CN105475354B - A kind of CNT/four acicular type zinc oxide crystal whisker composite antibacterial material and preparation method thereof - Google Patents
A kind of CNT/four acicular type zinc oxide crystal whisker composite antibacterial material and preparation method thereof Download PDFInfo
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- CN105475354B CN105475354B CN201510834608.9A CN201510834608A CN105475354B CN 105475354 B CN105475354 B CN 105475354B CN 201510834608 A CN201510834608 A CN 201510834608A CN 105475354 B CN105475354 B CN 105475354B
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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
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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
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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
Abstract
The invention provides a kind of anti-biotic material containing four acicular type zinc oxide crystal whisker, it is characterized in that ZnOw surface is uniformly attached with CNT.It is verified by experiments, two kinds of materials play synergic remove, better than individually using CNT or exclusive use four acicular type zinc oxide crystal whisker.This material not release metal ions, it is safe, and preparation method step is simple, energy consumption is low.
Description
Technical field：
The present invention relates to a kind of inorganic antibacterial material, and in particular to is loaded with the four acicular type zinc oxide crystal whisker of CNT
Composite antibacterial material and preparation method thereof.
Background technology：
The use of anti-biotic material is effectively to prevent bacterium from producing and growing method the most simple and efficient.Anti-biotic material is
Refer to a kind of new function material with sterilization and bacteria growing inhibiting function.
Zinc oxide has the performance of broad-spectrum antiseptic in itself, and four acicular type zinc oxide crystal whisker is due to nanoscale needle point, receiving
Meter level growth step makes itself and surrounding environment Interaction enhanced, therefore anti-microbial property is more preferable.Research shows four-needle-like zinc oxide
Whisker antibacterial action is mainly derived from its caused hydrogen peroxide (Journal of Fermentation and
Bioengineering 1998 years volume 86 page 521, Langmuir 2013 years volume 29 page 5573).Aoxidized based on four needle-likes
The broad spectrum antibacterial performance and its good safety of zinc whisker, by its compound with nano material or hydridization, it can further improve anti-
Bacterium activity.For example, patent (ZL 2,012 1 0005760.2) uses Nanometer Copper hybrid modification four acicular type zinc oxide crystal whisker, can show
Write and improve its anti-microbial property.
But four acicular type zinc oxide crystal whisker can only by discharge active material antibacterial, antibacterial mechanisms are more single, antibacterial activity not
It is too high.
CNT (CNTs) is a kind of allotrope of carbon, has the unique texture of tubulose.Its excellent energy of adsorption
Power and it will not develop immunity to drugs good basis is all provided as anti-biotic material for CNT.
But CNT should not be used alone as anti-biotic material, because the antibacterial action of CNT is mainly by suction
Attached physical action, antibacterial activity are not high enough.
Although the ZnOw of the heavy metals such as loading nano silvery or Nanometer Copper can be improved anti-by release metal ions
Bacterium activity, but heavy metal requires to use in high product, its use range is restricted.And Nano Silver or
Nanometer copper processing is higher.
The content of the invention
It is an object of the invention to provide a kind of four acicular type zinc oxide crystal whisker composite antibacterial material for loading nonmetallic materials, and
Technique is simple, easy to spread.
The present inventor has found first, carries out loaded modified, two kinds of nanometer materials to four acicular type zinc oxide crystal whisker with CNT
Material can produce concerted catalysis activity, bring more preferable antibacterial effect by mechanism such as structure hybridizations：Both CNT can be played
The effect such as superpower absorption, the effect that four acicular type zinc oxide crystal whisker release active material kills bacterium can be played again, can solve four
Needle-shape zinc oxide crystal whisker is only by discharging the problem of antibacterial mechanisms of active material antibacterial are more single, antibacterial activity is less high.
It is described loaded modified, it is that CNT is evenly affixed to by ZnOw surface by certain method.
Load is different from common mixing, and the material of attachment has certain adhesion with the matrix being supported.It is specifically shown in Fig. 1
With Fig. 3 difference.
Therefore, the invention provides a kind of anti-biotic material containing four acicular type zinc oxide crystal whisker, it is characterized in that also being received containing carbon
Mitron, the CNT are evenly affixed to ZnOw surface.
The scope of CNT and the four acicular type zinc oxide crystal whisker amount ratio is 1:1~10 parts by weight：Preferable amount ratio
It is 1:2.
Due to stronger Van der Waals force between CNT be present, its huge specific surface area and very high major diameter in addition
Than forming it into reunion or winding.To reach the uniform attachment of CNT, should be scattered in the media such as water first.And
CNT does not have hydrophilic active group, is difficult scattered in water.
