CN113209959B - Preparation method of load type rod-shaped magnesium oxide composite antibacterial agent - Google Patents
Preparation method of load type rod-shaped magnesium oxide composite antibacterial agent Download PDFInfo
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- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 title claims abstract description 119
- 239000000395 magnesium oxide Substances 0.000 title claims abstract description 118
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 title claims abstract description 118
- 239000002131 composite material Substances 0.000 title claims abstract description 57
- 239000003242 anti bacterial agent Substances 0.000 title claims abstract description 39
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 239000000843 powder Substances 0.000 claims abstract description 16
- 229910052751 metal Inorganic materials 0.000 claims abstract description 7
- 239000002184 metal Substances 0.000 claims abstract description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 57
- 239000008367 deionised water Substances 0.000 claims description 30
- 229910021641 deionized water Inorganic materials 0.000 claims description 30
- 238000001291 vacuum drying Methods 0.000 claims description 22
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 20
- 238000001354 calcination Methods 0.000 claims description 20
- 238000003756 stirring Methods 0.000 claims description 20
- 238000006243 chemical reaction Methods 0.000 claims description 18
- 238000005406 washing Methods 0.000 claims description 13
- 241000894006 Bacteria Species 0.000 claims description 11
- 238000001035 drying Methods 0.000 claims description 10
- 238000009210 therapy by ultrasound Methods 0.000 claims description 10
- 238000005303 weighing Methods 0.000 claims description 10
- 229910052760 oxygen Inorganic materials 0.000 claims description 9
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 7
- 241000192125 Firmicutes Species 0.000 claims description 3
- 239000000022 bacteriostatic agent Substances 0.000 claims description 3
- 229910052708 sodium Inorganic materials 0.000 claims description 3
- 230000000844 anti-bacterial effect Effects 0.000 abstract description 48
- 239000000463 material Substances 0.000 abstract description 28
- 238000000034 method Methods 0.000 abstract description 12
- 239000002073 nanorod Substances 0.000 abstract description 2
- 238000001556 precipitation Methods 0.000 abstract description 2
- 229940088710 antibiotic agent Drugs 0.000 abstract 1
- 230000015556 catabolic process Effects 0.000 abstract 1
- 238000006731 degradation reaction Methods 0.000 abstract 1
- 238000007654 immersion Methods 0.000 abstract 1
- 150000002739 metals Chemical class 0.000 abstract 1
- 238000013033 photocatalytic degradation reaction Methods 0.000 abstract 1
- 238000001179 sorption measurement Methods 0.000 abstract 1
- 235000012245 magnesium oxide Nutrition 0.000 description 95
- 239000011734 sodium Substances 0.000 description 20
- 239000001267 polyvinylpyrrolidone Substances 0.000 description 17
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 description 17
- 229920000036 polyvinylpyrrolidone Polymers 0.000 description 17
- 229910052720 vanadium Inorganic materials 0.000 description 9
- 239000002270 dispersing agent Substances 0.000 description 8
- UINUVOICOPGDCZ-UHFFFAOYSA-N [O-2].[V+5].[Mg+2] Chemical compound [O-2].[V+5].[Mg+2] UINUVOICOPGDCZ-UHFFFAOYSA-N 0.000 description 7
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 description 7
- 230000000694 effects Effects 0.000 description 6
- 238000001228 spectrum Methods 0.000 description 6
- 238000012360 testing method Methods 0.000 description 6
- 241000588724 Escherichia coli Species 0.000 description 5
- 239000011777 magnesium Substances 0.000 description 5
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 4
- 238000002474 experimental method Methods 0.000 description 4
- 239000001301 oxygen Substances 0.000 description 4
- 230000001580 bacterial effect Effects 0.000 description 3
- 239000001963 growth medium Substances 0.000 description 3
- 229910052749 magnesium Inorganic materials 0.000 description 3
- 229910044991 metal oxide Inorganic materials 0.000 description 3
- 150000004706 metal oxides Chemical class 0.000 description 3
- 230000003287 optical effect Effects 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- 229910052709 silver Inorganic materials 0.000 description 3
- 239000000725 suspension Substances 0.000 description 3
- 229920001817 Agar Polymers 0.000 description 2
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 2
- 240000004808 Saccharomyces cerevisiae Species 0.000 description 2
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 2
- 241000700605 Viruses Species 0.000 description 2
- 238000000026 X-ray photoelectron spectrum Methods 0.000 description 2
- 239000008272 agar Substances 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 239000012153 distilled water Substances 0.000 description 2
- TUJKJAMUKRIRHC-UHFFFAOYSA-N hydroxyl Chemical compound [OH] TUJKJAMUKRIRHC-UHFFFAOYSA-N 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 244000005700 microbiome Species 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 230000001737 promoting effect Effects 0.000 description 2
- 102000004169 proteins and genes Human genes 0.000 description 2
- 108090000623 proteins and genes Proteins 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 239000004332 silver Substances 0.000 description 2
- 239000011780 sodium chloride Substances 0.000 description 2
