CN110844917A - Preparation method of magnesium boride nanoparticles - Google Patents

Preparation method of magnesium boride nanoparticles Download PDF

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Publication number
CN110844917A
CN110844917A CN201911226603.2A CN201911226603A CN110844917A CN 110844917 A CN110844917 A CN 110844917A CN 201911226603 A CN201911226603 A CN 201911226603A CN 110844917 A CN110844917 A CN 110844917A
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magnesium boride
mgcl
borane
infection
product
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童东革
向桓冬
周瑞
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Chengdu Univeristy of Technology
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Chengdu Univeristy of Technology
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B35/00—Boron; Compounds thereof
    • C01B35/02—Boron; Borides
    • C01B35/04—Metal borides
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K33/00—Medicinal preparations containing inorganic active ingredients
    • A61K33/22—Boron compounds
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
    • A61P31/00—Antiinfectives, i.e. antibiotics, antiseptics, chemotherapeutics
    • A61P31/04—Antibacterial agents
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00—Manufacture or treatment of nanostructures
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
    • C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/01—Particle morphology depicted by an image
    • C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size
    • C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer

Abstract

The invention discloses a preparation method of magnesium boride nanoparticles. MgCl is reduced by borane in triethylphenylammonium bis (trifluoromethanesulfonyl) imide ionic liquid at room temperature through a liquid phase plasma technology2Synthesizing the magnesium boride nano particles. Compared with commercial magnesium boride, the magnesium boride nano particle prepared by the invention has larger specific surface area and stronger bacteriostatic effect. Compared with amikacin and wittigmine sulfate, the magnesium boride nano-particle prepared by the invention has stronger antibacterial activity on enterobacter cloacae. The excellent antibacterial property of the enterobacter cloacae is expected to expand bacterial infectious diseases of hospital infection, such as skin soft tissue infection, urinary tract infection, respiratory tract infectionIs widely applied in the field of clinical treatment of infection, septicemia and the like.