The present invention has selected graphene oxide aqueous suspensions, greatly improves dispersiveness of the CNT in water, can obtain
The uniform dispersion of CNT.
Graphene oxide not only containing aromatic ring structure but also contained hydrophilic oxy radical, can pass through shape between CNT
The effect stacked into π-π, breaks the mutual entanglement between CNT, and its hydrophilic radical and can increases them
Dispersiveness in water.Be advantageous to CNT by dispersiveness of the graphene oxide raising CNT in water to hang in water
Equably loaded in liquid on four acicular type zinc oxide crystal whisker, just can guarantee that the suction of formed composite antibacterial material CNT
Attached effect cooperates with performance with the bactericidal action of four acicular type zinc oxide crystal whisker, could improve the effect of antibacterial.
The concentration range of the graphene oxide aqueous suspensions is 0.5~2mg/mL, preferred concentration 1mg/mL.
Amount ratio between CNT, four acicular type zinc oxide crystal whisker, graphene oxide aqueous suspensions three is 1:1.5~
2.5:4~6 parts by weight；Preferable amount ratio is 1:2:5 parts by weight.
The preparation method of anti-biotic material of the present invention, its step are：
(a) graphene oxide aqueous suspensions are added in the mixed-powder of CNT and four acicular type zinc oxide crystal whisker；
(b) it is jointly processed by through mechanical agitation and ultrasonic wave, obtains the dispersion liquid of mixed-powder；
(c) filter the dispersion liquid, the decorating film isolated dried, obtain the composite antibacterial material of black powder into
Product.
In step (a), the compound method of the graphene oxide aqueous suspensions is as follows：
(1) graphite oxide is prepared using Hummers methods：Claim 8g graphite powders and 4g NaNO3It is placed in dry 1000mL's
In three-neck flask, it is placed in ice-water bath, adds the 184mL concentrated sulfuric acid, opens agitating device.24g KMnO4 are claimed to be slowly added to
In above-mentioned mixed liquor, controlling reaction temperature is less than 10 DEG C, reacts 3h.It is then transferred to after reacting 1h under 35 DEG C of water-baths, then slowly
368mL water is added, while it is 90 DEG C to set water-bath pot temperature, keeps 90 DEG C of isothermal reaction 3h.Add 20mL H2O2(30%) after
Continuous stirring 15min, then add the dilution of 600mL water and stir evenly, reaction product is transferred to 2000mL large beakers, 2 days is stood, obtains
To graphite oxide.
(2) graphene oxide aqueous suspensions are prepared：After the graphite product stratification after above-mentioned oxidation, go to upper strata clear
Liquid, the reaction product of lower floor is sub-packed in centrifuge tube, existed respectively with 5% HCl, distillation water washing, centrifugal rotational speed control
8000rpm, until centrifuged supernatant pH value is close to 6~7.Then the filemot floating in the upper strata after centrifugation is collected with beaker to produce
Thing, by the product after collection in 100w Ultrasound Instrument ultrasonic 2h, that is, obtain final product graphene oxide.Measure certain body
Long-pending graphene oxide aqueous suspensions, dry, calculate the mass concentration of graphene oxide aqueous suspensions.Hanged in graphene oxide water
The mass concentration that addition water is diluted to graphene oxide in liquid is 0.5~2mg/mL.
In step (b),
The time that mechanical agitation and ultrasonic wave are jointly processed by is 30~90 minutes, preferably 60 minutes.
Churned mechanically speed is 100~200 revs/min, preferably 200 revs/min.
The power of ultrasonic wave is 80~100W, preferably 100W；
The frequency of ultrasonic wave is 30~60kHZ, preferably 40kHZ.
Having for the composite antibacterial material that the present invention obtains widely uses field, and being related to industry includes packaging for foodstuff, meal
Tool, drinking tool, toy for children, family's electrical article, family daily necessity, building and ornament materials, IT product, communication product etc..Example
Such as, the composite antibacterial material is added in the raw material of manufacture plastics, fiber, coating, can obtains that there is each of antibacterial action
Kind material, for manufacturing antibacterial household electrical appliances, antibacterial fabric, antibacterial plastic product, antibiotic packaging material, antibacterial floor, antibacterial man
The products such as tool, antibiotic paint.