- 230000002195 synergetic effect Effects 0.000 description 2
- 239000012137 tryptone Substances 0.000 description 2
- 229910052725 zinc Inorganic materials 0.000 description 2
- 241000711573 Coronaviridae Species 0.000 description 1
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 1
- 239000012880 LB liquid culture medium Substances 0.000 description 1
- 239000006142 Luria-Bertani Agar Substances 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- 229910019092 Mg-O Inorganic materials 0.000 description 1
- 229910019395 Mg—O Inorganic materials 0.000 description 1
- 229910019501 NaVO3 Inorganic materials 0.000 description 1
- OUUQCZGPVNCOIJ-UHFFFAOYSA-M Superoxide Chemical compound [O-][O] OUUQCZGPVNCOIJ-UHFFFAOYSA-M 0.000 description 1
- 239000013543 active substance Substances 0.000 description 1
- 230000000845 anti-microbial effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 210000000170 cell membrane Anatomy 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000012258 culturing Methods 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000011534 incubation Methods 0.000 description 1
- 230000002045 lasting effect Effects 0.000 description 1
- 238000009630 liquid culture Methods 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 230000036542 oxidative stress Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 238000001338 self-assembly Methods 0.000 description 1
- CMZUMMUJMWNLFH-UHFFFAOYSA-N sodium metavanadate Chemical compound [Na+].[O-][V](=O)=O CMZUMMUJMWNLFH-UHFFFAOYSA-N 0.000 description 1
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/16—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/20—Vanadium, niobium or tantalum
- B01J23/22—Vanadium
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L2/00—Methods or apparatus for disinfecting or sterilising materials or objects other than foodstuffs or contact lenses; Accessories therefor
- A61L2/02—Methods or apparatus for disinfecting or sterilising materials or objects other than foodstuffs or contact lenses; Accessories therefor using physical phenomena
- A61L2/08—Radiation
- A61L2/088—Radiation using a photocatalyst or photosensitiser
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- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/34—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation
- B01J37/341—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation
- B01J37/343—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation of ultrasonic wave energy
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Abstract
The invention discloses a preparation method of a rod-shaped magnesium oxide composite antibacterial agent, which is characterized in that a magnesium oxide nanorod is prepared by a direct precipitation method, and a composite powder material doped with different metals is obtained by an immersion method and can be used for antibacterial and photocatalytic degradation of organic matters and degradation of antibiotics. The material prepared by the invention combines the advantages of strong magnesium oxide adsorption capacity and good antibacterial performance, improves the photoresponse of magnesium oxide by doping different elements, thereby improving the performance of the magnesium oxide in various aspects, and the magnesium oxide composite antibacterial material prepared by the method can play a good application prospect in various fields.
Description
Technical Field
The invention belongs to the technical field of antibacterial material preparation, and particularly relates to a preparation method of a load type rod-shaped magnesium oxide composite antibacterial agent.
Background
Bacteria, viruses, microorganisms and molds are ubiquitous in daily life, and the mass propagation time of the bacteria, the viruses, the microorganisms and the molds threatens the life safety of people. Under the influence of novel coronavirus outbreaks at the end of 2019, the requirements of people on healthy life are higher and higher. Endows the surface of the material with antibacterial performance, adds a layer of protective cover for healthy life, and is always concerned by the scientific community and the society. Magnesium oxide has the characteristics of being non-toxic, efficient, environment-friendly and the like as a low-cost antibacterial agent, and recently draws the attention of scientists. Ag. Cu and Zn always occupy the main market of the antibacterial agent, but the silver cost is high, and the silver is easy to oxidize and discolor in the using process, so that the appearance is influenced; in agriculture, the use of Cu-type antibacterial agents has been banned, and magnesium oxide antibacterial agents have been studied as substitutes for Cu-type antibacterial agents; in addition, the Zn-type antibacterial agent has poor antibacterial property and broad antibacterial spectrum, so that the development of a low-cost, high-efficiency and safe antibacterial agent is imperative.
In phaseIn the related research, it has been pointed out that Ag, cu and Zn are mainly combined with proteins of bacteria, so that the bacteria are denatured and inactivated. The corresponding metal oxide has certain optical property and can generate active substances (superoxide anion (O)) under the irradiation condition of ultraviolet or visible light 2 -), hydroxyl radical (. OH), singlet oxygen (. C.), ( 1 O 2 ) Hydrogen peroxide (H) 2 O 2 ) And causing oxidative stress damage to the cell membrane, protein and DNA of the bacteria to die.
