CN107041378A - A kind of yittrium oxide graphene composite Nano antibacterial material, preparation and application - Google Patents
A kind of yittrium oxide graphene composite Nano antibacterial material, preparation and application Download PDFInfo
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- CN107041378A CN107041378A CN201611223063.9A CN201611223063A CN107041378A CN 107041378 A CN107041378 A CN 107041378A CN 201611223063 A CN201611223063 A CN 201611223063A CN 107041378 A CN107041378 A CN 107041378A
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Abstract
The present invention relates to a kind of yittrium oxide graphene composite Nano antibacterial material, preparation and application.Comprise the following steps：Graphene oxide powder is evenly spread in yittrium oxide synthetic system, reacted in autoclave, sediment is centrifuged and dries and stay overnight, obtain yittrium oxide graphene complex；After nano material is sterilized through absolute ethyl alcohol, centrifugation removes supernatant again, adds water and is fully mixed evenly.The yittrium oxide graphene complex material that concentration is not waited is added in certain density Escherichia coli and staphylococcic test tube, is respectively placed in light and dark lower shaken cultivation certain time；Then suppression efficiency of the nano material to gram-positive bacteria and Gram-negative bacteria is analyzed using colony counting method, the yittrium oxide graphene composite material is respectively provided with good inhibition to Gram-negative and positive bacteria, especially suppress efficiency to Gram-negative bacteria very high, and it is environmentally friendly the problems such as will not trigger the drug resistance of bacterium.
Description
Technical field
The present invention relates to a kind of yittrium oxide-graphene composite nano material, belong to antibacterial material preparation field.
Background technology
Health is always one of topic that people most pay close attention to, however, bacterium is ubiquitous, it is all-pervasive, wherein being no lack of cause
The harmful bacteria of disease, their propagation and spreads the serious health that threaten the mankind.In recent years, the biography caused by various pathogenic bacteria
Catch an illness continuous outburst, and antibiotic resistance also constantly strengthens, anti-biotic material research and development are increasingly by scientific and technological circle and industrial circle
Extensive concern.Anti-biotic material is mainly the purpose that suppression is reached by adding antiseptic, bacterium is killed.In recent years, to antibacterial
The requirement of material is also changed into while high bactericidal activity from initially main pursuit bactericidal effect requires there is environment-friendly spy
Property.Nano material due to higher specific surface area and unique physics, chemical property and as a kind of novel antiseptic.
At present, researchers have developed a variety of nano anti-biotic materials, and such as silver nano-grain has been shown to have good antibacterial work(
Effect, can effectively suppress bacterium, virus and other eukaryotic microorganisms.Though nano material has obtained certain development as antiseptic,
But still need to continually develop more efficient and more inexpensive antiseptic.
Photocatalysis antibacterial agent is the inorganic antiseptic of most researching value and DEVELOPMENT PROSPECT at present, its have source it is wide,
It is cheap, the advantages of prepare simple, portion of material can also directly utilize sunshine, make full use of the energy, and to environment without dirt
Dye.Therefore more researchers start to be directed to developing novel photocatalysis antiseptic.
The content of the invention
It is an object of the present invention to problems of the prior art are overcome there is provided a kind of new antiseptic, it is specific to provide
A kind of yittrium oxide-graphene complex, this compound has excellent anti-microbial property and light enhancing anti-microbial property.
Realizing the technical solution of the object of the invention is：A kind of yittrium oxide-graphene composite Nano antibacterial material, the suppression
Bacterium material is composited by yittrium oxide and graphene, wherein, yttrium：The weight ratio of graphene is（2~42.5）:1.
The preparation method of above-mentioned antibacterial material, comprises the following steps：
（1）Weigh a certain amount of six nitric hydrates yttrium, polyvinylpyrrolidone and appropriate graphite oxide and add water and ethanol
In system and stir, then the hydro-thermal reaction at 150 ~ 220 DEG C；
（2）To step（1）Reaction product is centrifuged after moisture removal, is dried after ethanol cleaning, washing, is produced oxidation
Yttrium-graphene complex nano material.
Further, step（1）In, by quality ratio, yttrium nitrate：Polyvinylpyrrolidone=（2~6.25）：1.
Further, step（1）In, the system water of water and ethanol and the volume ratio of ethanol are（0.14~0.33）：1.
Suppressing Gram-negative bacteria and Gram-positive present invention also offers yittrium oxide-graphene composite Nano antibacterial material
Application on bacterium.
In described application, Gram-negative bacteria is Escherichia coli, and gram-positive bacteria is staphylococcus.
