CN106622300B - A kind of preparation and application of molybdenum sulfide-ferroso-ferric oxide composite Nano antibacterial material - Google Patents
A kind of preparation and application of molybdenum sulfide-ferroso-ferric oxide composite Nano antibacterial material Download PDFInfo
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- CN106622300B CN106622300B CN201611168994.3A CN201611168994A CN106622300B CN 106622300 B CN106622300 B CN 106622300B CN 201611168994 A CN201611168994 A CN 201611168994A CN 106622300 B CN106622300 B CN 106622300B
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- SZVJSHCCFOBDDC-UHFFFAOYSA-N iron(II,III) oxide Inorganic materials O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 title claims abstract description 38
- 239000000463 material Substances 0.000 title claims abstract description 36
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 title claims abstract description 32
- 229910052750 molybdenum Inorganic materials 0.000 title claims abstract description 32
- 239000011733 molybdenum Substances 0.000 title claims abstract description 32
- 229940056319 ferrosoferric oxide Drugs 0.000 title claims abstract description 26
- 239000002131 composite material Substances 0.000 title claims abstract description 23
- 230000000844 anti-bacterial effect Effects 0.000 title claims abstract description 22
- 238000002360 preparation method Methods 0.000 title abstract description 12
- 241000894006 Bacteria Species 0.000 claims abstract description 63
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 57
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 33
- 238000012360 testing method Methods 0.000 claims abstract description 25
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000002086 nanomaterial Substances 0.000 claims abstract description 15
- 229960000935 dehydrated alcohol Drugs 0.000 claims abstract description 13
- 238000005119 centrifugation Methods 0.000 claims abstract description 11
- 241000588724 Escherichia coli Species 0.000 claims abstract description 9
- 239000000243 solution Substances 0.000 claims description 67
- 235000010469 Glycine max Nutrition 0.000 claims description 65
- 244000068988 Glycine max Species 0.000 claims description 64
- 239000001963 growth medium Substances 0.000 claims description 49
- 229920001817 Agar Polymers 0.000 claims description 39
- 239000008272 agar Substances 0.000 claims description 39
- 239000001888 Peptone Substances 0.000 claims description 35
- 108010080698 Peptones Proteins 0.000 claims description 35
- 235000019319 peptone Nutrition 0.000 claims description 35
- 210000000496 pancreas Anatomy 0.000 claims description 33
- 238000012545 processing Methods 0.000 claims description 22
- 238000003756 stirring Methods 0.000 claims description 22
- 230000001954 sterilising effect Effects 0.000 claims description 18
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 16
- 238000011534 incubation Methods 0.000 claims description 16
- 238000010790 dilution Methods 0.000 claims description 12
- 239000012895 dilution Substances 0.000 claims description 12
- 230000004913 activation Effects 0.000 claims description 10
- 238000000034 method Methods 0.000 claims description 10
- 238000004659 sterilization and disinfection Methods 0.000 claims description 10
- 238000009631 Broth culture Methods 0.000 claims description 9
- 241000191940 Staphylococcus Species 0.000 claims description 9
- 239000011780 sodium chloride Substances 0.000 claims description 8
- 244000046052 Phaseolus vulgaris Species 0.000 claims description 7
- 235000010627 Phaseolus vulgaris Nutrition 0.000 claims description 7
- 235000013372 meat Nutrition 0.000 claims description 7
- 235000014347 soups Nutrition 0.000 claims description 7
- 239000012137 tryptone Substances 0.000 claims description 7
- 230000000249 desinfective effect Effects 0.000 claims description 2
- -1 ferroferric oxide compound Chemical class 0.000 claims description 2
- 239000002537 cosmetic Substances 0.000 claims 1
- 239000010977 jade Substances 0.000 claims 1
- 239000007788 liquid Substances 0.000 claims 1
- 239000013049 sediment Substances 0.000 abstract description 8
- 239000006228 supernatant Substances 0.000 abstract description 8
- 241000192125 Firmicutes Species 0.000 abstract description 6
- 230000005764 inhibitory process Effects 0.000 abstract description 3
- 206010059866 Drug resistance Diseases 0.000 abstract description 2
- 230000005307 ferromagnetism Effects 0.000 abstract description 2
- 230000002401 inhibitory effect Effects 0.000 abstract description 2
- 238000003786 synthesis reaction Methods 0.000 abstract 1
- 239000000047 product Substances 0.000 description 41
- 239000008367 deionised water Substances 0.000 description 16
- 229910021641 deionized water Inorganic materials 0.000 description 16
- 239000007795 chemical reaction product Substances 0.000 description 14
- 235000019441 ethanol Nutrition 0.000 description 11
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 9
- RWVGQQGBQSJDQV-UHFFFAOYSA-M sodium;3-[[4-[(e)-[4-(4-ethoxyanilino)phenyl]-[4-[ethyl-[(3-sulfonatophenyl)methyl]azaniumylidene]-2-methylcyclohexa-2,5-dien-1-ylidene]methyl]-n-ethyl-3-methylanilino]methyl]benzenesulfonate Chemical compound [Na+].C1=CC(OCC)=CC=C1NC1=CC=C(C(=C2C(=CC(C=C2)=[N+](CC)CC=2C=C(C=CC=2)S([O-])(=O)=O)C)C=2C(=CC(=CC=2)N(CC)CC=2C=C(C=CC=2)S([O-])(=O)=O)C)C=C1 RWVGQQGBQSJDQV-UHFFFAOYSA-M 0.000 description 9
- 238000004140 cleaning Methods 0.000 description 8
- 229960004756 ethanol Drugs 0.000 description 8
- YUKQRDCYNOVPGJ-UHFFFAOYSA-N thioacetamide Chemical compound CC(N)=S YUKQRDCYNOVPGJ-UHFFFAOYSA-N 0.000 description 8
- DLFVBJFMPXGRIB-UHFFFAOYSA-N thioacetamide Natural products CC(N)=O DLFVBJFMPXGRIB-UHFFFAOYSA-N 0.000 description 8
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 7
- VTLYFUHAOXGGBS-UHFFFAOYSA-N Fe3+ Chemical compound [Fe+3] VTLYFUHAOXGGBS-UHFFFAOYSA-N 0.000 description 7