The metal oxide has a certain optical activity catalytic antibacterial effect, and magnesium oxide has been studied as an antibacterial agent, wherein the antibacterial effect of the rod-like and sheet-like is optimal, and O generated by the catalysis of the oxide 2 - Is considered to be a factor of the antibacterial activity of magnesium oxide, and V 2 O 5 An N-type semiconductor responding to visible light has many electrons and is easily excited to react with oxygen in water to generate more O 2 - Thereby improving the antibacterial effect. At the same time, the electron excitation is at V 2 O 5 Leaving a hole (h) in the valence band + ) The reaction with water to generate hydroxyl radical (. OH) also becomes a factor for enhancing the antibacterial effect.
(MgO)e - +O 2 →·O 2 -
·O 2 w+H 2 O→·HO 2 +OH -
·HO 2 +·HO 2 →H 2 O 2 +O 2
(V 2 O 5 )h + +H 2 O→·OH
Magnesium oxide and semiconductor V 2 O 5 And the antibacterial composite material with lasting and high efficiency is prepared by combining the components, and has good application prospect.
Disclosure of Invention
The invention provides a preparation method of a load type rod-shaped magnesium oxide composite antibacterial agent based on optical activity catalytic antibacterial of metal oxide.
In order to realize the purpose, the invention adopts the technical scheme that:
a supported rod-shaped magnesium oxide composite antibacterial agent comprises rod-shaped magnesium oxide doped with metal elements; the rod-shaped magnesium oxide is of a magnesium oxide flower-stick structure with a flaky assembled surface; the doped metal element is V.
Furthermore, the length of the composite antibacterial agent is 5-15 μm, and the diameter of the composite antibacterial agent is 0.5-1.5 μm.
Further, the preparation method of the supported rod-shaped magnesium oxide composite antibacterial agent comprises the following steps:
s1, measuring a certain amount of 1M MgCl 2 ·6H 2 O, adding a certain amount of 1M Na dropwise under the condition of water bath at 50 DEG C 2 CO 3 During which stirring is continued;
s2, waiting for Na 2 CO 3 After the solution is dripped, continuously stirring for 2-4 hours, after the reaction is finished, respectively centrifugally washing the solution for three times by using deionized water and absolute ethyl alcohol, firstly drying the solution in vacuum, and then calcining the solution by using a muffle furnace to obtain rod-shaped magnesium oxide powder;
s3, weighing a certain amount of the rod-shaped magnesium oxide powder obtained in the step S2, adding the rod-shaped magnesium oxide powder into deionized water, and performing ultrasonic dispersion for 4-8min to ensure that the rod-shaped magnesium oxide powder is uniformly dispersed;
s4, dropwise adding NaVO with a certain concentration under the condition of water bath at 40-80 DEG C 3 And (3) after the solution is completely dripped, carrying out ultrasonic treatment for 5-10min, continuously stirring for 3-4 hours, respectively carrying out centrifugal washing on deionized water and absolute ethyl alcohol for 2-3 times, drying in vacuum, and calcining in a muffle furnace to obtain the load-type rod-shaped magnesium oxide composite antibacterial agent.
Further, in step S1, mgCl 2 ·6H 2 O and Na 2 CO 3 1.
Further, in step S1, na 2 CO 3 After the addition, 0-0.4g of PVP is added.
Further, the reaction is carried out at normal temperature and pressure, na 2 CO 3 The dropping speed is 3-4s/d; naVO 3 The dropping speed is 3-4s/d.
Further, in step S2, the drying condition is vacuum drying at 60 ℃; the calcining condition is 600 ℃ and 3 hours; in the step S4, the drying condition is vacuum drying at 60 ℃; the calcination conditions were 600 ℃ for 2 hours.
Further, the stirring rotation speeds in the step S1 and the step S4 are consistent and are 200-300r/min.
Further, the NaVO 3 The concentration of the solution was 1mol/L.
Further, the composite antibacterial agent is used as a bacteriostatic agent for gram-positive bacteria, gram-negative bacteria and moulds.
Compared with the prior art, the invention at least has the following beneficial effects:
(1) The invention adopts a low-cost and simple precipitation method combined with a dipping method to prepare the load type magnesium oxide composite antibacterial material, and the antibacterial durability of the material is researched by a coating flat plate method, so that the material is found to have excellent antibacterial performance; by compounding the element V and the rodlike magnesium oxide, the shape of the rodlike magnesium oxide is influenced on one hand, and the antibacterial effect is obviously improved by the synergistic antibacterial effect on the other hand.
(2) According to the invention, by controlling the reaction preparation method and related experimental parameters, the particle size of the antibacterial material is controlled to be in a micron level, and compared with a common nano-level antibacterial agent, the antibacterial material has a good dispersion effect, is not easy to agglomerate and is not easy to be adsorbed and agglomerated by bacteria.
