CN105475354A - Carbon nanotube/tetrapod-shaped zinc oxide whisker composite antibacterial material and preparation method thereof - Google Patents
Carbon nanotube/tetrapod-shaped zinc oxide whisker composite antibacterial material and preparation method thereof Download PDFInfo
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- CN105475354A CN105475354A CN201510834608.9A CN201510834608A CN105475354A CN 105475354 A CN105475354 A CN 105475354A CN 201510834608 A CN201510834608 A CN 201510834608A CN 105475354 A CN105475354 A CN 105475354A
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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 tetrapod-shaped zinc oxide whisker-containing antibacterial material. The antibacterial material is characterized in that carbon nanotubes uniformly adhere to the surface of the zinc oxide whisker. An experiment proves that the two materials produce synergetic bactericidal effects better than that of carbon nanotube or tetrapod-shaped zinc oxide whisker. The tetrapod-shaped zinc oxide whisker-containing antibacterial material does not release metal ions and has high safety. The preparation method has simple processes and low energy consumption.
Description
Technical field:
The present invention relates to a kind of inorganic antibacterial material, being specifically related to load has composite antibacterial material of the four acicular type zinc oxide crystal whisker of CNT and preparation method thereof.
Background technology:
Anti-biotic material is used to be effectively prevent bacterium from producing and growing method the most simple and efficient.Anti-biotic material refers to a class new function material with sterilization and bacteria growing inhibiting function.
Zinc oxide itself has the performance of broad-spectrum antiseptic, and four acicular type zinc oxide crystal whisker owing to having nanoscale needle point, nanoscale growth step makes it and surrounding environment Interaction enhanced, therefore anti-microbial property is better.Research shows that four acicular type zinc oxide crystal whisker antibacterial action is mainly derived from the hydrogen peroxide (JournalofFermentationandBioengineering1998 the 86th volume 521 pages, Langmuir2013 the 29th volume 5573 pages) of its generation.Based on broad spectrum antibacterial performance and the good safety thereof of four acicular type zinc oxide crystal whisker, by itself and nano material compound or hydridization, can further improve antibacterial activity.Such as, patent (ZL201210005760.2) adopts Nanometer Copper hybrid modification four acicular type zinc oxide crystal whisker, can significantly improve its anti-microbial property.
But four acicular type zinc oxide crystal whisker can only lean on release of active agent antibacterial, antibacterial mechanisms is more single, antibacterial activity is not too high.
CNT (CNTs) is a kind of allotrope of carbon, has the unique texture of tubulose.The adsorption capacity of its excellence and can not to develop immunity to drugs be all that CNT provides good basis as anti-biotic material.
But should not be used alone CNT as anti-biotic material, because the antibacterial action of CNT is mainly by the physical action of absorption, antibacterial activity is not high enough.
Although the ZnOw of the heavy metal such as loading nano silvery or Nanometer Copper improves antibacterial activity by release metal ions, heavy metal requires can not use in high product, and its scope of application is restricted.And Nano Silver or Nanometer Copper price higher.
Summary of the invention
The object of this invention is to provide a kind of four acicular type zinc oxide crystal whisker composite antibacterial material of load nonmetallic materials, and technique is simple, is easy to promote.
The present inventor's Late Cambrian, carry out loaded modified with CNT to four acicular type zinc oxide crystal whisker, two kinds of nano materials are by mechanism such as structure hybridizations, concerted catalysis activity can be produced, bring better antibacterial effect: the superpower absorption that both can play CNT waits effect, the effect of four acicular type zinc oxide crystal whisker release of active agent kill bacteria can be played again, the problem that antibacterial mechanisms is more single, antibacterial activity is not too high that four acicular type zinc oxide crystal whisker only leans on release of active agent antibacterial can be solved.
Described loaded modified, be, by certain method, even carbon nanotube is attached to ZnOw surface.
Load is different from common mixing, the material of attachment with had certain adhesion by the matrix of load.Specifically see the difference of Fig. 1 and Fig. 3.
Therefore, the invention provides a kind of anti-biotic material containing four acicular type zinc oxide crystal whisker, it is characterized in that described even carbon nanotube is attached to ZnOw surface also containing CNT.
The scope of described CNT and four acicular type zinc oxide crystal whisker amount ratio is 1:1 ~ 10 weight portions: preferable amount ratio is 1:2.