Compared with prior art, the beneficial effects of the invention are as follows:
1st, two kinds of materials play synergic remove, than CNT is used alone respectively or the oxidation of four needle-likes is used alone
Zinc whisker bactericidal power is all strong
Play in ZnOw surface, two kinds of mechanism collaborations by carbon nanotube loaded and improve its anti-microbial property：Have
The CNT of adsorption function is adsorbable and fixes bacterium, and the active material of ZnOw release continues directly with bacterium
Bacterium is killed in effect.
Meanwhile the present invention uses graphene oxide as the dispersant of CNT to realize CNT in four needle-like oxygen
Change the uniform and stable load in zinc whisker surface.
Confirmed by contrast experiment：The composite antibacterial material that the present invention obtains than being used alone CNT or independent respectively
It is all strong using four acicular type zinc oxide crystal whisker bactericidal power.
It is smaller than four acicular type zinc oxide crystal whisker composite antibacterial material 4 is used alone after four acicular type zinc oxide crystal whisker is loaded modified
When sterilizing rate brought up to more than 95% from 72.5%, hence it is evident that improve its antibacterial effect.
2nd, not release metal ions, it is safe
Relative to the loading nano silvery of release metal ions or the modification technology of Nanometer Copper, the carbon loaded in the present invention is received
Mitron not release metal ions, safe, environmental pollution is small.
3rd, preparation method step is simple, energy consumption is low.
Brief description of the drawings：
Fig. 1 is the microscopic appearance figure for amplifying 20,000 times of four acicular type zinc oxide crystal whiskers observed with field emission scanning electron microscope；
Fig. 2 is the microscopic appearance figure for amplifying 80,000 times of CNTs observed with field emission scanning electron microscope；
Fig. 3 is to amplify the needle-like of nanotube/tetra- that 40,000 times of embodiments 1 observed obtain with field emission scanning electron microscope to aoxidize
The microscopic appearance figure of zinc whisker composite antibacterial material；
Fig. 4 is to amplify the needle-like of nanotube/tetra- that 80,000 times of embodiments 1 observed obtain with field emission scanning electron microscope to aoxidize
The local microscopic appearance figure in the spicule surface of zinc whisker composite antibacterial material；
Fig. 5 is the CNT/four acicular type zinc oxide crystal whisker composite antibacterial material and alone four needle-like oxygen that embodiment 1 obtains
Change zinc whisker or alone CNT to the antibacterial effect comparison diagram after Escherichia coli sterilization in 4 hours.Wherein：
A is the blank control without anti-biotic material；
B is the antibacterial effect of alone four acicular type zinc oxide crystal whisker；
C is the antibacterial effect of alone CNT；
D is the antibacterial effect for CNT/four acicular type zinc oxide crystal whisker composite antibacterial material that embodiment 1 obtains.
Embodiment：
In following antibacterial experiment, Escherichia coli used are Escherichia coli (ATCC 25922), bacteria suspension used
Concentration be 5.6 × 104Cfu/ml, count of bacteria use the method for plate culture count.
The preparation of 1 CNT of embodiment/four acicular type zinc oxide crystal whisker composite antibacterial material and antibacterial ability measure (one)
Step is：
(a) it is 1 1mg/mL graphene oxide aqueous suspensions to be added to equipped with mass ratio:2 CNT and four needle-likes
In the container of ZnOw mixed-powder, mixed liquor is formed；
(b) by mixed liquor mechanical agitation obtained by step (a) with 200 revs/min of speed and ultrasonic wave with 40kHZ's
Frequency, 100W power are jointly processed by obtaining within 60 minutes CNT/ZnOw composite dispersion liquid；
(c) by composite dispersion liquid obtained by step (b) with organic membrane filtration, dried 12 hours at 70 DEG C after obtain carbon
Nanotube/four acicular type zinc oxide crystal whisker composite antibacterial material.
Fig. 1 and Fig. 2 is to amplify the 20000 times and 80,000 times four-needle-like zinc oxides observed crystalline substances with field emission scanning electron microscope respectively
Must be with CNT microscopic appearance figure.
Fig. 3 is to amplify 40,000 times of obtained CNT/four-needle-like zinc oxides of this example observed with field emission scanning electron microscope
The microscopic appearance figure of whisker composite antibacterial material.
By Fig. 1, Fig. 2 contrast, can be observed, it is in figure 3, all uniform negative on the pin of four acicular type zinc oxide crystal whisker
Carry by the scattered CNT of graphene oxide.
Fig. 4 is that 80,000 times of results observed are amplified on the spicule surface of whisker, and graphene oxide obtains carbon nanotubes
It has been coated on whisker surface.