(3) According to the method, the reaction preparation method and relevant experimental parameters are controlled, the addition of vanadium element is combined, the magnesium oxide appearance is controlled to be in a micron level, and the surface of the magnesium oxide is of a flaky assembled magnesium oxide flower stick structure; the structure integrates the advantages of rod shape and sheet shape, increases the contact sites of the material and bacteria, and further improves the antibacterial effect.
(2) The preparation method combines magnesium oxide and a semiconductor V 2 O 5 The performance of the two components widens the photoresponse range of the magnesium oxide, can improve the antibacterial property of the magnesium oxide, and simultaneously has certain influence on the appearance of the material, and the preparation method constructs more magnesium oxides with the same type and novel structureThe multifunctional antibacterial material provides a certain early basis.
Drawings
FIG. 1 is a scanning electron micrograph of pure magnesium oxide and vanadium-magnesium oxide composite;
FIG. 2 is a graph of the effect of varying contents of vanadium-magnesium oxide composite on E.coli;
FIG. 3 is an XPS spectrum of a vanadium-magnesium oxide composite.
Detailed Description
The principles and features of this invention are described below in conjunction with the following drawings, which are set forth to illustrate, but are not to be construed to limit the scope of the invention.
As shown in the figure:
example 1:
a supported rod-shaped magnesium oxide composite antibacterial agent comprises rod-shaped magnesium oxide doped with metal elements; the rod-shaped magnesium oxide is of a magnesium oxide flower stick structure with the surface of which is assembled in a sheet shape; the doped metal element is V.
Example 2:
on the basis of the embodiment 1, the length of the composite antibacterial agent is 5-15 μm, and the diameter is 0.5-1.5 μm.
Example 3:
on the basis of the embodiment 1-2, the preparation method of the load type rod-shaped magnesium oxide composite antibacterial agent comprises the following steps:
s1, measuring a certain amount of 1M MgCl 2 ·6H 2 O, dropwise adding a certain amount of 1M Na under the condition of 50 ℃ water bath 2 CO 3 During which stirring is continued;
s2, waiting for Na 2 CO 3 After the solution is dripped, continuously stirring for 2-4 hours, after the reaction is finished, respectively centrifugally washing the solution for three times by using deionized water and absolute ethyl alcohol, firstly drying the solution in vacuum, and then calcining the solution by using a muffle furnace to obtain rod-shaped magnesium oxide powder;
s3, weighing a certain amount of the rod-shaped magnesium oxide powder obtained in the step S2, adding the rod-shaped magnesium oxide powder into deionized water, and performing ultrasonic dispersion for 4-8min to ensure that the rod-shaped magnesium oxide powder is uniformly dispersed;
s4, dropwise adding the mixture under the water bath condition of 40-80 DEG CAdding NaVO with a certain concentration 3 And (3) after the solution is completely dripped, carrying out ultrasonic treatment for 5-10min, continuously stirring for 3-4 h, respectively carrying out centrifugal washing on deionized water and absolute ethyl alcohol for 2-3 times, carrying out vacuum drying, and then calcining in a muffle furnace to obtain the load type rod-shaped magnesium oxide composite antibacterial agent.
Example 4:
on the basis of examples 1 to 3, in step S1, mgCl 2 ·6H 2 O and Na 2 CO 3 1 is 1.
Example 5:
on the basis of examples 1 to 4, na 2 CO 3 And adding a certain amount of PVP after the addition is finished.
Example 6:
the reaction was carried out at ordinary temperature and pressure based on examples 1 to 5, na 2 CO 3 The dropping speed is 3-4s/d; naVO 3 The dropping speed is 3-4s/d.
Example 7:
on the basis of examples 1 to 6, in step S2, the drying conditions were vacuum drying at 60 ℃; the calcining condition is 600 ℃ and 3 hours; in the step S4, the drying condition is vacuum drying at 60 ℃; the calcination conditions were 600 ℃ for 2 hours.
Example 8:
on the basis of the embodiments 1 to 7, the stirring rotation speeds of the step S1 and the step S4 are consistent and are 200 to 300r/min.
Example 9:
on the basis of examples 1 to 8, the NaVO 3 The concentration of the solution was 1mol/L.
Example 10:
based on examples 1-9, the composite antibacterial agent is used as a bacteriostatic agent for gram-positive bacteria, gram-negative bacteria and molds.
Example 11:
the preparation method of the load type magnesium oxide composite antibacterial material comprises the following specific operations:
(1) 25mL 1M MgCl was measured 2 ·6H 2 O, adding 25mL 1M Na dropwise under the condition of water bath at 50 DEG C 2 CO 3 。
(2) To be Na 2 CO 3 After the solution is dripped, the solution is continuously stirred for 2 hours, after the reaction is finished, deionized water and absolute ethyl alcohol are centrifugally washed for three times, vacuum drying is carried out at the temperature of 60 ℃, and the solution is calcined for 3 hours at the temperature of 600 ℃ in a muffle furnace. Obtaining the rod-shaped magnesium oxide.