Relative to prior art, the present invention achieves following beneficial effect：
1. the structure that graphene regulates and controls yittrium oxide is added in yittrium oxide synthetic system so that compound specific surface area increases, point
Scattered performance improves.And the synergy of yittrium oxide and graphene, effectively reduce the band gap width of composite photocatalyst material so that
It has good photocatalysis antibacterial performance.
2. yttrium in yittrium oxide-graphene composite material produced by the present invention：The weight ratio of graphene is about（2~42.5）:
1, with excellent anti-microbial property and light enhancing anti-microbial property, and cost is relatively low, has for germ contamination waste water very high
Clearance, with higher potential industrial application value.It is the molten of 0.5 ~ 1.0 × 107 CFU/mL for initial bacterial concentration
Liquid, according to 60 mg/L yittrium oxide-graphene, illumination is irradiated 30 minutes（Large intestine）Or 60 minutes（Staphylococcus）Afterwards, removal of bacteria
Rate is up to more than 90%.
The present invention is further detailed explanation with reference to the accompanying drawings and detailed description, accompanying drawing only provide with reference to
Illustrate to use, be not used to the limitation present invention.
Brief description of the drawings
Fig. 1 is the infrared spectrogram of yittrium oxide-graphene complex of the embodiment of the present invention 1.
Fig. 2 be in the present invention yittrium oxide-graphene different operating concentration under dark and light to the antibacterial of Escherichia coli
Rate.
Fig. 3 be in the present invention yittrium oxide-graphene different operating concentration under dark and light to staphylococcic antibacterial
Rate.
Embodiment
Yittrium oxide of the present invention-graphene composite Nano antibacterial material preparation method and its antibacterial technology, including such as
Lower step：
（1）Weigh a certain amount of six nitric hydrates yttrium, polyvinylpyrrolidone and appropriate graphite oxide and add water and ethanol
In system and stir, then solution is transferred in autoclave, reacted at 150 ~ 220 DEG C；
（2）To step（1）Reaction product is centrifuged after moisture removal, is respectively washed for several times with ethanol and deionized water,
By the reaction product drying after cleaning, yittrium oxide-graphene complex nano material is produced；
（3）Take step（2）The mg of product 2 ~ 5 in 1 ~ 2 mL test tubes, add 1 ~ 1.5 milliliter of absolute ethyl alcohol and sterilize 5 ~ 20 minutes,
It is then centrifuged for removing alcohol, adds 0.5 ~ 1.5 milliliter of aqua sterilisa and fully suspend；
（4）Weigh the stirring of 20 ~ 50 g pancreas peptone soybean broths culture mediums to be dissolved in 0.5 ~ 2.0 L water, that is, obtain tryptone
Soybean broth, by pancreas peptone soybean broth, it is divided into two parts.5 ~ 10 are added in wherein a pancreas peptone soybean broth
They, are then placed in high-pressure sterilizing pot and sterilize by g agar powders, i.e. tryptose soya agar culture medium.By the pancreas egg of sterilizing
Flat board is made with standby in white peptone soy agar culture medium, wherein, autoclaved temperature is 110 ~ 125 DEG C, sterilization time is 10 ~
30 minutes；
（5）Take the Escherichia coli preserved at -80 DEG C（Gram-negative bacteria）And staphylococcus（Gram-positive bacteria）, respectively in pancreas
Plate is drawn on peptone soybean agar medium flat board, activation culture is inverted and stays overnight.Then picking monoclonal is in containing 3 ~ 6 mL pancreas eggs
In the test tube of white peptone soy broth, the overnight incubation on shaking table takes the centrifugation of 0.5 ~ 1.5 ml bacterium to remove culture medium, then use
Aqua sterilisa containing 5 ~ 15 g sodium chloride dilutes bacterium, produces Escherichia coli and bacterium is used in staphylococcic experiment, wherein, activation culture
Temperature is 32 ~ 38 DEG C, and shaking table culture temperature is 32 ~ 38 DEG C, and rotating speed is 150 ~ 220 revs/min, and the concentration after dilution is 0.5 ~ 1.0
×107CFU/mL；
（6）Take not same amount step（3）Product is added to 2 ~ 8 mL steps（5）Product in so that by step（3）Product is configured to
10 ~ 100mg/L working concentration.Then these solution are placed under dark and illumination and handled, wherein, processing time 0.5 ~ 2
Hour；Temperature during processing is 32 ~ 38 DEG C, and rotating speed is not less than 150 ~ 220 revs/min, and the power of light is 50 ~ 500 watts；
（7）By step（6）Product dilution 10-1~10-4, then respectively take 50 ~ 200 ul to be evenly coated in tryptose soya agar training
Support on base flat board, be inverted, 32 ~ 38 DEG C of overnight incubations are simultaneously counted；
（8）Calculate removal of bacteria rate or bacteriostasis rate=(C0 − C1)/C0× 100% （C0It is not added with bacterium solution after material process
CFU, C1The CFU added in bacterium solution after material process）.