Owing to there is stronger Van der Waals force between CNT, its huge specific surface area and very high draw ratio in addition, makes it be formed and reunites or be wound around.For reaching the even attachment of CNT, first should be scattered in the media such as water.And CNT does not have hydrophilic active group, in water, be difficult to dispersion.
The present invention has selected graphene oxide aqueous suspensions, greatly improves the dispersiveness of CNT in water, can obtain the uniform dispersion of CNT.
Graphene oxide is not only containing aromatic ring structure but also containing hydrophilic oxy radical, can by forming the stacking effect of π-π between CNT, break the mutual entanglement between CNT, and the hydrophilic radical that it has can increase their dispersivenesses in water.Be conducive to CNT by the dispersiveness of graphene oxide raising CNT in water to load to equably on four acicular type zinc oxide crystal whisker in aqueous suspensions, the suction-operated of the composite antibacterial material CNT that guarantee is formed and the bactericidal action of four acicular type zinc oxide crystal whisker are worked in coordination with and are played, and could improve antibacterial effect.
The concentration range of described graphene oxide aqueous suspensions is 0.5 ~ 2mg/mL, and preferred concentration is 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 weight portions; Preferable amount ratio is 1:2:5 weight portion.
The preparation method of anti-biotic material of the present invention, the steps include:
A () adds graphene oxide aqueous suspensions in the mixed-powder of CNT and four acicular type zinc oxide crystal whisker;
B (), through mechanical agitation and ultrasonic co-treatment, obtains the dispersion liquid of mixed-powder;
C () filters described dispersion liquid, isolated decorating film is dry, obtains the composite antibacterial material finished product of black powder.
In step (a), the compound method of described graphene oxide aqueous suspensions is as follows:
(1) adopt Hummers legal system for graphite oxide: to claim 8g graphite powder and 4gNaNO
3be placed in the three-neck flask of dry 1000mL, be placed in ice-water bath, add the concentrated sulfuric acid of 184mL, open agitating device.Claim 24gKMnO4 slowly to add in above-mentioned mixed liquor, control reaction temperature lower than 10 DEG C, reaction 3h.Then after reacting 1h under being transferred to 35 DEG C of water-baths, more slowly add 368mL water, arrange water-bath temperature is 90 DEG C simultaneously, keeps 90 DEG C of isothermal reaction 3h.Add 20mLH
2o
2(30%) continue to stir 15min, add the dilution of 600mL water subsequently and stir evenly, product is transferred to 2000mL large beaker, leaves standstill 2 days, obtain graphite oxide.
(2) graphene oxide aqueous suspensions is prepared: after the graphite product stratification after above-mentioned oxidation, remove supernatant liquor, the product of lower floor is sub-packed in centrifuge tube, respectively with 5% HCl, distilled water washing, centrifugal rotational speed controls at 8000rpm, until centrifuged supernatant pH value is close to 6 ~ 7.Then with beaker collect centrifugal after the filemot floating product in upper strata, by collect after product ultrasonic 2h in the Ultrasound Instrument of 100w, namely obtain end product graphene oxide.Measure the graphene oxide aqueous suspensions of certain volume, dry, calculate the mass concentration of graphene oxide aqueous suspensions.In graphene oxide aqueous suspensions, add the mass concentration that water is diluted to graphene oxide is 0.5 ~ 2mg/mL.
In step (b),
The time of mechanical agitation and ultrasonic co-treatment is 30 ~ 90 minutes, is preferably 60 minutes.
Churned mechanically speed is 100 ~ 200 revs/min, is preferably 200 revs/min.
Hyperacoustic power is 80 ~ 100W, is preferably 100W;
Hyperacoustic frequency is 30 ~ 60kHZ, is preferably 40kHZ.
Having of the composite antibacterial material that the present invention obtains uses field widely, relates to industry and comprises packaging for foodstuff, tableware, drinking tool, toy for children, family's electrical article, family daily necessity, building and ornament materials, IT product, communication product etc.Such as, this composite antibacterial material is added in the raw material manufacturing plastics, fiber, coating, the various materials with antibacterial action can be obtained, for the manufacture of products such as antibacterial household electrical appliances, antibacterial fabric, antibacterial plastic product, antibiotic packaging material, antibacterial floor, antibacterial furniture, antibiotic paints.