(3) Weighing 0.5g of magnesium oxide obtained in the step (2), placing the magnesium oxide in a round-bottom flask, adding the magnesium oxide into 25mL of deionized water, and performing ultrasonic dispersion for 5min to uniformly disperse the magnesium oxide.
(4) Under the condition of 50 ℃ water bath, naVO with different volume fractions (1%, 3%,5%,7%, 9%) is added dropwise 3 After the complete dropwise addition, carrying out ultrasonic treatment for 5min, continuously stirring for 3 hours, carrying out centrifugal washing for 2 times by using deionized water and absolute ethyl alcohol, carrying out vacuum drying at 60 ℃, and calcining for 2 hours at 600 ℃ by using a muffle furnace to obtain the composite antibacterial material.
Example 12:
the preparation method of the load type magnesium oxide composite antibacterial material comprises the following specific operations:
(1) 25mL 1M MgCl was measured 2 ·6H 2 O, adding 25mL 1M Na dropwise under the condition of water bath at 50 DEG C 2 CO 3 And 0.4g of PVP (polyvinylpyrrolidone) was added as a dispersant.
(2) To be Na 2 CO 3 After the solution is dripped, the solution is continuously stirred for 2 hours, after the reaction is finished, deionized water and absolute ethyl alcohol are centrifugally washed for three times, vacuum drying is carried out at the temperature of 60 ℃, and the solution is calcined for 3 hours at the temperature of 600 ℃ in a muffle furnace to obtain the rod-shaped magnesium oxide.
(3) And (3) weighing 0.5g of magnesium oxide obtained in the step (2), placing the magnesium oxide into a round-bottom flask, adding the magnesium oxide into 25mL of deionized water, and ultrasonically dispersing for 5min to uniformly disperse the magnesium oxide.
(4) Under the condition of 50 ℃ water bath, naVO with different volume fractions (1%, 3%,5%,7%, 9%) is added dropwise 3 After complete dripping, carrying out ultrasonic treatment for 5min, continuously stirring for 3 hours, carrying out centrifugal washing for 2 times by using deionized water and absolute ethyl alcohol, carrying out vacuum drying at 60 ℃, and calcining for 2 hours at 600 ℃ by using a muffle furnace to obtain the composite antibacterial material.
Example 13:
the preparation method of the load type magnesium oxide composite antibacterial material comprises the following specific operations:
(1) 25mL of 1M MgCl was measured out 2 ·6H 2 O, adding 25mL of 1M Na dropwise under the condition of water bath at 50 DEG C 2 CO 3 And 0.2g PVP (polyvinylpyrrolidone) was added as a dispersant. PVP is used as a dispersing agent, so that the dispersibility of the raw materials is improved, the reaction is more uniform, and the subsequent NaVO is treated 3 The addition effect of (2) plays a certain promoting role, and according to experiments, when the addition amount of other raw materials is as described in this example, the addition effect of 0.2g PVP is best.
(2) To be Na 2 CO 3 After the solution is dripped, stirring is continuously carried out for 2 hours, after the reaction is finished, deionized water and absolute ethyl alcohol are centrifugally washed for three times, vacuum drying is carried out at the temperature of 60 ℃, and calcining is carried out for 3 hours at the temperature of 600 ℃ by a muffle furnace. Obtaining the rod-shaped magnesium oxide.
(3) And (3) weighing 0.5g of magnesium oxide obtained in the step (2), placing the magnesium oxide into a round-bottom flask, adding the magnesium oxide into 25mL of deionized water, and ultrasonically dispersing for 5min to uniformly disperse the magnesium oxide.
(4) Under the condition of 50 ℃ water bath, naVO with different volume fractions (1%, 3%,5%,7%, 9%) is added dropwise 3 After complete dripping, carrying out ultrasonic treatment for 5min, continuously stirring for 3 hours, carrying out centrifugal washing for 2 times by using deionized water and absolute ethyl alcohol, carrying out vacuum drying at 60 ℃, and calcining for 2 hours at 600 ℃ by using a muffle furnace to obtain the composite antibacterial material.
Example 14:
the preparation method of the load type magnesium oxide composite antibacterial material comprises the following specific operations:
(4) 25mL 1M MgCl was measured 2 ·6H 2 O, adding 25mL of 1M Na dropwise under the condition of water bath at 50 DEG C 2 CO 3 And 0.2g PVP (polyvinylpyrrolidone) was added as a dispersant.
(5) To be Na 2 CO 3 After the solution is dripped, the solution is continuously stirred for 4 hours, after the reaction is finished, deionized water and absolute ethyl alcohol are centrifugally washed for three times, vacuum drying is carried out at the temperature of 60 ℃, and the solution is calcined for 3 hours at the temperature of 600 ℃ in a muffle furnace to obtain the rod-shaped magnesium oxide.