Embodiment 1
A kind of preparation and application of yittrium oxide-graphene composite Nano antibacterial material of the present invention, in turn include the following steps：
（1）2g graphite powders and 1.5g sodium nitrate mixtures are weighed, 98% mL of the concentrated sulfuric acid 35 is added, stirred 2 hours under ice bath；
（2）Under condition of ice bath, to above-mentioned steps（1）Mixed liquor in add and 4g potassium permanganate and stir；
（3）By step（2）Mixed liquor be placed in 35 DEG C of stirred in water bath 2.5 hours；
（4）Step is taken out from water-bath（3）Mixed liquor, and add 40 mL deionized waters, heating holding be boiling for stirring
2.5h；
（5）By step（4）Mixed liquor be cooled to normal temperature and add 200 mL deionized water, then add 100 mL peroxide
Change hydrogen, solidliquid mixture is obtained after stirring；
（6）By step（5）Then obtained solidliquid mixture is washed with deionized 4 times with 4% salt acid elution 4 times, is made solid
The pH value of liquid mixture is more than 6.8；
（7）To step（6）The solidliquid mixture of gained is centrifuged removing moisture and obtains graphene oxide solid, centrifuges
The rotating speed of separation is 4000 revs/min, and the time is 20 minutes；
（8）Step（7）The graphene oxide solid of gained is dried 16 hours at 60 DEG C, is then ground to graphene oxide
Powder is standby；
（9）Weigh the nitric hydrate yttriums of 1.552 g six, 0.5 g polyvinylpyrrolidones and 50mg steps（8）Product add
In the system of 14mL water and 66mL ethanol and stir, then solution is transferred in autoclave, it is anti-at 160 DEG C
Should；
（10）To step（9）Reaction product is centrifuged after moisture removal, is respectively washed with ethanol and deionized water 4 times,
Reaction product after cleaning is placed in dry in 60 DEG C of baking ovens and stayed overnight, yittrium oxide-graphene complex nano material is produced, such as schemed
1；
（11）Take step（10）The mg of product 4 in 1.5mL test tubes, add 1 milliliter of absolute ethyl alcohol and sterilize 10 minutes, Ran Houli
The heart removes alcohol, adds 1 milliliter of aqua sterilisa and fully suspends；
（12）Weigh the stirring of 30 g pancreas peptone soybean broths culture mediums to be dissolved in 1.0 L water, that is, obtain Triptic soya meat
Soup, by pancreas peptone soybean broth, it is divided into two parts.7.5 g agar are added in wherein a pancreas peptone soybean broth
They, are then placed in 121 DEG C of high-pressure sterilizing pots and sterilize 15 minutes by powder, i.e. tryptose soya agar culture medium.Will sterilizing
Tryptose soya agar culture medium flat board is made with standby；
（13）Take the Escherichia coli preserved at -80 DEG C, on tryptose soya agar culture medium flat plate draw plate, at 37 DEG C fall
Activation culture is put to stay overnight.Then picking monoclonal is in the test tube of the culture medium of pancreas peptone soybean broth containing 5mL, at 37 DEG C
With 180 rpm/min rotating speed overnight incubation on shaking table, the centrifugation of 1ml bacterium is taken to remove culture medium, then with the sterilizing of the NaCl containing 8.5g
Bacterium is diluted to 1 ~ 0.5 × 10 by water7CFU/mL, so that preparing coli test uses bacterium；
（14）Take not same amount step（11）Product is added to 5 mL steps（13）Product in so that by step（11）Product is prepared
Into 15mg/L working concentration.Then these solution are placed under 37 DEG C of dark and 400W illumination, with 180 rpm/min
Rotating speed under handle 0.5 hour.
（15）By step（14）Product dilution 10-1、10-2、10-3、10-4, then respectively take 100 ul to be evenly coated in tryptone
On soy agar culture medium flat plate, it is inverted, 37 DEG C of overnight incubations are simultaneously counted；
（16）Calculate removal of bacteria rate or bacteriostasis rate=(C0 − C1)/C0× 100% （C0It is not added with bacterium solution after material process
CFU, C1The CFU added in bacterium solution after material process）.