- 229910021578 Iron(III) chloride Inorganic materials 0.000 description 7
- 230000032683 aging Effects 0.000 description 7
- 235000000396 iron Nutrition 0.000 description 7
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 description 7
- 239000002609 medium Substances 0.000 description 7
- 239000011259 mixed solution Substances 0.000 description 7
- 239000000843 powder Substances 0.000 description 7
- 230000001376 precipitating effect Effects 0.000 description 7
- 230000000845 anti-microbial effect Effects 0.000 description 5
- 239000003242 anti bacterial agent Substances 0.000 description 4
- 230000003115 biocidal effect Effects 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 230000003321 amplification Effects 0.000 description 1
- 229940088710 antibiotic agent Drugs 0.000 description 1
- 230000001580 bacterial effect Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 231100001261 hazardous Toxicity 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 208000015181 infectious disease Diseases 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 229910001410 inorganic ion Inorganic materials 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 239000002114 nanocomposite Substances 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 238000003199 nucleic acid amplification method Methods 0.000 description 1
- 230000001699 photocatalysis Effects 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 239000001267 polyvinylpyrrolidone Substances 0.000 description 1
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 description 1
- 229920000036 polyvinylpyrrolidone Polymers 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
- 229910052727 yttrium Inorganic materials 0.000 description 1
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 description 1
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/02—Sulfur, selenium or tellurium; Compounds thereof
- B01J27/04—Sulfides
- B01J27/047—Sulfides with chromium, molybdenum, tungsten or polonium
- B01J27/051—Molybdenum
- B01J27/0515—Molybdenum with iron group metals or platinum group metals
-
- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/40—Catalysts, in general, characterised by their form or physical properties characterised by dimensions, e.g. grain size
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/60—Catalysts, in general, characterised by their form or physical properties characterised by their surface properties or porosity
- B01J35/61—Surface area
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/50—Treatment of water, waste water, or sewage by addition or application of a germicide or by oligodynamic treatment
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2303/00—Specific treatment goals
- C02F2303/04—Disinfection
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- Engineering & Computer Science (AREA)
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- Life Sciences & Earth Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Inorganic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- Agronomy & Crop Science (AREA)
- Hydrology & Water Resources (AREA)
- Pest Control & Pesticides (AREA)
- Plant Pathology (AREA)
- Water Supply & Treatment (AREA)
- Dentistry (AREA)
- General Health & Medical Sciences (AREA)
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Abstract
The present invention relates to a kind of preparation and application of molybdenum sulfide-ferroso-ferric oxide composite Nano antibacterial material.Include the following steps: that the nano ferriferrous oxide for obtaining chemical synthesis is evenly spread in molybdenum sulfide synthetic system, reacted in autoclave, sediment separate out is simultaneously dried, and molybdenum sulfide-ferroferric oxide compound is obtained.By nano material after dehydrated alcohol sterilizes, centrifugation removes supernatant again, adds water and is sufficiently mixed evenly.Not equal molybdenum sulfide-ferroferric oxide compound the material of concentration is added to containing in Escherichia coli and staphylococcic test tube, being respectively placed in shaken cultivation on shaking table and analyze inhibition efficiency.Molybdenum sulfide-ferriferrous oxide composite material of the invention only has excellent inhibitory effect to gram-positive bacteria, has good selectivity in certain concentration range to the inhibition of gram-positive bacteria.The problems such as composite nano materials of invention can also be recycled using the ferromagnetism of ferroso-ferric oxide, the environmentally friendly drug resistance that will not cause bacterium.
Description
Technical field
The present invention relates to a kind of molybdenum sulfide-ferroso-ferric oxide composite nano materials preparation technical fields, further relate to antibacterial
Method and technology.
Background technique
Bacterium is widely present in the environment around us.Bacterium infection has seriously threatened the health of people.
Traditional antibacterial agent (such as nanometer Ag, antibiotic etc.), which is widely used in, kills bacterium, but its to environment there are potentially hazardous and
Efficiency is lower, higher cost, has certain limitation.So environment amenable, inexpensive, efficient anti-biotic material
Research and development is critically important.
In recent years, semiconductor is significantly paid close attention to due to its nontoxic, harmless and excellent anti-microbial property.Molybdenum sulfide is
A kind of excellent conductive material, and there is typical two-dimensional structure, it is a kind of good complex carrier.Ferroso-ferric oxide is a kind of
Common ferriferous oxide.Have fabulous resist using molybdenum sulfide-ferriferrous oxide nano composite material prepared by hydrothermal synthesis method
Bacterium performance there is excellent antibacterial to imitate gram-positive bacteria the invention demonstrates that its anti-microbial property has selectivity well
Fruit.