Compared with prior art, the invention has the beneficial effects as follows:
1, bi-material plays synergic remove, all stronger than being used alone CNT respectively or being used alone four acicular type zinc oxide crystal whisker bactericidal power
By carbon nanotube loaded in ZnOw surface, the collaborative performance of two kinds of mechanism improves its anti-microbial properties: the CNT with adsorption function is adsorbable and fix bacterium, and active substance and the bacterium of ZnOw release continue direct effect kill bacteria.
Meanwhile, the present invention uses graphene oxide as the dispersant of CNT to realize CNT at four acicular type zinc oxide crystal whisker surface uniform and stable load.
Confirm through contrast experiment: composite antibacterial material that the present invention obtains is all stronger than being used alone CNT respectively or being used alone four acicular type zinc oxide crystal whisker bactericidal power.
After four acicular type zinc oxide crystal whisker is loaded modified, than be used alone four acicular type zinc oxide crystal whisker composite antibacterial material 4 little time sterilizing rate brought up to more than 95% from 72.5%, significantly improve its antibacterial effect.
2, not release metal ions, safety is high
Relative to the loading nano silvery of release metal ions or the modification technology of Nanometer Copper, the CNT of load not release metal ions in the present invention, safety is high, and environmental pollution is little.
3, preparation method's step is simple, energy consumption is low.
Accompanying drawing illustrates:
Fig. 1 is the microscopic appearance figure amplifying the four acicular type zinc oxide crystal whisker that 20,000 times are observed with field emission scanning electron microscope;
Fig. 2 is the microscopic appearance figure amplifying the four acicular type zinc oxide crystal whisker that 80,000 times are observed with field emission scanning electron microscope;
Fig. 3 is the microscopic appearance figure amplifying nanotube/four acicular type zinc oxide crystal whisker composite antibacterial material that 40,000 times of embodiments observed 1 obtain with field emission scanning electron microscope;
Fig. 4 is the microscopic appearance figure of the local, spicule surface of amplifying nanotube/four acicular type zinc oxide crystal whisker composite antibacterial material that 80,000 times of embodiments observed 1 obtain with field emission scanning electron microscope;
Fig. 5 is that CNT/four acicular type zinc oxide crystal whisker composite antibacterial material of obtaining of embodiment 1 and alone four acicular type zinc oxide crystal whisker or alone CNT are to the antibacterial effect comparison diagram after Escherichia coli sterilization in 4 hours.Wherein:
A is the blank 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 of CNT/four acicular type zinc oxide crystal whisker composite antibacterial material that embodiment 1 obtains.
Embodiment:
In following antibacterial experiment, Escherichia coli used are dust Xi Shi Escherichia coli (ATCC25922), and the concentration of bacteria used thereby suspension is 5.6 × 10
4cfu/ml, count of bacteria adopts the method for plate culture count.
Preparation and the antibacterial ability of embodiment 1 CNT/four acicular type zinc oxide crystal whisker composite antibacterial material measure (one)
Step is:
A the graphene oxide aqueous suspensions of 1mg/mL joins in the container that CNT that mass ratio is 1:2 and four acicular type zinc oxide crystal whisker mixed-powder are housed by (), form mixed liquor;
B step (a) gained mixed liquor mechanical agitation is obtained CNT/ZnOw composite dispersion liquid with the speed of 200 revs/min and ultrasonic for 60 minutes with the power co-treatment of the frequency of 40kHZ, 100W by ();
C () by the organic membrane filtration of step (b) gained composite dispersion liquid, obtain CNT/four acicular type zinc oxide crystal whisker composite antibacterial material after dry 12 hours at 70 DEG C.
Fig. 1 and Fig. 2 amplifies 20,000 times and 80,000 times of four acicular type zinc oxide crystal whiskers observed and CNT microscopic appearance figure with field emission scanning electron microscope.
Fig. 3 is the microscopic appearance figure amplifying CNT/four acicular type zinc oxide crystal whisker composite antibacterial material that 40,000 times of these examples observed obtain with field emission scanning electron microscope.
By the contrast of Fig. 1, Fig. 2, can be observed, in figure 3, on the pin of four acicular type zinc oxide crystal whisker, all uniform load 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 carbon nanotubes must be coated on whisker surface by graphene oxide.