Dark treatment bacteriostasis rate=(C0 − C1)/C0 × 100%=94.8%
Light handles bacteriostasis rate=(C0 − C1)/C0 × 100%=95.9%。
Embodiment 2
A kind of preparation and application of yittrium oxide-graphene composite Nano antibacterial material of the present invention, in turn include the following steps：
（1）2g graphite powders and 1.5g sodium nitrate mixtures are weighed, 98% mL of the concentrated sulfuric acid 35 is added, stirred 2 hours under ice bath；
（2）Under condition of ice bath, to above-mentioned steps（1）Mixed liquor in add and 4g potassium permanganate and stir；
（3）By step（2）Mixed liquor be placed in 35 DEG C of stirred in water bath 2.5 hours；
（4）Step is taken out from water-bath（3）Mixed liquor, and add 40 mL deionized waters, heating holding be boiling for stirring
2.5h；
（5）By step（4）Mixed liquor be cooled to normal temperature and add 200 mL deionized water, then add 100 mL peroxide
Change hydrogen, solidliquid mixture is obtained after stirring；
（6）By step（5）Then obtained solidliquid mixture is washed with deionized 4 times with 4% salt acid elution 4 times, is made solid
The pH value of liquid mixture is more than 6.8；
（7）To step（6）The solidliquid mixture of gained is centrifuged removing moisture and obtains graphene oxide solid, centrifuges
The rotating speed of separation is 4000 revs/min, and the time is 20 minutes；
（8）Step（7）The graphene oxide solid of gained is dried 16 hours at 60 DEG C, is then ground to graphene oxide
Powder is standby；
（9）Weigh the nitric hydrate yttriums of 1.552 g six, 0.5 g polyvinylpyrrolidones and 50mg steps（8）Product add
In the system of 14mL water and 66mL ethanol and stir, then solution is transferred in autoclave, it is anti-at 160 DEG C
Should；
（10）To step（9）Reaction product is centrifuged after moisture removal, is respectively washed with ethanol and deionized water 4 times,
Reaction product after cleaning is placed in dry in 60 DEG C of baking ovens and stayed overnight, yittrium oxide-graphene complex nano material is produced；
（11）Take step（10）The mg of product 4 in 1.5mL test tubes, add 1 milliliter of absolute ethyl alcohol and sterilize 10 minutes, Ran Houli
The heart removes alcohol, adds 1 milliliter of aqua sterilisa and fully suspends；
（12）Weigh the stirring of 30 g pancreas peptone soybean broths culture mediums to be dissolved in 1.0 L water, that is, obtain Triptic soya meat
Soup, by pancreas peptone soybean broth, it is divided into two parts.7.5 g agar are added in wherein a pancreas peptone soybean broth
They, are then placed in 121 DEG C of high-pressure sterilizing pots and sterilize 15 minutes by powder, i.e. tryptose soya agar culture medium.Will sterilizing
Tryptose soya agar culture medium flat board is made with standby；
（13）Take the Escherichia coli preserved at -80 DEG C, on tryptose soya agar culture medium flat plate draw plate, at 37 DEG C fall
Activation culture is put to stay overnight.Then picking monoclonal is in the test tube of the culture medium of pancreas peptone soybean broth containing 5mL, at 37 DEG C
With 180 rpm/min rotating speed overnight incubation on shaking table, the centrifugation of 1ml bacterium is taken to remove culture medium, then with the sterilizing of the NaCl containing 8.5g
Bacterium is diluted to 1 ~ 0.5 × 10 by water7CFU/mL, so that preparing coli test uses bacterium；
（14）Take not same amount step（11）Product is added to 5 mL steps（13）Product in so that by step（11）Product is prepared
Into 30mg/L working concentration.Then these solution are placed under 37 DEG C of dark and 400W illumination, with 180 rpm/min
Rotating speed under handle 0.5 hour.
（15）By step（14）Product dilution 10-1、10-2、10-3、10-4, then respectively take 100 ul to be evenly coated in tryptone
On soy agar culture medium flat plate, it is inverted, 37 DEG C of overnight incubations are simultaneously counted；
（16）Calculate removal of bacteria rate or bacteriostasis rate=(C0 − C1)/C0× 100% （C0It is not added with bacterium solution after material process
CFU, C1The CFU added in bacterium solution after material process）.