Summary of the invention
It is an object of the present invention to overcome problems of the prior art, a kind of new antibacterial agent is provided, and in particular to
Molybdenum sulfide-ferroferric oxide compound preparation method and antibacterial technology, this compound have excellent anti-microbial property, are a kind of new
The Gram-positive antibacterial agent of type.
Realizing the technical solution of the object of the invention is:
A kind of preparation method of molybdenum sulfide-ferroso-ferric oxide composite Nano antibacterial material, includes the following steps:
(1) ferric chloride (FeCl36H2O) and four water irons are dissolved in the molar ratio that Fe (III): Fe (II) is 2:1
In deionized water, N is advertised into solution2Carry out deoxidation；
(2) solution is placed in 60 DEG C of water-bath, keeps N2It protects and stirs 5min energetically, then by NH4OH solution is slow
Be added in solution until pH be 8, then mixed solution and the aging at 60 DEG C；
(3) sediment in solution is separated by external magnetic field power, and supernatant is poured out.Precipitating is washed with deionized water 4 times,
Then it is dried overnight at 40 DEG C to get nano ferriferrous oxide is arrived；
(4) Sodium Molybdate Dihydrate is weighed, the nano ferriferrous oxide of thioacetamide and appropriate step (3) is added to the water
And stir evenly, then solution is transferred in autoclave, pyroreaction；
(5) after moisture removal being centrifuged to step (4) reaction product, number is respectively washed with ethyl alcohol and deionized water
It is secondary, the reaction product after cleaning is placed in baking oven and is dried overnight to get molybdenum sulfide-ferroferric oxide compound nano material；
Step (4) Sodium Molybdate Dihydrate and thioacetamide, by the meter of substance, ratio is (1~2): (3~7)；Often
1mmol~2mmol Sodium Molybdate Dihydrate is corresponding to be added 40mg~800mg nano ferriferrous oxide and 60mL water.
Reaction temperature described in step (4) is 160~200 DEG C, and the reaction time is 10~18 hours.
The wash number of second alcohol and water described in step (5) be 3~5 times, 60~80 DEG C of oven temperature, drying time 8
~16 hours.
The invention also discloses utilize above-mentioned molybdenum sulfide-antibacterial method of ferroso-ferric oxide composite Nano antibacterial material, packet
Include following steps:
A) it takes molybdenum sulfide -2~5mg of ferroferric oxide compound nano material in 1~2mL test tube, dehydrated alcohol is added
Disinfection is then centrifuged for removal alcohol, and aqua sterilisa is added and sufficiently suspends；
B) stirring of 20~50g pancreas peptone soybean broth culture medium is weighed to be dissolved in 0.5~2.0L water to get tryptose is arrived
Peptone soybean broth, by pancreas peptone soybean broth, it is divided into two parts；It is added 5 in wherein a pancreas peptone soybean broth~
They, are then placed in high-pressure sterilizing pot and sterilize by 10g agar powder, i.e. tryptose soya agar culture medium；By the pancreas of sterilizing
Plate is made with spare in peptone soybean agar medium；
C) Escherichia coli (Gram-negative bacteria) and staphylococcus (gram-positive bacteria) saved at -80 DEG C are taken, respectively
Plate is drawn on tryptose soya agar culture medium flat plate, is inverted activation culture and is stayed overnight；Then picking monoclonal is in containing 3~6mL
In the test tube of pancreas peptone soybean broth culture medium, the overnight incubation on shaking table takes 0.5~1.5ml bacterium centrifugation removal culture medium,
Bacterium is diluted with the aqua sterilisa of the sodium chloride Han 5~15g again and uses bacterium to get Escherichia coli and staphylococcic test；
D) take not same amount step a) product be added in the product of 2~8mL step c), so that step a) product product be matched
The working concentration of 10~100mg/L is made；These solution are then placed in shaking table processing；
E) it by the product dilution of step d), then respectively takes 50~200ul to be evenly coated in tryptose soya agar culture medium and puts down
On plate, it is inverted overnight incubation and counts；
Calculate removal of bacteria rate or bacteriostasis rate=(C0-C1)/C0× 100% (C0CFU after material processing is not added in bacterium solution,
The CFU after material processing is added in C1 bacterium solution).
The volume that dehydrated alcohol is added described in step a) is 1~1.5 milliliter, and disinfecting time is 5~20 minutes, and addition is gone out
The volume of bacterium water is 0.5~1.5 milliliter；Centrifugation rate described in step a) is 2000~6000 revs/min, the cleaning of second alcohol and water
Number is 3~6 times, and baking oven stablizes 60~80 DEG C.
The autoclaved temperature of step b) is 120~125 DEG C, and sterilization time is 10~30 minutes.
Activation culture temperature described in step c) be 32~38 DEG C, shaking table culture temperature be 32~38 DEG C, revolving speed be 150~
220 revs/min, the concentration after dilution is 0.5~1.0 × 107CFU/mL。
0.5~2 hour processing time of step d)；Temperature when processing is 32~38 DEG C, revolving speed not less than 150~
220 revs/min, the power of light is 300~500 watts.
Concentration range after dilution described in step e) is 10-1~10-4, cultivation temperature is 32~38 DEG C.
