CN110773109A - Preparation method of boron nitride nanoflower - Google Patents

Preparation method of boron nitride nanoflower Download PDF

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CN110773109A
CN110773109A CN201911057533.2A CN201911057533A CN110773109A CN 110773109 A CN110773109 A CN 110773109A CN 201911057533 A CN201911057533 A CN 201911057533A CN 110773109 A CN110773109 A CN 110773109A
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boron nitride
nanoflower
oxygen
cub
nitric acid
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童东革
李传奇
周瑞
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Chengdu Univeristy of Technology
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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
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
    • B01J20/0262—Compounds of O, S, Se, Te
    • 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
    • A01N59/14—Boron; 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
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
    • B01J20/28002—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their physical properties
    • B01J20/28004—Sorbent size or size distribution, e.g. particle size
    • B01J20/28007—Sorbent size or size distribution, e.g. particle size with size in the range 1-100 nanometers, e.g. nanosized particles, nanofibers, nanotubes, nanowires or the like
    • 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
    • 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
    • B01J2220/00—Aspects relating to sorbent materials
    • B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
    • B01J2220/48—Sorbents characterised by the starting material used for their preparation
    • B01J2220/4806—Sorbents characterised by the starting material used for their preparation the starting material being of inorganic character
    • 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
    • B01J2220/00—Aspects relating to sorbent materials
    • B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
    • B01J2220/48—Sorbents characterised by the starting material used for their preparation
    • B01J2220/4812—Sorbents characterised by the starting material used for their preparation the starting material being of organic character

Abstract

The invention discloses a preparation method of an oxygen-containing boron nitride nanoflower. In the invention, concentrated nitric acid is induced to oxidize CuB in nitroimidazole ionic liquid by a liquid-phase plasma technology 23The nanometer flower is used for successfully preparing the boron nitride containing oxygen nanometer flower at room temperature for the first time. Compared with commercial boron nitride oxide, the boron nitride oxide nanoflower prepared by the invention has larger specific surface area and stronger bacteriostatic effect. Compared with amikacin and kanamycin, the boron nitride oxide prepared by the inventionThe nanoflower shows stronger antibacterial activity against staphylococcus aureus. The excellent antibacterial property of staphylococcus aureus is expected to expand the application of the oxygen-containing boron nitride compound in the clinical medical fields of air purification, sewage disinfection, skin, nasal cavity, throat, intestines and stomach, carbuncle, suppurative sore and the like.