Description

Preparation method of magnesium boride nanoparticles
Technical Field
The invention relates to a method for preparing magnesium boride nano particles, belonging to the technical field of advanced nano material preparation.
Background
Magnesium boride is a superconducting material, and is generally prepared by a high-temperature sintering method, which is not only energy-consuming, but also time-consuming. Therefore, it is very necessary to develop a new green synthesis method or a new technical approach for preparing magnesium boride.
At present, liquid plasma process (SPP) has become an effective way to synthesize metal borides. The metal borides synthesized by SPP technology that have been reported so far are: nickel-boron, cobalt-boron, europium-boron and ytterbium-boron.
Disclosure of Invention
The invention reduces MgCl by borane in triethylphenylammonium bis (trifluoromethanesulfonyl) imide ionic liquid at room temperature for the first time through a liquid phase plasma technology2As conditional pathogenic bacteria, with the wide use of cephalosporins, enterobacter cloacae becomes pathogenic bacteria which are more and more important for hospital infection, bacterial infectious diseases caused by the pathogenic bacteria often involve multiple organ systems, including skin soft tissue infection, urinary tract infection, respiratory tract infection, septicemia and the like.
The invention adopts the following technical scheme:
MgCl of the invention2The preparation method of the nano particles comprises the following specific steps:
(1) 4mmol of MgCl2Adding 20mL of triethylphenylammonium bis (trifluoromethanesulfonyl) imide ionic liquid, and stirring for 20 minutes under the protection of argon to form a solution;
(2) transferring the mixed solution obtained in the step (1) into a 50mL reaction kettle under the protection of argon, introducing borane, and enabling the borane and MgCl to be mixed2The molar ratio of (1) to (3-6), and sealing the reaction kettle;
(3) starting liquid phase plasma with the power of 400-;
(4) washing the product with deionized water for three times, then washing the product with absolute ethyl alcohol for three times, and drying the product for later use.
In step (2), the borane and MgCl are preferably carried out under argon protection2Introducing borane into the mixed liquid in the step (1) at a molar ratio of 4.5:1, and sealing the reaction kettle.
In the step (3), the power of the liquid phase plasma is preferably 500W.
In the step (3), the reaction time is preferably 30 min.
The invention has the following positive effects:
1) the invention successfully synthesizes the magnesium boride nano-particles at room temperature for the first time by adopting the SPP technology.
2) Compared with commercial magnesium boride, the magnesium boride nano particle synthesized by the method has larger specific surface area.
3) Compared with commercial magnesium boride, the synthesized magnesium boride nano particle shows stronger antibacterial activity.
4) Compared with amikacin and wittigmine sulfate, the synthesized magnesium boride nano-particles have stronger antibacterial activity on enterobacter cloacae.
Drawings
FIG. 1 is a TEM photograph of magnesium boride nanoparticles prepared in example 1.
FIG. 2 is an X-ray diffraction pattern of magnesium boride nanoparticles prepared in example 1.
Detailed Description
The following examples are further detailed descriptions of the present invention.
The experimental procedures used in the following examples are all conventional procedures unless otherwise specified.
Materials, reagents and the like used in the following examples are commercially available unless otherwise specified.
Example 1
(1) 4mmol of MgCl2Adding 20mL of triethylphenylammonium bis (trifluoromethanesulfonyl) imide ionic liquid, and stirring for 20 minutes under the protection of argon to form a solution;
(2) transferring the mixed solution obtained in the step (1) into a 50mL reaction kettle under the protection of argon, introducing borane, and enabling the borane and MgCl to be mixed2The molar ratio of (3) to (4.5: 1), and sealing the reaction kettle;
(3) starting liquid-phase plasma with the power of 500W, and treating the mixed solution in the reaction kettle in the step (2) at room temperature for 30min to obtain a crude product of magnesium boride nanoparticles;
(4) washing the product with deionized water for three times, then washing the product with absolute ethyl alcohol for three times, and drying the product for later use.
Example 2
(1) 4mmol of MgCl2Adding 20mL of triethylphenylammonium bis (trifluoromethanesulfonyl) imide ionic liquid, and stirring for 20 minutes under the protection of argon to form a solution;
(2) transferring the mixed solution obtained in the step (1) into a 50mL reaction kettle under the protection of argon, introducing borane, and enabling the borane and MgCl to be mixed2The molar ratio of (3) to (4.5: 1), and sealing the reaction kettle;
(3) starting liquid-phase plasma with the power of 600W, and treating the mixed solution in the reaction kettle in the step (2) at room temperature for 30min to obtain a crude product of magnesium boride nanoparticles;
(4) washing the product with deionized water for three times, then washing the product with absolute ethyl alcohol for three times, and drying the product for later use.
Example 3
(1) 4mmol of MgCl2Adding 20mL of triethylphenylammonium bis (trifluoromethanesulfonyl) imide ionic liquid, and stirring for 20 minutes under the protection of argon to form a solution;
(2) transferring the mixed solution obtained in the step (1) into a 50mL reaction kettle under the protection of argon, introducing borane, and enabling the borane and MgCl to be mixed2The molar ratio of (3) to (4.5: 1), and sealing the reaction kettle;
(3) starting liquid-phase plasma with the power of 400W, and treating the mixed solution in the reaction kettle in the step (2) at room temperature for 30min to obtain a crude product of magnesium boride nanoparticles;
(4) washing the product with deionized water for three times, then washing the product with absolute ethyl alcohol for three times, and drying the product for later use.
The properties of the magnesium boride nanoparticles of the invention are as follows:
the sample prepared in example 1 was characterized by TEM, and fig. 1 is a TEM image of the sample. As can be seen from FIG. 1, the average particle size of the sample was about 8 nm.
The phase composition of the samples was analyzed by XRD. As can be seen from the spectrum (FIG. 2), the positions of the diffraction peaks of the sample are consistent with the standard spectrum (JCPDF-74-0982).
The ICP-AES analysis and test result shows that the prepared magnesium boride nano particles have the same element mass percentage composition with the commercial magnesium boride (Mg: 52.93; B: 47.07). Example 1 the specific surface area of the prepared magnesium boride nanoparticles is 112.3m2g-1Much larger than commercial magnesium boride (8.5 m)2g-1)。
The antibacterial activity of the prepared magnesium boride nanoparticles was studied (table 1). Determination of the inhibitory concentration by colorimetry (MICs, μ gmL)-1) To determine the antibacterial activity of a sample against methicillin-susceptible staphylococcus aureus (s.aureus), staphylococcus epidermidis (s.epidermidis), enterobacter cloacae (e.cloacae), proteus mirabilis (p.mirabilis) and enterobacter aerogenes (e.aerogenes). For comparison, the antibacterial activity of commercial magnesium boride, amikacin and venemicin sulfate are also listed.
TABLE 1 antibacterial Activity of the samples
Figure BDA0002302404600000041
The invention adopts liquid phase plasma technology to successfully prepare the magnesium boride nano-particles. Compared with commercial magnesium boride, the magnesium boride nanoparticles have stronger antibacterial activity. The enhancement of antibacterial activity is attributed to its large specific surface area. In addition, the antibacterial activity of magnesium boride nanoparticles against enterobacter cloacae was stronger than that of amikacin and venemicin sulfate. The magnesium boride nano-particle has strong bacterium inhibition function of enterobacter cloacae, so that the magnesium boride nano-particle is expected to be widely applied to the clinical treatment fields of nosocomial infectious bacterial diseases, such as skin soft tissue infection, urinary tract infection, respiratory tract infection, septicemia and the like.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.

