antibacterial and antifungal effect and preparation method therefor |
| CN115777703A (en) * | 2022-11-09 | 2023-03-14 | 普沃思环保科技无锡有限公司 | Metal oxide sterilization material and preparation method and application thereof |
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Cited By (5)
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| WO2021102746A1 (en) * | 2019-11-27 | 2021-06-03 | 惠州学院 | Dry powder paint with long-lasting antibacterial and antifungal effect and preparation method therefor |
| CN111296483A (en) * | 2020-03-05 | 2020-06-19 | 浙江大学 | Preparation method of zinc-containing molecular sieve antibacterial material |
| CN115777703A (en) * | 2022-11-09 | 2023-03-14 | 普沃思环保科技无锡有限公司 | Metal oxide sterilization material and preparation method and application thereof |
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