(6) Weighing 0.5g of magnesium oxide obtained in the step (2), placing the magnesium oxide in a round-bottom flask, adding the magnesium oxide into 25mL of deionized water, and performing ultrasonic dispersion for 5min to uniformly disperse the magnesium oxide.
(4) Under the condition of water bath at 40 ℃, naVO with different volume fractions (1%, 3%,5%,7%, 9%) is added dropwise 3 After the complete dropwise addition, carrying out ultrasonic treatment for 5min, continuously stirring for 3 hours, carrying out centrifugal washing for 2 times by using deionized water and absolute ethyl alcohol, carrying out vacuum drying at 60 ℃, and calcining for 2 hours at 600 ℃ by using a muffle furnace to obtain the composite antibacterial material.
Example 15:
the preparation method of the load type magnesium oxide composite antibacterial material comprises the following specific operations:
(7) 25mL 1M MgCl was measured 2 ·6H 2 O, adding 25mL 1M Na dropwise under the condition of water bath at 50 DEG C 2 CO 3 And 0.2g PVP (polyvinylpyrrolidone) was added as a dispersant.
(8) To be Na 2 CO 3 After the solution is dripped, the solution is continuously stirred for 4 hours, after the reaction is finished, deionized water and absolute ethyl alcohol are centrifugally washed for three times, vacuum drying is carried out at the temperature of 60 ℃, and the solution is calcined for 3 hours at the temperature of 600 ℃ in a muffle furnace to obtain the rod-shaped magnesium oxide.
(9) Weighing 0.5g of magnesium oxide obtained in the step (2), placing the magnesium oxide in a round-bottom flask, adding the magnesium oxide into 25mL of deionized water, and performing ultrasonic dispersion for 5min to uniformly disperse the magnesium oxide.
(4) Under the condition of water bath at 80 ℃, naVO with different volume fractions (1%, 3%,5%,7%, 9%) is added dropwise 3 After the complete dropwise addition, carrying out ultrasonic treatment for 5min, continuously stirring for 3 hours, carrying out centrifugal washing for 2 times by using deionized water and absolute ethyl alcohol, carrying out vacuum drying at 60 ℃, and calcining for 2 hours at 600 ℃ by using a muffle furnace to obtain the composite antibacterial material.
Example 16:
the preparation method of the load type magnesium oxide composite antibacterial material comprises the following specific operations:
(1) 25mL 1M MgCl was measured 2 ·6H 2 O, adding 25mL of 1M Na dropwise under the condition of water bath at 50 DEG C 2 CO 3 And 0.2g of PVP (polyvinylpyrrolidone) was added as a dispersant. PVP is used as a dispersing agent, so that the dispersibility of the raw materials is improved, the reaction is more uniform, and the subsequent NaVO is treated 3 Has the addition effectHas certain promoting effect.
(2) To be Na 2 CO 3 After the solution is dripped, the solution is continuously stirred for 2 hours, after the reaction is finished, deionized water and absolute ethyl alcohol are centrifugally washed for three times, vacuum drying is carried out at the temperature of 60 ℃, and the solution is calcined for 3 hours at the temperature of 600 ℃ in a muffle furnace. Obtaining the rod-shaped magnesium oxide.
(3) Weighing 0.5g of magnesium oxide obtained in the step (2), placing the magnesium oxide in a round-bottom flask, adding the magnesium oxide into 25mL of deionized water, and performing ultrasonic dispersion for 5min to uniformly disperse the magnesium oxide.
(4) Under the condition of 50 ℃ water bath, naVO with different volume fractions (1%, 3%,5%,7%, 9%) is added dropwise 3 After complete dripping, carrying out ultrasonic treatment for 5min, continuously stirring for 3 hours, carrying out centrifugal washing for 2 times by using deionized water and absolute ethyl alcohol, carrying out vacuum drying at 60 ℃, and calcining for 2 hours at 600 ℃ by using a muffle furnace to obtain the composite antibacterial material. The influence of different water bath temperatures can influence the load of the V element, and the flaky structure of the rodlike magnesium oxide is most uniform and the shape is optimal under the water bath temperature of 50 ℃.
Example 17:
the preparation method of the load type magnesium oxide composite antibacterial material comprises the following specific operations:
(1) 25mL 1M MgCl was measured 2 ·6H 2 O, adding 30mL 1M Na dropwise under the condition of water bath at 50 DEG C 2 CO 3 And 0.2g PVP (polyvinylpyrrolidone) was added as a dispersant.
(2) To be Na 2 CO 3 After the solution is dripped, the solution is continuously stirred for 2 hours, after the reaction is finished, deionized water and absolute ethyl alcohol are centrifugally washed for three times, vacuum drying is carried out at the temperature of 60 ℃, and the solution is calcined for 3 hours at the temperature of 600 ℃ in a muffle furnace. Obtaining the rod-shaped magnesium oxide.