The CNT that this example is obtained/four acicular type zinc oxide crystal whisker composite antibacterial material is added with every liter containing 5 grams of concentration
Enter into escherichia coli suspension concussion and cultivate 4 hours, the Escherichia coli for testing front and rear are counted, draw 4 hours and sterilize
Rate.
A figures in Fig. 5 are the controls for not adding anti-biotic material, and B figures are non-modified four acicular type zinc oxide crystal whiskers to big
Design sketch after enterobacteria sterilization in 4 hours, C figures are that CNT is to the design sketch after Escherichia coli sterilization in 4 hours, D figures
Antibacterial effect figure of the CNT that this example obtains/four acicular type zinc oxide crystal whisker composite antibacterial material to Escherichia coli.
The result difference of three kinds of materials, 4 hours sterilizing rates is as follows：
The four acicular type zinc oxide crystal whisker of unsupported modification：72.5%；
CNT：63.2%；
CNT/four acicular type zinc oxide crystal whisker composite antibacterial material prepared by this example：99.8%.
The preparation of 2 CNTs of embodiment/four acicular type zinc oxide crystal whisker composite antibacterial material and antibacterial ability measure (two)
Step is：
(a) it is 1 0.5mg/mL graphene oxide aqueous suspensions to be added to equipped with mass ratio:10 CNT and four pins
In the container of shape ZnOw mixed-powder, mixed liquor is formed；
(b) by mixed liquor mechanical agitation obtained by step (a) with 100 revs/min of speed and ultrasonic wave with 40kHZ's
Frequency, 80W power are jointly processed by obtaining within 30 minutes CNT/ZnOw composite dispersion liquid；
(c) by composite dispersion liquid obtained by step (b) with organic membrane filtration, dried 48 hours at 40 DEG C after obtain carbon
Nanotube/four acicular type zinc oxide crystal whisker composite antibacterial material.
The CNT that this example is obtained/four acicular type zinc oxide crystal whisker composite antibacterial material is added with every liter containing 5 grams of concentration
Enter into escherichia coli suspension concussion and cultivate 4 hours, the Escherichia coli for testing front and rear are counted, draw 4 hours and sterilize
Rate.
As a result show：4 hours sterilizing rates are 95.2%.
The preparation of 3 CNTs of embodiment/four acicular type zinc oxide crystal whisker composite antibacterial material and antibacterial ability measure (three)
Step is：
(a) it is 1 2mg/mL graphene oxide aqueous suspensions to be added to equipped with mass ratio:1 CNT and four needle-likes
In the container of ZnOw mixed-powder, mixed liquor is formed；
(b) by mixed liquor mechanical agitation obtained by step (a) with 200 revs/min of speed and ultrasonic wave with 40kHZ's
Frequency, 100W power are jointly processed by obtaining within 60 minutes CNT/ZnOw composite dispersion liquid；
(c) by composite dispersion liquid obtained by step (b) with organic membrane filtration, dried 36 hours at 70 DEG C after obtain carbon
Nanotube/four acicular type zinc oxide crystal whisker composite antibacterial material.
The CNT that this example is obtained/four acicular type zinc oxide crystal whisker composite antibacterial material is added with every liter containing 5 grams of concentration
Enter into escherichia coli suspension concussion and cultivate 4 hours, the Escherichia coli for testing front and rear are counted, draw 4 hours and sterilize
Rate.
As a result show：4 hours sterilizing rates are 99.9%.
The preparation of 4 CNTs of embodiment/four acicular type zinc oxide crystal whisker composite antibacterial material and antibacterial ability measure (four)
Step is：
(a) it is 1 2mg/mL graphene oxide aqueous suspensions to be added to equipped with mass ratio:5 CNT and four needle-likes
In the container of ZnOw mixed-powder, mixed liquor is formed；
(b) by mixed liquor mechanical agitation obtained by step (a) with 200 revs/min of speed and ultrasonic wave with 60kHZ's
Frequency, 100W power are jointly processed by obtaining within 90 minutes CNT/ZnOw composite dispersion liquid；
(c) by composite dispersion liquid obtained by step (b) with organic membrane filtration, dried 24 hours at 60 DEG C after obtain carbon
Nanotube/four acicular type zinc oxide crystal whisker composite antibacterial material.
The CNT that this example is obtained/four acicular type zinc oxide crystal whisker composite antibacterial material is added with every liter containing 5 grams of concentration
Enter into escherichia coli suspension concussion and cultivate 4 hours, the Escherichia coli for testing front and rear are counted, draw 4 hours and sterilize
Rate.