Compared with the existing technology, the present invention achieve it is following the utility model has the advantages that
1. it is the structure in order to regulate and control molybdenum sulfide that ferroso-ferric oxide is added in molybdenum sulfide synthetic system, promote molybdenum sulfide multiple
Closing object has bigger specific surface area and better dispersion performance, and the synergistic effect of ferroso-ferric oxide and molybdenum sulfide can effectively drop
The band gap width of low molybdenum sulfide, so that it is guaranteed that gained compound has better photocatalysis antibacterial performance.
2. step (7) in first clean the unreacted polyvinylpyrrolidone of removal with ethyl alcohol, then clean removal with deionized water
Unreacted inorganic ions can obtain pure molybdenum sulfide-ferroferric oxide compound nano material.
3. step (8) in be added dehydrated alcohol purpose be removal molybdenum sulfide-ferroferric oxide compound nano material in can
The bacterium that can be carried, guarantees the accuracy of subsequent antibacterial experiment result.
4. yttrium in molybdenum sulfide-ferriferrous oxide composite material produced by the present invention: the molar ratio of iron be about (1.7~
17): 1, there is excellent anti-microbial property and light to enhance anti-microbial property, and cost is relatively low, has very for germ contamination waste water
High removal rate, potential industrial application value with higher.It is 0.5~1.0 × 10 for initial bacterial concentration7CFU/mL's
Water is handled staphylococcus 60 minutes, removal of bacteria rate is up to 90% or more according to 15mg/L molybdenum sulfide-ferroso-ferric oxide.
Molybdenum sulfide-ferriferrous oxide composite material of the invention only has excellent inhibitory effect to gram-positive bacteria,
The inhibition of gram-positive bacteria is had good selectivity in certain concentration range.In addition, the composite nano materials are also
The problems such as ferromagnetism that can use ferroso-ferric oxide is recycled, the environmentally friendly drug resistance that will not cause bacterium.
Detailed description of the invention
Fig. 1 is molybdenum sulfide-ferroferric oxide compound infared spectrum of the embodiment of the present invention 1.
Fig. 2 is bacteriostasis rate of the molybdenum sulfide-ferroso-ferric oxide in different operating concentration to Escherichia coli in the present invention.
Fig. 3 be in the present invention molybdenum sulfide-ferroso-ferric oxide in different operating concentration to staphylococcic bacteriostasis rate.
Specific embodiment
The present invention will be further described in detail below with reference to the accompanying drawings and specific embodiments, attached drawing only provide with reference to
Illustrate to use, it is non-to limit the present invention.
Embodiment 1
A kind of preparation and application of molybdenum sulfide of the invention-ferroso-ferric oxide composite Nano antibacterial material successively include such as
Lower step:
(1) ferric chloride (FeCl36H2O) and four water irons are dissolved in the molar ratio that Fe (III): Fe (II) is 2:1
In ionized water, N is advertised into solution2Carry out deoxidation；
(2) solution is placed in 60 DEG C of water-bath, keeps N2It protects and stirs 5min energetically, then by NH4OH solution is slow
Be added in solution until pH be 8, then mixed solution and the aging at 60 DEG C；
(3) the sediment in solution is separated by external magnetic field power, and supernatant is poured out.Precipitating is washed with deionized water 4 times,
Then it is dried overnight at 40 DEG C to get nano ferriferrous oxide is arrived；
(4) 1mmol Sodium Molybdate Dihydrate is weighed, and the product of 5mmol thioacetamide and 0.5g step (3) adds in 60mL water simultaneously
It stirs evenly, then solution is transferred in autoclave, 200 DEG C are reacted 20 hours；
(5) after (4) moisture removal is centrifuged in reaction product, number is respectively washed with ethyl alcohol and deionized water to step
It is secondary, the reaction product after cleaning is placed in baking oven and is dried overnight to get molybdenum sulfide-ferroferric oxide compound nano material；
(6) take the 2~5mg of product of step (5) in 1~2mL test tube, dehydrated alcohol disinfection is added, be then centrifuged for removal wine
Essence is added aqua sterilisa and sufficiently suspends；
(7) the stirring of 30g pancreas peptone soybean broth culture medium is weighed to be dissolved in 1000mL water to get Triptic soya is arrived
Meat soup, by pancreas peptone soybean broth, it is divided into two parts.7.5g agar is added in wherein a pancreas peptone soybean broth
They, are then placed in high-pressure sterilizing pot by powder, i.e. tryptose soya agar culture medium, sterilize 15 minutes at 121 DEG C.It will go out
Plate is made with spare in the tryptose soya agar culture medium of bacterium.
(8) the Escherichia coli saved at -80 DEG C are taken, plate are drawn on tryptose soya agar culture medium flat plate, at 37 DEG C
Activation culture is inverted 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 the revolving speed overnight incubation of 180rpm/min on shaking table, 1ml bacterium centrifugation removal culture medium, then the sterilizing with the NaCl containing 8.5g are taken
Bacterium is diluted to 1~0.5 × 10 by water7CFU/mL, so that coli test, which is prepared, uses bacterium；
(9) take not that (6) product is added in the product of 2~8mL step (8) same amount step, so that (6) product is configured to by step
The working concentration of 15mg/L.Then these solution are placed on 37 DEG C of shaking table, are handled 2 hours with the revolving speed of 180rpm/min；
(10) by step product dilution (9) at 10-1、10-2、10-3、10-4, then respectively to take 100ul to be evenly coated in tryptone big
On beans agar medium plate, it is inverted overnight incubation at 37 DEG C and counts.