Dark treatment bacteriostasis rate=(C0 − C1)/C0 × 100%=97.5%
Light handles bacteriostasis rate=(C0 − C1)/C0 × 100%=99.7%。
Embodiment 3
A kind of preparation and application of yittrium oxide-graphene composite Nano antibacterial material of the present invention, in turn include the following steps：
（1）2g graphite powders and 1.5g sodium nitrate mixtures are weighed, 98% mL of the concentrated sulfuric acid 35 is added, stirred 2 hours under ice bath；
（2）Under condition of ice bath, to above-mentioned steps（1）Mixed liquor in add and 4g potassium permanganate and stir；
（3）By step（2）Mixed liquor be placed in 35 DEG C of stirred in water bath 2.5 hours；
（4）Step is taken out from water-bath（3）Mixed liquor, and add 40 mL deionized waters, heating holding be boiling for stirring
2.5h；
（5）By step（4）Mixed liquor be cooled to normal temperature and add 200 mL deionized water, then add 100 mL peroxide
Change hydrogen, solidliquid mixture is obtained after stirring；
（6）By step（5）Then obtained solidliquid mixture is washed with deionized 4 times with 4% salt acid elution 4 times, is made solid
The pH value of liquid mixture is more than 6.8；
（7）To step（6）The solidliquid mixture of gained is centrifuged removing moisture and obtains graphene oxide solid, centrifuges
The rotating speed of separation is 4000 revs/min, and the time is 20 minutes；
（8）Step（7）The graphene oxide solid of gained is dried 16 hours at 60 DEG C, is then ground to graphene oxide
Powder is standby；
（9）Weigh the nitric hydrate yttriums of 1.552 g six, 0.5 g polyvinylpyrrolidones and 50mg steps（8）Product add
In the system of 14mL water and 66mL ethanol and stir, then solution is transferred in autoclave, it is anti-at 160 DEG C
Should；
（10）To step（9）Reaction product is centrifuged after moisture removal, is respectively washed with ethanol and deionized water 4 times,
Reaction product after cleaning is placed in dry in 60 DEG C of baking ovens and stayed overnight, yittrium oxide-graphene complex nano material is produced；
（11）Take step（10）The mg of product 4 in 1.5mL test tubes, add 1 milliliter of absolute ethyl alcohol and sterilize 10 minutes, Ran Houli
The heart removes alcohol, adds 1 milliliter of aqua sterilisa and fully suspends；
（12）Weigh the stirring of 30 g pancreas peptone soybean broths culture mediums to be dissolved in 1.0 L water, that is, obtain Triptic soya meat
Soup, by pancreas peptone soybean broth, it is divided into two parts.7.5 g agar are added in wherein a pancreas peptone soybean broth
They, are then placed in 121 DEG C of high-pressure sterilizing pots and sterilize 15 minutes by powder, i.e. tryptose soya agar culture medium.Will sterilizing
Tryptose soya agar culture medium flat board is made with standby；
（13）Take the Escherichia coli preserved at -80 DEG C, on tryptose soya agar culture medium flat plate draw plate, at 37 DEG C fall
Activation culture is put to stay overnight.Then picking monoclonal is in the test tube of the culture medium of pancreas peptone soybean broth containing 5mL, at 37 DEG C
With 180 rpm/min rotating speed overnight incubation on shaking table, the centrifugation of 1ml bacterium is taken to remove culture medium, then with the sterilizing of the NaCl containing 8.5g
Bacterium is diluted to 1 ~ 0.5 × 10 by water7CFU/mL, so that preparing coli test uses bacterium；
（14）Take not same amount step（11）Product is added to 5 mL steps（13）Product in so that by step（11）Product is prepared
Into 60mg/L working concentration.Then these solution are placed under 37 DEG C of dark and 400W illumination, with 180 rpm/min
Rotating speed under handle 0.5 hour.
（15）By step（14）Product dilution 10-1、10-2、10-3、10-4, then respectively take 100 ul to be evenly coated in tryptone
On soy agar culture medium flat plate, it is inverted, 37 DEG C of overnight incubations are simultaneously counted；
（16）Calculate removal of bacteria rate or bacteriostasis rate=(C0 − C1)/C0× 100% （C0It is not added with bacterium solution after material process
CFU, C1The CFU added in bacterium solution after material process）.