As a result show：4 hours sterilizing rates are 97.2%.
The specific experiment data that above example 1~4 obtains refer to table 1
Antibacterial experiment result of the 1 each anti-biotic material of table to Escherichia coli
It is the SiO 2 powder without antibacterial activity of national standard defined with control sample described in upper table.
Claims (9)
1. a kind of anti-biotic material containing four acicular type zinc oxide crystal whisker, it is characterized in that also containing CNT, the CNT is equal
It is even to be attached to ZnOw surface；The scope of CNT and the four acicular type zinc oxide crystal whisker amount ratio is 1:1~10 weight
Measure part.
2. the anti-biotic material described in claim 1, CNT and the four acicular type zinc oxide crystal whisker amount ratio is 1:2.
3. the anti-biotic material described in claim 1, it is characterized in that, when preparing the anti-biotic material, CNT used is uniform
It is scattered in the dispersion liquid formed in graphene oxide aqueous suspensions.
4. the anti-biotic material described in claim 3, in the graphene oxide aqueous suspensions, the concentration range of graphene oxide is
0.5~2mg/mL.
5. the anti-biotic material described in claim 4, the concentration of graphene oxide is 1mg/mL.
6. the anti-biotic material described in claim 3, CNT, four acicular type zinc oxide crystal whisker, graphene oxide aqueous suspensions three
Between amount ratio be 1:1.5~2.5:4~6 parts by weight.
7. the anti-biotic material described in claim 3, CNT, four acicular type zinc oxide crystal whisker, graphene oxide aqueous suspensions three
Between amount ratio be 1:2:5 parts by weight.
8. the preparation method of anti-biotic material described in claim 1, step are：
(a) graphene oxide aqueous suspensions are added in the mixed-powder of CNT and four acicular type zinc oxide crystal whisker；
(b) it is jointly processed by through mechanical agitation and ultrasonic wave, obtains the dispersion liquid of mixed-powder；
(c) dispersion liquid is filtered, the decorating film isolated is dried, obtains the composite antibacterial material finished product of black powder.
9. the preparation method described in claim 8, in step (a), the compound method of the graphene oxide aqueous suspensions is as follows：
(1) graphite oxide is prepared using Hummers methods：Claim 8g graphite powders and 4g NaNO3Three necks for being placed in dry 1000mL burn
In bottle, it is placed in ice-water bath, adds the 184mL concentrated sulfuric acid, opens agitating device；24g KMnO4 are claimed to be slowly added to above-mentioned mixed
Close in liquid, controlling reaction temperature is less than 10 DEG C, reacts 3h；It is then transferred to after reacting 1h under 35 DEG C of water-baths, is slow added into
368mL water, while it is 90 DEG C to set water-bath pot temperature, keeps 90 DEG C of isothermal reaction 3h；Add 20mL 30% H2O2Continue to stir
15min is mixed, the dilution of 600mL water is then added and stirs evenly, reaction product is transferred to 2000mL large beakers, 2 days is stood, is aoxidized
Graphite；
(2) graphene oxide aqueous suspensions are prepared：After the graphite product stratification after above-mentioned oxidation, supernatant liquor is removed,
The reaction product of lower floor is sub-packed in centrifuge tube, existed respectively with 5% HCl, distillation water washing, centrifugal rotational speed control
8000rpm, until centrifuged supernatant pH value is close to 6~7；Then the filemot floating in the upper strata after centrifugation is collected with beaker to produce
Thing, by the product after collection in 100w Ultrasound Instrument ultrasonic 2h, that is, obtain final product graphene oxide；Measure certain volume
Graphene oxide aqueous suspensions, drying, calculate the mass concentrations of graphene oxide aqueous suspensions；In graphene oxide aqueous suspensions
The mass concentration that addition water is diluted to graphene oxide is 0.5~2mg/mL；
In step (b),
The time that mechanical agitation and ultrasonic wave are jointly processed by is 30~90 minutes；
Churned mechanically speed is 100~200 revs/min；
The power of ultrasonic wave is 80~100W；
The frequency of ultrasonic wave is 30~60kHZ.
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| CN106359373A (en) * | 2016-08-29 | 2017-02-01 | 佛山市高明区尚润盈科技有限公司 | Porous graphene zinc-oxide-loaded antibacterial composite material and preparation method thereof |
| CN109440027B (en) * | 2018-10-31 | 2020-06-23 | 哈尔滨工业大学 | Preparation method of hybrid prefabricated block with whisker surface coated with carbon nano tube |
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