The CNT this example obtained/four acicular type zinc oxide crystal whisker composite antibacterial material to join in Escherichia coli suspension containing the concentration of 5 grams with often liter and shakes cultivation 4 hours, counts, draw 4 hours sterilizing rates to the Escherichia coli before and after experiment.
A figure in Fig. 5 is the contrast not adding anti-biotic material, B figure is that the four acicular type zinc oxide crystal whisker of non-modified is to the design sketch after Escherichia coli sterilization in 4 hours, C figure be CNT to the design sketch after Escherichia coli sterilization in 4 hours, D figure is that CNT/four acicular type zinc oxide crystal whisker composite antibacterial material of obtaining of this example is to colibacillary antibacterial effect figure.
The result of three kinds of materials, 4 hours sterilizing rates is as follows respectively:
Not loaded modified four acicular type zinc oxide crystal whisker: 72.5%;
CNT: 63.2%;
CNT/four acicular type zinc oxide crystal whisker the composite antibacterial material of this example preparation: 99.8%.
Preparation and the antibacterial ability of embodiment 2 CNTs/four acicular type zinc oxide crystal whisker composite antibacterial material measure (two)
Step is:
A the graphene oxide aqueous suspensions of 0.5mg/mL joins in the container that CNT that mass ratio is 1:10 and four acicular type zinc oxide crystal whisker mixed-powder are housed by (), form mixed liquor;
B step (a) gained mixed liquor mechanical agitation is obtained CNT/ZnOw composite dispersion liquid with the speed of 100 revs/min and ultrasonic for 30 minutes with the power co-treatment of the frequency of 40kHZ, 80W by ();
C () by the organic membrane filtration of step (b) gained composite dispersion liquid, obtain CNT/four acicular type zinc oxide crystal whisker composite antibacterial material after dry 48 hours at 40 DEG C.
The CNT this example obtained/four acicular type zinc oxide crystal whisker composite antibacterial material to join in Escherichia coli suspension containing the concentration of 5 grams with often liter and shakes cultivation 4 hours, counts, draw 4 hours sterilizing rates to the Escherichia coli before and after experiment.
Result shows: within 4 hours, sterilizing rate is 95.2%.
Preparation and the antibacterial ability of embodiment 3 CNTs/four acicular type zinc oxide crystal whisker composite antibacterial material measure (three)
Step is:
A the graphene oxide aqueous suspensions of 2mg/mL joins in the container that CNT that mass ratio is 1:1 and four acicular type zinc oxide crystal whisker mixed-powder are housed by (), form mixed liquor;
B step (a) gained mixed liquor mechanical agitation is obtained CNT/ZnOw composite dispersion liquid with the speed of 200 revs/min and ultrasonic for 60 minutes with the power co-treatment of the frequency of 40kHZ, 100W by ();
C () by the organic membrane filtration of step (b) gained composite dispersion liquid, obtain CNT/four acicular type zinc oxide crystal whisker composite antibacterial material after dry 36 hours at 70 DEG C.
The CNT this example obtained/four acicular type zinc oxide crystal whisker composite antibacterial material to join in Escherichia coli suspension containing the concentration of 5 grams with often liter and shakes cultivation 4 hours, counts, draw 4 hours sterilizing rates to the Escherichia coli before and after experiment.
Result shows: within 4 hours, sterilizing rate is 99.9%.
Preparation and the antibacterial ability of embodiment 4 CNTs/four acicular type zinc oxide crystal whisker composite antibacterial material measure (four)
Step is:
A the graphene oxide aqueous suspensions of 2mg/mL joins in the container that CNT that mass ratio is 1:5 and four acicular type zinc oxide crystal whisker mixed-powder are housed by (), form mixed liquor;
B step (a) gained mixed liquor mechanical agitation is obtained CNT/ZnOw composite dispersion liquid with the speed of 200 revs/min and ultrasonic for 90 minutes with the power co-treatment of the frequency of 60kHZ, 100W by ();
C () by the organic membrane filtration of step (b) gained composite dispersion liquid, obtain CNT/four acicular type zinc oxide crystal whisker composite antibacterial material after dry 24 hours at 60 DEG C.
The CNT this example obtained/four acicular type zinc oxide crystal whisker composite antibacterial material to join in Escherichia coli suspension containing the concentration of 5 grams with often liter and shakes cultivation 4 hours, counts, draw 4 hours sterilizing rates to the Escherichia coli before and after experiment.