Dark treatment bacteriostasis rate=(C0 − C1)/C0 × 100%=100%
Light handles bacteriostasis rate=(C0 − C1)/C0 × 100%=100%。
Embodiment 4
A kind of preparation and application of yittrium oxide-graphene composite Nano antibacterial material of the present invention, in turn include the following steps：
（1）2g graphite powders and 1.5g sodium nitrate mixtures are weighed, 98% mL of the concentrated sulfuric acid 35 is added, stirred 2 hours under ice bath；
（2）Under condition of ice bath, to above-mentioned steps（1）Mixed liquor in add and 4g potassium permanganate and stir；
（3）By step（2）Mixed liquor be placed in 35 DEG C of stirred in water bath 2.5 hours；
（4）Step is taken out from water-bath（3）Mixed liquor, and add 40 mL deionized waters, heating holding be boiling for stirring
2.5h；
（5）By step（4）Mixed liquor be cooled to normal temperature and add 200 mL deionized water, then add 100 mL peroxide
Change hydrogen, solidliquid mixture is obtained after stirring；
（6）By step（5）Then obtained solidliquid mixture is washed with deionized 4 times with 4% salt acid elution 4 times, is made solid
The pH value of liquid mixture is more than 6.8；
（7）To step（6）The solidliquid mixture of gained is centrifuged removing moisture and obtains graphene oxide solid, centrifuges
The rotating speed of separation is 4000 revs/min, and the time is 20 minutes；
（8）Step（7）The graphene oxide solid of gained is dried 16 hours at 60 DEG C, is then ground to graphene oxide
Powder is standby；
（9）Weigh the nitric hydrate yttriums of 1.552 g six, 0.5 g polyvinylpyrrolidones and 50mg steps（8）Product add
In the system of 14mL water and 66mL ethanol and stir, then solution is transferred in autoclave, it is anti-at 160 DEG C
Should；
（10）To step（9）Reaction product is centrifuged after moisture removal, is respectively washed with ethanol and deionized water 4 times,
Reaction product after cleaning is placed in dry in 60 DEG C of baking ovens and stayed overnight, yittrium oxide-graphene complex nano material is produced；
（11）Take step（10）The mg of product 4 in 1.5mL test tubes, add 1 milliliter of absolute ethyl alcohol and sterilize 10 minutes, Ran Houli
The heart removes alcohol, adds 1 milliliter of aqua sterilisa and fully suspends；
（12）Weigh the stirring of 30 g pancreas peptone soybean broths culture mediums to be dissolved in 1.0 L water, that is, obtain Triptic soya meat
Soup, by pancreas peptone soybean broth, it is divided into two parts.7.5 g agar are added in wherein a pancreas peptone soybean broth
They, are then placed in 121 DEG C of high-pressure sterilizing pots and sterilize 15 minutes by powder, i.e. tryptose soya agar culture medium.Will sterilizing
Tryptose soya agar culture medium flat board is made with standby；
（13）Take the staphylococcus preserved at -80 DEG C, on tryptose soya agar culture medium flat plate draw plate, at 37 DEG C fall
Activation culture is put to stay overnight.Then picking monoclonal is in the test tube of the culture medium of pancreas peptone soybean broth containing 5mL, at 37 DEG C
With 180 rpm/min rotating speed overnight incubation on shaking table, the centrifugation of 1ml bacterium is taken to remove culture medium, then with the sterilizing of the NaCl containing 8.5g
Bacterium is diluted to 1 ~ 0.5 × 10 by water7CFU/mL, so that preparing staphylococcus experiment uses bacterium；
（14）Take not same amount step（11）Product is added to 5 mL steps（13）Product in so that by step（11）Product is prepared
Into 15mg/L working concentration.Then these solution are placed under 37 DEG C of dark and 400W illumination, with 180 rpm/min
Rotating speed under handle 1 hour.
（15）By step（14）Product dilution 10-1、10-2、10-3、10-4, then respectively take 100 ul to be evenly coated in tryptone
On soy agar culture medium flat plate, it is inverted, 37 DEG C of overnight incubations are simultaneously counted；
（16）Calculate removal of bacteria rate or bacteriostasis rate=(C0 − C1)/C0× 100% （C0It is not added with bacterium solution after material process
CFU, C1The CFU added in bacterium solution after material process）.
Dark treatment bacteriostasis rate=(C0 − C1)/C0 × 100%=42.1%
Light handles bacteriostasis rate=(C0 − C1)/C0 × 100%=46.9%。
Embodiment 5
A kind of preparation and application of yittrium oxide-graphene composite Nano antibacterial material of the present invention, in turn include the following steps：
（1）2g graphite powders and 1.5g sodium nitrate mixtures are weighed, 98% mL of the concentrated sulfuric acid 35 is added, stirred 2 hours under ice bath；
（2）Under condition of ice bath, to above-mentioned steps（1）Mixed liquor in add and 4g potassium permanganate and stir；
（3）By step（2）Mixed liquor be placed in 35 DEG C of stirred in water bath 2.5 hours；
（4）Step is taken out from water-bath（3）Mixed liquor, and add 40 mL deionized waters, heating holding be boiling for stirring
2.5h；
（5）By step（4）Mixed liquor be cooled to normal temperature and add 200 mL deionized water, then add 100 mL peroxide