(11) removal of bacteria rate or bacteriostasis rate=(C are calculated0-C1)/C0× 100% (C0After material processing is not added in bacterium solution
The CFU after material processing is added in CFU, C1 bacterium solution)
Bacteriostasis rate=(C0-C1)/C0× 100%=13.4%
Embodiment 2
A kind of preparation and application of molybdenum sulfide of the invention-ferroso-ferric oxide composite Nano antibacterial material successively include such as
Lower step:
(1) ferric chloride (FeCl36H2O) and four water irons are dissolved in the molar ratio that Fe (III): Fe (II) is 2:1
In ionized water, N is advertised into solution2Carry out deoxidation；
(2) solution is placed in 60 DEG C of water-bath, keeps N2It protects and stirs 5min energetically, then by NH4OH solution is slow
Be added in solution until pH be 8, then mixed solution and the aging at 60 DEG C；
(3) the sediment in solution is separated by external magnetic field power, and supernatant is poured out.Precipitating is washed with deionized water 4 times,
Then it is dried overnight at 40 DEG C to get nano ferriferrous oxide is arrived；
(4) 1mmol Sodium Molybdate Dihydrate is weighed, and the product of 5mmol thioacetamide and 0.5g step (3) adds in 60mL water simultaneously
It stirs evenly, then solution is transferred in autoclave, 200 DEG C are reacted 20 hours；
(5) after (4) moisture removal is centrifuged in reaction product, number is respectively washed with ethyl alcohol and deionized water to step
It is secondary, the reaction product after cleaning is placed in baking oven and is dried overnight to get molybdenum sulfide-ferroferric oxide compound nano material；
(6) take the 2~5mg of product of step (5) in 1~2mL test tube, dehydrated alcohol disinfection is added, be then centrifuged for removal wine
Essence is added aqua sterilisa and sufficiently suspends；
(7) the stirring of 30g pancreas peptone soybean broth culture medium is weighed to be dissolved in 1000mL water to get Triptic soya is arrived
Meat soup, by pancreas peptone soybean broth, it is divided into two parts.7.5g agar is added in wherein a pancreas peptone soybean broth
They, are then placed in high-pressure sterilizing pot by powder, i.e. tryptose soya agar culture medium, sterilize 15 minutes at 121 DEG C.It will go out
Plate is made with spare in the tryptose soya agar culture medium of bacterium.
(8) the Escherichia coli saved at -80 DEG C are taken, plate are drawn on tryptose soya agar culture medium flat plate, at 37 DEG C
Activation culture is inverted 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 the revolving speed overnight incubation of 180rpm/min on shaking table, 1ml bacterium centrifugation removal culture medium, then the sterilizing with the NaCl containing 8.5g are taken
Bacterium is diluted to 1~0.5 × 10 by water7CFU/mL, so that coli test, which is prepared, uses bacterium；
(9) take not that (6) product is added in the product of 2~8mL step (8) same amount step, so that (6) product is configured to by step
The working concentration of 30mg/L.Then these solution are placed on 37 DEG C of shaking table, are handled 2 hours with the revolving speed of 180rpm/min；
(10) by step product dilution (9) at 10-1、10-2、10-3、10-4, then respectively to take 100ul to be evenly coated in tryptone big
On beans agar medium plate, it is inverted overnight incubation at 37 DEG C and counts.
(11) removal of bacteria rate or bacteriostasis rate=(C are calculated0-C1)/C0× 100% (C0After material processing is not added in bacterium solution
The CFU after material processing is added in CFU, C1 bacterium solution)
Bacteriostasis rate=(C0-C1)/C0× 100%=17.1%
Embodiment 3
A kind of preparation and application of molybdenum sulfide of the invention-ferroso-ferric oxide composite Nano antibacterial material successively include such as
Lower step:
(1) ferric chloride (FeCl36H2O) and four water irons are dissolved in the molar ratio that Fe (III): Fe (II) is 2:1
In ionized water, N is advertised into solution2Carry out deoxidation；
(2) solution is placed in 60 DEG C of water-bath, keeps N2It protects and stirs 5min energetically, then by NH4OH solution is slow
Be added in solution until pH be 8, then mixed solution and the aging at 60 DEG C；
(3) the sediment in solution is separated by external magnetic field power, and supernatant is poured out.Precipitating is washed with deionized water 4 times,
Then it is dried overnight at 40 DEG C to get nano ferriferrous oxide is arrived；
(4) 1mmol Sodium Molybdate Dihydrate is weighed, and the product of 5mmol thioacetamide and 0.5g step (3) adds in 60mL water simultaneously
It stirs evenly, then solution is transferred in autoclave, 200 DEG C are reacted 20 hours；
(5) after (4) moisture removal is centrifuged in reaction product, number is respectively washed with ethyl alcohol and deionized water to step
It is secondary, the reaction product after cleaning is placed in baking oven and is dried overnight to get molybdenum sulfide-ferroferric oxide compound nano material；
(6) take the 2~5mg of product of step (5) in 1~2mL test tube, dehydrated alcohol disinfection is added, be then centrifuged for removal wine
Essence is added aqua sterilisa and sufficiently suspends；
(7) the stirring of 30g pancreas peptone soybean broth culture medium is weighed to be dissolved in 1000mL water to get Triptic soya is arrived
Meat soup, by pancreas peptone soybean broth, it is divided into two parts.7.5g agar is added in wherein a pancreas peptone soybean broth
They, are then placed in high-pressure sterilizing pot by powder, i.e. tryptose soya agar culture medium, sterilize 15 minutes at 121 DEG C.It will go out
Plate is made with spare in the tryptose soya agar culture medium of bacterium.