Result shows: within 4 hours, sterilizing rate is 97.2%.
The specific experiment data that above embodiment 1 ~ 4 obtains refer to table 1
The each anti-biotic material of table 1 is to colibacillary antibacterial experiment result
More than control sample described in table, is the SiO 2 powder without antibacterial activity of national standard defined.
Claims (10)
1., containing an anti-biotic material for four acicular type zinc oxide crystal whisker, it is characterized in that described even carbon nanotube is attached to ZnOw surface also containing CNT.
2. anti-biotic material according to claim 1, the scope of described CNT and four acicular type zinc oxide crystal whisker amount ratio is 1:1 ~ 10 weight portions.
3. anti-biotic material according to claim 2, described CNT and four acicular type zinc oxide crystal whisker amount ratio are 1:2.
4. anti-biotic material according to claim 1, is characterized in that, when preparing described anti-biotic material, CNT used is dispersed in the dispersion liquid formed in graphene oxide aqueous suspensions.
5. anti-biotic material according to claim 4, in described graphene oxide aqueous suspensions, the concentration range of graphene oxide is 0.5 ~ 2mg/mL.
6. anti-biotic material according to claim 5, the concentration of graphene oxide is 1mg/mL.
7. anti-biotic material according to claim 4, the amount ratio between CNT, four acicular type zinc oxide crystal whisker, graphene oxide aqueous suspensions three is 1:1.5 ~ 2.5:4 ~ 6 weight portions.
8. anti-biotic material according to claim 4, the amount ratio between CNT, four acicular type zinc oxide crystal whisker, graphene oxide aqueous suspensions three is 1:2:5 weight portion.
9. the preparation method of anti-biotic material described in claim 1, step is:
A () adds graphene oxide aqueous suspensions in the mixed-powder of CNT and four acicular type zinc oxide crystal whisker;
B (), through mechanical agitation and ultrasonic co-treatment, obtains the dispersion liquid of mixed-powder;
C () filters described dispersion liquid, isolated decorating film is dry, obtains the composite antibacterial material finished product of black powder.
10. preparation method according to claim 9, in step (a), the compound method of described graphene oxide aqueous suspensions is as follows:
(1) adopt Hummers legal system for graphite oxide: to claim 8g graphite powder and 4gNaNO
3be placed in the three-neck flask of dry 1000mL, be placed in ice-water bath, add the concentrated sulfuric acid of 184mL, open agitating device; Claim 24gKMnO4 slowly to add in above-mentioned mixed liquor, control reaction temperature lower than 10 DEG C, reaction 3h; Then after reacting 1h under being transferred to 35 DEG C of water-baths, more slowly add 368mL water, arrange water-bath temperature is 90 DEG C simultaneously, keeps 90 DEG C of isothermal reaction 3h; Add 20mLH
2o
2(30%) continue to stir 15min, add the dilution of 600mL water subsequently and stir evenly, product is transferred to 2000mL large beaker, leaves standstill 2 days, obtain graphite oxide;
(2) graphene oxide aqueous suspensions is prepared: after the graphite product stratification after above-mentioned oxidation, remove supernatant liquor, the product of lower floor is sub-packed in centrifuge tube, respectively with 5% HCl, distilled water washing, centrifugal rotational speed controls at 8000rpm, until centrifuged supernatant pH value is close to 6 ~ 7; Then with beaker collect centrifugal after the filemot floating product in upper strata, by collect after product ultrasonic 2h in the Ultrasound Instrument of 100w, namely obtain end product graphene oxide; Measure the graphene oxide aqueous suspensions of certain volume, dry, calculate the mass concentration of graphene oxide aqueous suspensions; In graphene oxide aqueous suspensions, add the mass concentration that water is diluted to graphene oxide is 0.5 ~ 2mg/mL;
In step (b),
The time of mechanical agitation and ultrasonic co-treatment is 30 ~ 90 minutes;
Churned mechanically speed is 100 ~ 200 revs/min;
Hyperacoustic power is 80 ~ 100W;
Hyperacoustic frequency is 30 ~ 60kHZ.
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| Publication number | Publication date |
|---|---|
| CN105475354B (en) | 2018-03-02 |
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