(3) And (3) weighing 0.5g of magnesium oxide obtained in the step (2), placing the magnesium oxide into a round-bottom flask, adding the magnesium oxide into 25mL of deionized water, and ultrasonically dispersing for 5min to uniformly disperse the magnesium oxide.
(4) Under the condition of water bath at 50 ℃, dropwise adding NaVO3 with different volume fractions (1%, 3%,5%,7%, 9%), after complete dropwise adding, carrying out ultrasonic treatment for 5min, continuously stirring for 3 hours, carrying out centrifugal washing for 2 times by using deionized water and absolute ethyl alcohol, carrying out vacuum drying at 60 ℃ and calcining for 2 hours at 600 ℃ by using a muffle furnace to obtain the composite antibacterial material.
Example 18:
the scanning electron microscope image of the pure magnesium oxide and vanadium-magnesium oxide composite material obtained in example 16 of the present invention is shown in fig. 1, where a is pure magnesium oxide, and b and c are SEM images of the vanadium-doped magnesium oxide composite antibacterial material at different magnifications.
The microscopic morphology of the pure magnesium oxide and the composite material is observed through a scanning electron microscope, and a, b and c are compared to find that the morphology of the rod-shaped magnesium oxide becomes rough and changed after the vanadium element is doped, and the rod-shaped magnesium oxide is changed from a smooth magnesium oxide rod into a magnesium oxide flower rod assembled in a sheet shape. The reason for this change is that vanadium enters into the crystal lattice of magnesium oxide, so that the magnesium oxide nano-rod has a self-assembly process, and the purpose of loading vanadium is achieved.
Example 19:
and (3) antibacterial experiments:
gram-negative bacteria escherichia coli (e.coli, CCTCC 204033) were selected as the test strain for antimicrobial detection. Firstly, preparing an LB agar culture medium (5 g of tryptone, 2.5g of yeast powder, 5g of sodium chloride, 500mL of distilled water and 7.5g of agar) and pouring the agar for later use; preparing LB liquid culture medium (tryptone 5g, yeast powder 2.5g, sodium chloride 5g, distilled water 500 mL), adding the strain into aseptic liquid culture medium with proper content, culturing to obtain bacterial suspension, diluting the bacterial suspension to 5 × 10 with aseptic water 6 CFU/mL. And mixing the sample with the diluted bacterium solution, and placing the mixture into a sterile test tube to prepare suspension. All the test tubes are placed on a shaking table at 37 ℃ and 200rpm for incubation for 15min to ensure that the effect is uniform, then the test tubes are taken out, 100 mu L of upper layer liquid is absorbed and dripped into a culture dish, and the bacterial liquid is uniformly coated on a culture medium by adopting a coating plate method. The culture dish is placed in a constant temperature incubator for 18 to 24 hours. After the culture, the antibacterial rate of each sample is calculated by adopting a colony counting method. The calculation formula is as follows:
example 14:
the addition amount of V element has an influenceIn the experiment, escherichia coli is selected as a research object, and different NaVO are tested by the antibacterial method in example 19 and the preparation method in example 16 3 The antibacterial rate of the composite material with the solution addition amount (1%, 3%,5%,7%, 9%) is 50 mug/mL, the test result is visually expressed by a colony counting method (as shown in the left part of figure 2 and table 1), the right part of figure 2 takes the addition amount as an independent variable (X axis) and the antibacterial rate as a dependent variable (Y axis), a curve of the change of the addition amount to the antibacterial rate is drawn, and the graph shows that the antibacterial rate is in a trend of increasing and then decreasing along with the increase of the vanadium addition amount, and is optimal when the addition amount is 5% -7%. The experiment results show that the addition of the element V has a synergistic improvement effect on the antibacterial effect of the rod-shaped magnesium oxide powder.
TABLE 1 antibacterial ratio of vanadium-magnesium oxide composite material with different contents to Escherichia coli
Example 15:
to verify whether the V element was doped into the magnesium oxide, XPS test was performed on the vanadium-magnesium oxide composite.
FIG. 3a is an XPS full scan spectrum of a vanadium-magnesium oxide composite material, b is an Mg 1s spectrum, c is a V2 p spectrum, and d is an O1s spectrum.
FIG. 3a is an XPS survey of samples from which XPS signature peaks of magnesium, oxygen, and vanadium can be found. To further investigate the presence of Mg, V and O, narrow scans of Mg, V and O elements were performed. As can be seen from FIG. 3b, the spectrum of Mg in the 1s region is 1303.0eV or 1304.2eV. On the other hand, V is at 2p 1/2 And 2p 3/2 The binding energies in the states 524.18eV and 516.93eV determine the presence of vanadium. In the O1s XPS spectrum, there are two characteristic peaks, of which 529.58eV is assigned to the binding energy of lattice oxygen in Mg-O; 531.48eV is the combination of oxygen vacancy structuresCan be used.