(8) the Escherichia coli saved at -80 DEG C are taken, plate are drawn on tryptose soya agar culture medium flat plate, at 37 DEG C
Activation culture is inverted 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 the revolving speed overnight incubation of 180rpm/min on shaking table, 1ml bacterium centrifugation removal culture medium, then the sterilizing with the NaCl containing 8.5g are taken
Bacterium is diluted to 1~0.5 × 10 by water7CFU/mL, so that coli test, which is prepared, uses bacterium；
(9) take not that (6) product is added in the product of 2~8mL step (8) same amount step, so that (6) product is configured to by step
The working concentration of 60mg/L.Then these solution are placed on 37 DEG C of shaking table, are handled 2 hours with the revolving speed of 180rpm/min；
(10) by step product dilution (9) at 10-1、10-2、10-3、10-4, then respectively to take 100ul to be evenly coated in tryptone big
On beans agar medium plate, it is inverted overnight incubation at 37 DEG C and counts.
(11) removal of bacteria rate or bacteriostasis rate=(C are calculated0-C1)/C0× 100% (C0After material processing is not added in bacterium solution
The CFU after material processing is added in CFU, C1 bacterium solution)
Bacteriostasis rate=(C0-C1)/C0× 100%=24.1%
Embodiment 4
A kind of preparation and application of molybdenum sulfide of the invention-ferroso-ferric oxide composite Nano antibacterial material successively include such as
Lower step:
(1) ferric chloride (FeCl36H2O) and four water irons are dissolved in the molar ratio that Fe (III): Fe (II) is 2:1
In ionized water, N is advertised into solution2Carry out deoxidation；
(2) solution is placed in 60 DEG C of water-bath, keeps N2It protects and stirs 5min energetically, then by NH4OH solution is slow
Be added in solution until pH be 8, then mixed solution and the aging at 60 DEG C；
(3) the sediment in solution is separated by external magnetic field power, and supernatant is poured out.Precipitating is washed with deionized water 4 times,
Then it is dried overnight at 40 DEG C to get nano ferriferrous oxide is arrived；
(4) 1mmol Sodium Molybdate Dihydrate is weighed, and the product of 5mmol thioacetamide and 0.5g step (3) adds in 60mL water simultaneously
It stirs evenly, then solution is transferred in autoclave, 200 DEG C are reacted 20 hours；
(5) after (4) moisture removal is centrifuged in reaction product, number is respectively washed with ethyl alcohol and deionized water to step
It is secondary, the reaction product after cleaning is placed in baking oven and is dried overnight to get molybdenum sulfide-ferroferric oxide compound nano material；
(6) take the 2~5mg of product of step (5) in 1~2mL test tube, dehydrated alcohol disinfection is added, be then centrifuged for removal wine
Essence is added aqua sterilisa and sufficiently suspends；
(7) the stirring of 30g pancreas peptone soybean broth culture medium is weighed to be dissolved in 1000mL water to get Triptic soya is arrived
Meat soup, by pancreas peptone soybean broth, it is divided into two parts.7.5g agar is added in wherein a pancreas peptone soybean broth
They, are then placed in high-pressure sterilizing pot by powder, i.e. tryptose soya agar culture medium, sterilize 15 minutes at 121 DEG C.It will go out
Plate is made with spare in the tryptose soya agar culture medium of bacterium.
(8) the staphylococcus saved at -80 DEG C is taken, plate is drawn on tryptose soya agar culture medium flat plate, at 37 DEG C
Activation culture is inverted 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 the revolving speed overnight incubation of 180rpm/min on shaking table, 1ml bacterium centrifugation removal culture medium, then the sterilizing with the NaCl containing 8.5g are taken
Bacterium is diluted to 1~0.5 × 10 by water7CFU/mL, so that staphylococcus test, which is prepared, uses bacterium；
(9) take not that (6) product is added in the product of 2~8mL step (8) same amount step, so that (6) product is configured to by step
The working concentration of 15mg/L.Then these solution are placed on 37 DEG C of shaking table, are handled 1 hour with the revolving speed of 180rpm/min；
(10) by step product dilution (9) at 10-1、10-2、10-3、10-4, then respectively to take 100ul to be evenly coated in tryptone big
On beans agar medium plate, it is inverted overnight incubation at 37 DEG C and counts.