Change hydrogen, solidliquid mixture is obtained after stirring；
（6）By step（5）Then obtained solidliquid mixture is washed with deionized 4 times with 4% salt acid elution 4 times, is made solid
The pH value of liquid mixture is more than 6.8；
（7）To step（6）The solidliquid mixture of gained is centrifuged removing moisture and obtains graphene oxide solid, centrifuges
The rotating speed of separation is 4000 revs/min, and the time is 20 minutes；
（8）Step（7）The graphene oxide solid of gained is dried 16 hours at 60 DEG C, is then ground to graphene oxide
Powder is standby；
（9）Weigh the nitric hydrate yttriums of 1.552 g six, 0.5 g polyvinylpyrrolidones and 50mg steps（8）Product add
In the system of 14mL water and 66mL ethanol and stir, then solution is transferred in autoclave, it is anti-at 160 DEG C
Should；
（10）To step（9）Reaction product is centrifuged after moisture removal, is respectively washed with ethanol and deionized water 4 times,
Reaction product after cleaning is placed in dry in 60 DEG C of baking ovens and stayed overnight, yittrium oxide-graphene complex nano material is produced；
（11）Take step（10）The mg of product 4 in 1.5mL test tubes, add 1 milliliter of absolute ethyl alcohol and sterilize 10 minutes, Ran Houli
The heart removes alcohol, adds 1 milliliter of aqua sterilisa and fully suspends；
（12）Weigh the stirring of 30 g pancreas peptone soybean broths culture mediums to be dissolved in 1.0 L water, that is, obtain Triptic soya meat
Soup, by pancreas peptone soybean broth, it is divided into two parts.7.5 g agar are added in wherein a pancreas peptone soybean broth
They, are then placed in 121 DEG C of high-pressure sterilizing pots and sterilize 15 minutes by powder, i.e. tryptose soya agar culture medium.Will sterilizing
Tryptose soya agar culture medium flat board is made with standby；
（13）Take the staphylococcus preserved at -80 DEG C, on tryptose soya agar culture medium flat plate draw plate, at 37 DEG C fall
Activation culture is put to stay overnight.Then picking monoclonal is in the test tube of the culture medium of pancreas peptone soybean broth containing 5mL, at 37 DEG C
With 180 rpm/min rotating speed overnight incubation on shaking table, the centrifugation of 1ml bacterium is taken to remove culture medium, then with the sterilizing of the NaCl containing 8.5g
Bacterium is diluted to 1 ~ 0.5 × 10 by water7CFU/mL, so that preparing staphylococcus experiment uses bacterium；
（14）Take not same amount step（11）Product is added to 5 mL steps（13）Product in so that by step（11）Product is prepared
Into 30mg/L working concentration.Then these solution are placed under 37 DEG C of dark and 400W illumination, with 180 rpm/min
Rotating speed under handle 1 hour.
（15）By step（14）Product dilution 10-1、10-2、10-3、10-4, then respectively take 100 ul to be evenly coated in tryptone
On soy agar culture medium flat plate, it is inverted, 37 DEG C of overnight incubations are simultaneously counted；
（16）Calculate removal of bacteria rate or bacteriostasis rate=(C0 − C1)/C0× 100% （C0It is not added with bacterium solution after material process
CFU, C1The CFU added in bacterium solution after material process）.
Dark treatment bacteriostasis rate=(C0 − C1)/C0 × 100%=70.6%
Light handles bacteriostasis rate=(C0 − C1)/C0 × 100%=93.9%。
Embodiment 6
A kind of preparation and application of yittrium oxide-graphene composite Nano antibacterial material of the present invention, in turn include the following steps：
（1）2g graphite powders and 1.5g sodium nitrate mixtures are weighed, 98% mL of the concentrated sulfuric acid 35 is added, stirred 2 hours under ice bath；
（2）Under condition of ice bath, to above-mentioned steps（1）Mixed liquor in add and 4g potassium permanganate and stir；
（3）By step（2）Mixed liquor be placed in 35 DEG C of stirred in water bath 2.5 hours；
（4）Step is taken out from water-bath（3）Mixed liquor, and add 40 mL deionized waters, heating holding be boiling for stirring
2.5h；
（5）By step（4）Mixed liquor be cooled to normal temperature and add 200 mL deionized water, then add 100 mL peroxide
Change hydrogen, solidliquid mixture is obtained after stirring；
（6）By step（5）Then obtained solidliquid mixture is washed with deionized 4 times with 4% salt acid elution 4 times, is made solid
The pH value of liquid mixture is more than 6.8；
（7）To step（6）The solidliquid mixture of gained is centrifuged removing moisture and obtains graphene oxide solid, centrifuges
The rotating speed of separation is 4000 revs/min, and the time is 20 minutes；
（8）Step（7）The graphene oxide solid of gained is dried 16 hours at 60 DEG C, is then ground to graphene oxide
Powder is standby；
（9）Weigh the nitric hydrate yttriums of 1.552 g six, 0.5 g polyvinylpyrrolidones and 50mg steps（8）Product add
In the system of 14mL water and 66mL ethanol and stir, then solution is transferred in autoclave, it is anti-at 160 DEG C
Should；