Claims (4)

1. A preparation method of magnesium boride nano particles is characterized by comprising the following steps: the preparation method comprises the following specific steps:
(1) 4mmol of MgCl2Adding 20mL of triethylphenylammonium bis (trifluoromethanesulfonyl) imide ionic liquid, and stirring for 20 minutes under the protection of argon to form a solution;
(2) transferring the mixed solution obtained in the step (1) into a 50mL reaction kettle under the protection of argon, introducing borane, and enabling the borane and MgCl to be mixed2The molar ratio of (1) to (3-6), and sealing the reaction kettle;
(3) starting liquid phase plasma with the power of 400-;
(4) washing the product with deionized water for three times, then washing the product with absolute ethyl alcohol for three times, and drying the product for later use.
2. The method for preparing magnesium boride nanoparticles according to claim 1, characterized in that: in the step (2), the borane and MgCl are introduced2Is 4.5: 1.
3. The method for preparing magnesium boride nanoparticles according to claim 1, characterized in that: in the step (3), the power of the liquid phase plasma is 500W.
4. The method for preparing magnesium boride nanoparticles according to claim 1, characterized in that: in the step (3), the reaction time is 30 min.
CN201911226603.2A 2019-12-04 2019-12-04 Preparation method of magnesium boride nanoparticles Pending CN110844917A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114735714A (en) * 2021-12-03 2022-07-12 上海市第十人民医院 Mg1-xRxB2Preparation method and application of material

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2005129412A (en) * 2003-10-24 2005-05-19 National Institute For Materials Science MgB2 SUPERCONDUCTIVE WIRE ROD AND ITS MANUFACTURING METHOD
CN102585809A (en) * 2012-01-18 2012-07-18 浙江工业大学 Preparation method of flower-structure magnesium borate microsphere europium-doped red fluorescent powder
KR20140065240A (en) * 2012-11-21 2014-05-29 대구가톨릭대학교산학협력단 Composite scaffold having excellent osteogenesis and its manufacturing method
CN104371394A (en) * 2014-12-10 2015-02-25 竺叶洪 Wearproof composite antibacterial coating material and preparation method and application thereof
CN109665537A (en) * 2019-02-22 2019-04-23 成都理工大学 A kind of low temperature preparation EuB6The method of nanocube crystal
CN110002459A (en) * 2019-04-12 2019-07-12 成都理工大学 A kind of preparation method for mixing nickel europium boride

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2005129412A (en) * 2003-10-24 2005-05-19 National Institute For Materials Science MgB2 SUPERCONDUCTIVE WIRE ROD AND ITS MANUFACTURING METHOD
CN102585809A (en) * 2012-01-18 2012-07-18 浙江工业大学 Preparation method of flower-structure magnesium borate microsphere europium-doped red fluorescent powder
KR20140065240A (en) * 2012-11-21 2014-05-29 대구가톨릭대학교산학협력단 Composite scaffold having excellent osteogenesis and its manufacturing method
CN104371394A (en) * 2014-12-10 2015-02-25 竺叶洪 Wearproof composite antibacterial coating material and preparation method and application thereof
CN109665537A (en) * 2019-02-22 2019-04-23 成都理工大学 A kind of low temperature preparation EuB6The method of nanocube crystal
CN110002459A (en) * 2019-04-12 2019-07-12 成都理工大学 A kind of preparation method for mixing nickel europium boride

Non-Patent Citations (3)

* Cited by examiner, † Cited by third party
Title
PIEKOSZEWSKI,J; ET AL.: "Ion implantation and transient melting：A new approach to formation of superconducting MgB2 phases", 《ACTA PHYSICA POLONICA A》 *
向桓冬等: "Ni-P微纳米材料的设计、合成及对水合肼的电催化氧化", 《2019年第四届全国新能源与化工新材料学术会议暨全国能量转换与存储材料学术研讨会摘要集》 *
李锦: "碱土金属硼酸盐掺Eu3+纳米材料的制备、表征及其性能的研究", 《中国优秀硕士学位论文全文数据库 工程科技I辑》 *

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114735714A (en) * 2021-12-03 2022-07-12 上海市第十人民医院 Mg1-xRxB2Preparation method and application of material
CN114735714B (en) * 2021-12-03 2023-08-22 上海市第十人民医院 Mg 1-x R x B 2 Preparation method and application of material

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Application publication date: 20200228