(11) removal of bacteria rate or bacteriostasis rate=(C are calculated0-C1)/C0× 100% (C0After material processing is not added in bacterium solution
The CFU after material processing is added in CFU, C1 bacterium solution)
Bacteriostasis rate=(C0-C1)/C0× 100%=99.4%
Embodiment 5
A kind of preparation and application of molybdenum sulfide of the invention-ferroso-ferric oxide composite Nano antibacterial material successively include such as
Lower step: (1) ferric chloride (FeCl36H2O) and four water irons are dissolved in the molar ratio that Fe (III): Fe (II) is 2:1
Ionized water
In, N is advertised into solution2Carry out deoxidation；
(2) solution is placed in 60 DEG C of water-bath, keeps N2It protects and stirs 5min energetically, then by NH4OH solution is slow
Be added in solution until pH be 8, then mixed solution and the aging at 60 DEG C；
(3) the sediment in solution is separated by external magnetic field power, and supernatant is poured out.Precipitating is washed with deionized water 4 times,
Then it is dried overnight at 40 DEG C to get nano ferriferrous oxide is arrived；
(4) 1mmol Sodium Molybdate Dihydrate is weighed, and the product of 5mmol thioacetamide and 0.5g step (3) adds in 60mL water simultaneously
It stirs evenly, then solution is transferred in autoclave, 200 DEG C are reacted 20 hours；
(5) after (4) moisture removal is centrifuged in reaction product, number is respectively washed with ethyl alcohol and deionized water to step
It is secondary, the reaction product after cleaning is placed in baking oven and is dried overnight to get molybdenum sulfide-ferroferric oxide compound nano material；
(6) take the 2~5mg of product of step (5) in 1~2mL test tube, dehydrated alcohol disinfection is added, be then centrifuged for removal wine
Essence is added aqua sterilisa and sufficiently suspends；
(7) the stirring of 30g pancreas peptone soybean broth culture medium is weighed to be dissolved in 1000mL water to get Triptic soya is arrived
Meat soup, by pancreas peptone soybean broth, it is divided into two parts.7.5g agar is added in wherein a pancreas peptone soybean broth
They, are then placed in high-pressure sterilizing pot by powder, i.e. tryptose soya agar culture medium, sterilize 15 minutes at 121 DEG C.It will go out
Plate is made with spare in the tryptose soya agar culture medium of bacterium.
(8) the staphylococcus saved at -80 DEG C is taken, plate is drawn on tryptose soya agar culture medium flat plate, at 37 DEG C
Activation culture is inverted 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 the revolving speed overnight incubation of 180rpm/min on shaking table, 1ml bacterium centrifugation removal culture medium, then the sterilizing with the NaCl containing 8.5g are taken
Bacterium is diluted to 1~0.5 × 10 by water7CFU/mL, so that staphylococcus test, which is prepared, uses bacterium；
(9) take not that (6) product is added in the product of 2~8mL step (8) same amount step, so that (6) product is configured to by step
The working concentration of 30mg/L.Then these solution are placed on 37 DEG C of shaking table, are handled 1 hour with the revolving speed of 180rpm/min；
(10) by step product dilution (9) at 10-1、10-2、10-3、10-4, then respectively to take 100ul to be evenly coated in tryptone big
On beans agar medium plate, it is inverted overnight incubation at 37 DEG C and counts.
(11) removal of bacteria rate or bacteriostasis rate=(C are calculated0-C1)/C0× 100% (C0After material processing is not added in bacterium solution
The CFU after material processing is added in CFU, C1 bacterium solution)
Bacteriostasis rate=(C0-C1)/C0× 100%=99.6%
Embodiment 6
A kind of preparation and application of molybdenum sulfide of the invention-ferroso-ferric oxide composite Nano antibacterial material successively include such as
Lower step: (1) ferric chloride (FeCl36H2O) and four water irons are dissolved in the molar ratio that Fe (III): Fe (II) is 2:1
Ionized water
In, N is advertised into solution2Carry out deoxidation；
(2) solution is placed in 60 DEG C of water-bath, keeps N2It protects and stirs 5min energetically, then by NH4OH solution is slow
Be added in solution until pH be 8, then mixed solution and the aging at 60 DEG C；
(3) the sediment in solution is separated by external magnetic field power, and supernatant is poured out.Precipitating is washed with deionized water 4 times,
Then it is dried overnight at 40 DEG C to get nano ferriferrous oxide is arrived；
(4) 1mmol Sodium Molybdate Dihydrate is weighed, and the product of 5mmol thioacetamide and 0.5g step (3) adds in 60mL water simultaneously
It stirs evenly, then solution is transferred in autoclave, 200 DEG C are reacted 20 hours；
(5) after (4) moisture removal is centrifuged in reaction product, number is respectively washed with ethyl alcohol and deionized water to step
It is secondary, the reaction product after cleaning is placed in baking oven and is dried overnight to get molybdenum sulfide-ferroferric oxide compound nano material；
(6) take the 2~5mg of product of step (5) in 1~2mL test tube, dehydrated alcohol disinfection is added, be then centrifuged for removal wine
Essence is added aqua sterilisa and sufficiently suspends；
(7) the stirring of 30g pancreas peptone soybean broth culture medium is weighed to be dissolved in 1000mL water to get Triptic soya is arrived
Meat soup, by pancreas peptone soybean broth, it is divided into two parts.7.5g agar is added in wherein a pancreas peptone soybean broth
They, are then placed in high-pressure sterilizing pot by powder, i.e. tryptose soya agar culture medium, sterilize 15 minutes at 121 DEG C.It will go out
Plate is made with spare in the tryptose soya agar culture medium of bacterium.