（10）To step（9）Reaction product is centrifuged after moisture removal, is respectively washed with ethanol and deionized water 4 times,
Reaction product after cleaning is placed in dry in 60 DEG C of baking ovens and stayed overnight, yittrium oxide-graphene complex nano material is produced；
（11）Take step（10）The mg of product 4 in 1.5mL test tubes, add 1 milliliter of absolute ethyl alcohol and sterilize 10 minutes, Ran Houli
The heart removes alcohol, adds 1 milliliter of aqua sterilisa and fully suspends；
（12）Weigh the stirring of 30 g pancreas peptone soybean broths culture mediums to be dissolved in 1.0 L water, that is, obtain Triptic soya meat
Soup, by pancreas peptone soybean broth, it is divided into two parts.7.5 g agar are added in wherein a pancreas peptone soybean broth
They, are then placed in 121 DEG C of high-pressure sterilizing pots and sterilize 15 minutes by powder, i.e. tryptose soya agar culture medium.Will sterilizing
Tryptose soya agar culture medium flat board is made with standby；
（13）Take the staphylococcus preserved at -80 DEG C, on tryptose soya agar culture medium flat plate draw plate, at 37 DEG C fall
Activation culture is put to stay overnight.Then picking monoclonal is in the test tube of the culture medium of pancreas peptone soybean broth containing 5mL, at 37 DEG C
With 180 rpm/min rotating speed overnight incubation on shaking table, the centrifugation of 1ml bacterium is taken to remove culture medium, then with the sterilizing of the NaCl containing 8.5g
Bacterium is diluted to 1 ~ 0.5 × 10 by water7CFU/mL, so that preparing staphylococcus experiment uses bacterium；
（14）Take not same amount step（11）Product is added to 5 mL steps（13）Product in so that by step（11）Product is prepared
Into 60mg/L working concentration.Then these solution are placed under 37 DEG C of dark and 400W illumination, with 180 rpm/min
Rotating speed under handle 1 hour.
（15）By step（14）Product dilution 10-1、10-2、10-3、10-4, then respectively take 100 ul to be evenly coated in tryptone
On soy agar culture medium flat plate, it is inverted, 37 DEG C of overnight incubations are simultaneously counted；
（16）Calculate removal of bacteria rate or bacteriostasis rate=(C0 − C1)/C0× 100% （C0It is not added with bacterium solution after material process
CFU, C1The CFU added in bacterium solution after material process）.
Dark treatment bacteriostasis rate=(C0 − C1)/C0 × 100%=80.9%
Light handles bacteriostasis rate=(C0 − C1)/C0 × 100%=98.9%。
To the data summarization such as following table of embodiment 1 ~ 6, and according to the data drafting pattern 2 of embodiment 1 ~ 3, according to implementation
The data drafting pattern 3 of example 4 ~ 6.
Sh-yz-B type photo catalysis reactor of the photo-irradiation treatment using Shanghai than bright laboratory apparatus Co., Ltd in text.
It the foregoing is only the preferable possible embodiments of the present invention, non-therefore the limitation present invention patent protection model
Enclose.In addition to the implementation, the present invention can also have other embodiment, such as can by the quality and volume of each composition compare
Example amplification several times.All use equivalent substitutions or the technical scheme of equivalent transformation formation, all fall within the protection model of application claims
In enclosing.Technical characteristic of the invention without description can be realized by or using prior art, will not be repeated here.
Claims (7)
1. a kind of yittrium oxide-graphene composite Nano antibacterial material, it is characterised in that the antibacterial material is by yittrium oxide and graphite
Alkene is composited, wherein, yttrium：The weight ratio of graphene is（2~42.5）:1.
2. antibacterial material as claimed in claim 1, it is characterised in that comprise the following steps：
（1）Yttrium nitrate, polyvinylpyrrolidone and graphite oxide are added in the system of water and ethanol and stirred, then
The hydro-thermal reaction at 150 ~ 220 DEG C；
（2）To step（1）Reaction product is centrifuged after moisture removal, is dried after ethanol cleaning, washing, is produced the suppression
Bacterium material.
3. antibacterial material as claimed in claim 2, it is characterised in that step（1）In, by quality ratio, yttrium nitrate：Polyethylene
Pyrrolidones=（2~6.25）：1.
4. antibacterial material as claimed in claim 2, it is characterised in that step（1）In, the system water of water and ethanol and ethanol
Volume ratio is（0.14~0.33）：1.
5. the preparation method of the antibacterial material as described in claim 1-4 is any.
6. yittrium oxide as claimed in claim 1-graphene composite Nano antibacterial material is suppressing Gram-negative bacteria and leather orchid
Application on family name's positive bacteria.
7. application as claimed in claim 6, it is characterised in that Gram-negative bacteria is Escherichia coli, and gram-positive bacteria is
Staphylococcus.
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