The preferred embodiments of the invention disclosed above are intended to be illustrative only. The preferred embodiments are not intended to be exhaustive or to limit the invention to the precise embodiments disclosed. Obviously, many modifications and variations are possible in light of the above teaching. The embodiments were chosen and described in order to best explain the principles of the invention and the practical application, to thereby enable others skilled in the art to best utilize the invention. The invention is limited only by the claims and their full scope and equivalents.
Claims (8)
1. A load type rod-shaped magnesium oxide composite antibacterial agent is characterized in that the composite antibacterial agent comprises rod-shaped magnesium oxide doped with metal elements; the rod-shaped magnesium oxide is of a magnesium oxide flower stick structure with the surface of which is assembled in a sheet shape; the doped metal element is V; the length of the composite antibacterial agent is 5-15 μm, and the diameter is 0.5-1.5 μm;
the preparation method of the load type rod-shaped magnesium oxide composite antibacterial agent comprises the following steps:
s1, measuring a certain amount of 1M MgCl 2 •6H 2 O, adding a certain amount of 1M Na dropwise under the condition of water bath at 50 DEG C 2 CO 3 During which stirring is continued;
s2, waiting for Na 2 CO 3 After the solution is dripped, continuously stirring for 2-4 hours, after the reaction is finished, respectively centrifugally washing the solution for three times by using deionized water and absolute ethyl alcohol, firstly drying the solution in vacuum, and then calcining the solution by using a muffle furnace to obtain rod-shaped magnesium oxide powder;
s3, weighing a certain amount of the rod-shaped magnesium oxide powder obtained in the step S2, adding the rod-shaped magnesium oxide powder into deionized water, and performing ultrasonic dispersion for 4-8min to uniformly disperse the rod-shaped magnesium oxide powder;
s4, dropwise adding NaVO with a certain concentration under the condition of water bath at 40-80 DEG C 3 And (3) after the solution is completely dripped, carrying out ultrasonic treatment for 5-10min, continuously stirring for 3-4 h, respectively carrying out centrifugal washing on deionized water and absolute ethyl alcohol for 2-3 times, carrying out vacuum drying, and then calcining in a muffle furnace to obtain the load type rod-shaped magnesium oxide composite antibacterial agent.
2. The supported rod-shaped magnesium oxide composite antibacterial agent according to claim 1, wherein in step S1, mgCl is added 2 •6H 2 O and Na 2 CO 3 1.
3. The supported rod-like magnesium oxide composite antibacterial agent according to claim 1, wherein in step S1, na is added 2 CO 3 And adding a certain amount of PVP after the addition is finished.
4. The supported rod-like magnesium oxide composite antibacterial agent according to claim 1, wherein the reaction is carried out at normal temperature and pressure, na 2 CO 3 The dropping speed is 3-4s/d; naVO 3 The dropping speed is 3-4s/d.
5. The supported rod-like magnesium oxide composite antibacterial agent according to claim 1, wherein in step S2, the drying conditions are 60 ℃ vacuum drying; the calcining condition is 600 ℃ and 3 hours; in the step S4, the drying condition is vacuum drying at 60 ℃; the calcination conditions were 600 ℃ for 2 hours.
6. The supported rod-shaped magnesium oxide composite antibacterial agent according to claim 1, wherein the rotation speed of the stirring in step S1 and step S4 is in accordance with each other and is 200 to 300r/min.
7. The supported rod-shaped magnesium oxide composite antibacterial agent according to claim 1, wherein said NaVO is 3 The concentration of the solution was 1mol/L.
8. The use of the supported rod-shaped magnesium oxide composite antibacterial agent according to claim 1, wherein the composite antibacterial agent includes but is not limited to the use as a bacteriostatic agent for gram-positive bacteria, gram-negative bacteria and molds.
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| CN1692735A (en) * | 2005-05-20 | 2005-11-09 | 东北大学 | Antibiosis material of low cost, and its prepn. method |
| CN108786785A (en) * | 2017-04-26 | 2018-11-13 | 中国科学院大连化学物理研究所 | Support type Mo-V/MgO-YSZ catalyst |
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| JP3896487B2 (en) * | 2003-04-24 | 2007-03-22 | 独立行政法人物質・材料研究機構 | Method for producing magnesium oxide nanowire and magnesium oxide nanorod |
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| CN105707122B (en) * | 2016-01-25 | 2018-08-28 | 南通中国科学院海洋研究所海洋科学与技术研究发展中心 | A kind of nano composite antibiotic material and its preparation method and application |
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| CN111097383A (en) * | 2019-12-09 | 2020-05-05 | 辽宁科技大学 | V-shaped groove2O5Preparation method and application of coal tar pitch-based composite spherical activated carbon |
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