(8) the staphylococcus saved at -80 DEG C is taken, plate is drawn on tryptose soya agar culture medium flat plate, at 37 DEG C
Activation culture is inverted 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 the revolving speed overnight incubation of 180rpm/min on shaking table, 1ml bacterium centrifugation removal culture medium, then the sterilizing with the NaCl containing 8.5g are taken
Bacterium is diluted to 1~0.5 × 10 by water7CFU/mL, so that staphylococcus test, which is prepared, uses bacterium；
(9) take not that (6) product is added in the product of 2~8mL step (8) same amount step, so that (6) product is configured to by step
The working concentration of 60mg/L.Then these solution are placed on 37 DEG C of shaking table, are handled 1 hour with the revolving speed of 180rpm/min；
(10) by step product dilution (9) at 10-1、10-2、10-3、10-4, then respectively to take 100ul to be evenly coated in tryptone big
On beans agar medium plate, it is inverted overnight incubation at 37 DEG C and counts.
(11) removal of bacteria rate or bacteriostasis rate=(C are calculated0-C1)/C0× 100% (C0After material processing is not added in bacterium solution
The CFU after material processing is added in CFU, C1 bacterium solution)
Bacteriostasis rate=(C0-C1)/C0× 100%=99.9%
To the data summarization such as following table of Examples 1 to 6, and according to the data drafting pattern 2 of Examples 1 to 3, according to reality
Apply the data drafting pattern 3 of example 4~6.
The foregoing is merely the preferable possible embodiments of the present invention, non-therefore limitation patent protection model of the invention
It encloses.In addition to the implementation, the present invention can also have other embodiments, such as can be by ratios such as the quality of each ingredient and volumes
Example amplification several times.It is all using equivalent substitution or equivalent transformation formed technical solution, all fall within the present invention claims protection model
In enclosing.Technical characteristic of the present invention without description can realize that details are not described herein by or using the prior art.
Claims (6)
1. a kind of utilize molybdenum sulfide-antibacterial method of ferroso-ferric oxide composite Nano antibacterial material, which is characterized in that including as follows
Step:
A) it takes molybdenum sulfide -2~5mg of ferroferric oxide compound nano material in 1~2mL test tube, dehydrated alcohol disinfection is added,
It is then centrifuged for removal dehydrated alcohol, aqua sterilisa is added and sufficiently suspends；
B) stirring of 20~50g pancreas peptone soybean broth culture medium is weighed to be dissolved in 0.5~2.0L water to get big to tryptone
Pancreas peptone soybean broth is divided into two parts by beans meat soup；5~10g fine jade is added in wherein a pancreas peptone soybean broth
Then they are placed in high-pressure sterilizing pot and sterilize to get tryptose soya agar culture medium by cosmetics；By the tryptose of sterilizing
Plate is made with spare in peptone soy agar culture medium；
C) Escherichia coli and staphylococcus saved at -80 DEG C are taken, are drawn on tryptose soya agar culture medium flat plate respectively
Plate is inverted activation culture and is stayed overnight；Then picking monoclonal is in the test tube of the culture medium Han 3~6mL pancreas peptone soybean broth,
Overnight incubation on shaking table takes 0.5~1.5mL bacterium centrifugation removal culture medium, then with the aqua sterilisa of the sodium chloride Han 5~15g that bacterium is dilute
It releases and uses bacterium to get Escherichia coli and staphylococcic test；
D) take not same amount step a) product be added in the product of 2~8mL step c), so that step a) product is configured to 10~
The working concentration of 100mg/L；These solution are then placed in shaking table processing；
E) by the product dilution of step d), then 50~200 μ L is respectively taken to be evenly coated on tryptose soya agar culture medium flat plate,
It is inverted overnight incubation and counts；
Calculate removal of bacteria rate or bacteriostasis rate=(C0-C1)/C0× 100%, C0CFU after material processing is not added in bacterium solution, C1Bacterium
The CFU after material processing is added in liquid.
2. it is according to claim 1 a kind of using molybdenum sulfide-antibacterial method of ferroso-ferric oxide composite Nano antibacterial material,
It is characterized in that, the volume that dehydrated alcohol is added described in step a) is 1~1.5 milliliter, disinfecting time is 5~20 minutes, is added
The volume for entering aqua sterilisa is 0.5~1.5 milliliter；Centrifugation rate described in step a) is 2000~6000 revs/min, second alcohol and water
Wash number is 3~6 times, and baking oven stablizes 60~80 DEG C.
3. it is according to claim 1 a kind of using molybdenum sulfide-antibacterial method of ferroso-ferric oxide composite Nano antibacterial material,
It is characterized in that, the autoclaved temperature of step b) is 120~125 DEG C, sterilization time is 10~30 minutes.
4. it is according to claim 1 a kind of using molybdenum sulfide-antibacterial method of ferroso-ferric oxide composite Nano antibacterial material,
It is characterized in that, activation culture temperature described in step c) is 32~38 DEG C, shaking table culture temperature is 32~38 DEG C, and revolving speed is
150~220 revs/min, the concentration after dilution is 0.5~1.0 × 107CFU/mL。
5. it is according to claim 1 a kind of using molybdenum sulfide-antibacterial method of ferroso-ferric oxide composite Nano antibacterial material,
It is characterized in that, 0.5~2 hour processing time of step d)；Temperature when processing is 32~38 DEG C, and revolving speed is not less than 150
~220 revs/min.
6. it is according to claim 1 a kind of using molybdenum sulfide-antibacterial method of ferroso-ferric oxide composite Nano antibacterial material,
It is characterized in that, diluted dilution described in step e) is 10-1~10-4, cultivation temperature is 32~38 DEG C.
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