Description

Preparation method of boron nitride nanoflower
Technical Field
The invention relates to the technical field of nano materials, in particular to a preparation method of an oxygen-containing boron nitride nanoflower.
Background
Boron oxynitride is an important electro-sorbent material. With the development of nanotechnology, people find that the morphological structure has a great influence on the performance of the material. But because the preparation of the boron nitride containing oxygen is not easy, the research on the morphological structure effect is not much. For example, only the structure-activity relationship of heavy metal ions adsorbed by oxygen-containing boron nitride nanosheets is reported at present, which severely limits the practical application process.
In conclusion, the research on the synthesis technology of the oxygen-containing boron nitride with a novel morphological structure is very meaningful. At present, no research report of the oxygen-containing boron nitride nanoflower exists. Further, CuB 23Can not react with concentrated nitric acid to generate the oxygen-containing boron nitride compound without the assistance of a liquid phase plasma technology or in a non-ionic liquid medium.
Disclosure of Invention
The invention adopts liquid phase plasma technology to prepare the ionic liquid of nitroimidazole by using CuB 23The nanometer flower is used as a sacrificial template, and the nanometer flower containing the oxygen and the boron nitride is prepared by oxidizing the nanometer flower with concentrated nitric acid at room temperature for the first time, has the average grain diameter of about 100nm and simultaneously has excellent staphylococcus aureus activity.
The invention adopts the following technical scheme:
(1) 2.0 mmol of CuB 23Adding 20-40 ml of nitroimidazole ionic liquid into the nanoflower, mixing, and stirring for 15 minutes;
(2) transferring the mixture obtained in the step (1) into a 200 ml reaction bottle, adding concentrated nitric acid with the mass fraction of 68%, and reacting the nitric acid with CuB 23The molar ratio of the nanoflower is 50-100;
(3) starting liquid phase plasma with the power of 400-800 watts, and treating the mixed solution in the reaction bottle in the step (2) at room temperature for 30-90 minutes to obtain a crude product of the boron nitride nanoflower;
(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 (1), the volume of the nitroimidazole ionic liquid is preferably 30 ml.
In step (2), nitric acid and CuB are preferred 23The molar ratio of the nanoflower is 75.
In the step (3), the power of the liquid phase plasma is preferably 600 watts.
In the step (3), the reaction time is preferably 60 minutes.
The invention has the following positive effects:
1) the invention uses nitroimidazole ionic liquid as a reaction medium and induces concentrated nitric acid to oxidize CuB by liquid-phase plasma technology 23The nanometer flower is used for successfully preparing the boron nitride containing oxygen nanometer flower at room temperature for the first time.
2) Compared with the commercial boron nitride oxide, the specific surface area of the synthesized boron nitride oxide nanoflower is larger.
3) Compared with the boron nitride oxide, the boron nitride oxide nanoflower synthesized by the method has stronger antibacterial activity.
4) Compared with amikacin and kanamycin, the boron nitride containing nanoflower synthesized by the method has stronger antibacterial activity on staphylococcus aureus.
Drawings
Fig. 1 is a TEM photograph of the boron nitride-containing nanoflower prepared in example 1.
Fig. 2 is a selected area electron diffraction photograph of the boron nitride containing nanoflower prepared in example 1.
Fig. 3 is an X-ray diffraction pattern of the boron nitride-containing nanoflower prepared in example 1.
FIG. 4 is a B1sXPS spectrum of the boron nitride containing nanoflower prepared in example 1.
FIG. 5 is an N1sXPS spectrum of the boron nitride containing nanoflower prepared in example 1.
FIG. 6 is an O1sXPS spectrum of the boron nitride containing nanoflower 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) 2.0 mmol of CuB 23Adding 30 ml of nitroimidazole ionic liquid into the nanoflower, mixing, and stirring for 15 minutes;
(2) transferring the mixture obtained in the step (1) into a 200 ml reaction bottle, adding concentrated nitric acid with the mass fraction of 68%, and reacting the nitric acid with CuB 23The molar ratio of the nanoflower is 75;
(3) starting liquid-phase plasma with the power of 600 watts, and treating the mixed solution in the reaction bottle in the step (2) at room temperature for 30 minutes to obtain a crude product of the boron nitride nanoflower;
(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) 2.0 mmol of CuB 23Adding 30 ml of nitroimidazole ionic liquid into the nanoflower, mixing, and stirring for 15 minutes;
(2) transferring the mixture obtained in the step (1) into a 200 ml reaction bottle, adding concentrated nitric acid with the mass fraction of 68%, and reacting the nitric acid with CuB 23The molar ratio of the nanoflower is 75;
(3) starting liquid-phase plasma with the power of 400 watts, and treating the mixed solution in the reaction bottle in the step (2) at room temperature for 30 minutes to obtain a crude product of the boron nitride nanoflower;
(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) 2.0 mmol of CuB 23Adding 30 ml of nitroimidazole ionic liquid into the nanoflower, mixing, and stirring for 15 minutes;
(2) transferring the mixture obtained in the step (1) into a 200 ml reaction bottle, adding concentrated nitric acid with the mass fraction of 68%, and reacting the nitric acid with CuB 23The molar ratio of the nanoflower is 75;
(3) starting liquid-phase plasma with the power of 800 watts, and treating the mixed solution in the reaction bottle in the step (2) at room temperature for 30 minutes to obtain a crude product of the boron nitride nanoflower;
(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 boron nitride containing nano flower 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 nano flowers of boron nitride containing oxygen were successfully prepared, and the average particle size was about 100 nm. The amorphous nature of the prepared boron nitride containing nanoflowers can be confirmed by the halo of the selected area electron diffraction photo (fig. 2).
The ICP-AES analysis test result shows that the atomic composition of the prepared nanometer flower containing the boron nitride oxide is (B) 47.6N 47.6O 4.8). Example 1 the specific surface area of the prepared boron nitride containing nanoflower was 278.2m 2g -1Much larger than commercial boron nitride containing oxygen (20.1 m) 2g -1)。
The phase composition of the samples was analyzed by XRD. As can be seen from the graph, the sample has no obvious diffraction peak, and further shows that the prepared boron nitride containing nano flower is amorphous (figure 3).
The results of XPS spectra (FIGS. 4-6) show that elements such as boron, nitrogen, and oxygen are present on the surface of the prepared samples.
The antibacterial activity of the prepared boron nitride oxide-containing nanoflower was studied (table 1). Determination of the inhibitory concentration by colorimetry (MICs, μ gmL) -1) To determine the antibacterial activity of a sample against staphylococcus aureus (s. aureus), candida albicans (c. albicans), escherichia coli (e.coli), salmonella typhimurium (s. typhimurium) and pseudomonas aeruginosa. For comparison, the antibacterial activity of commercial boron oxynitride, amikacin and kanamycin are also shown.
TABLE 1 antibacterial Activity of the samples
Figure BDA0002256909590000041
The invention uses nitroimidazole ionic liquid as a reaction medium and adopts a liquid-phase plasma technology to induce concentrated nitric acid to oxidize CuB 23The nanometer flower is used to prepare nanometer flower containing oxygen and boron nitride. Compared with commercial boron nitride oxide, the boron nitride oxide nanoflower has stronger antibacterial activity. AntibacterialThe enhancement of activity is attributed to its unique structure and large specific surface area. In addition, the antibacterial activity of boron nitride oxide nanoflowers against staphylococcus aureus was stronger than amikacin and kanamycin. CuB 23The strong bacteriostatic function of the staphylococcus aureus of the nanoflower ensures that the nanoflower is expected to be widely applied to the clinical medical fields of air purification, sewage disinfection, skin, nasal cavity, throat, intestines and stomach, carbuncle, suppurative sore 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 (5)

1. A method for preparing nanometer flower containing oxygen and boron nitride is characterized in that: the preparation method comprises the following specific steps:
(1) 2.0 mmol of CuB 23Adding 20-40 ml of nitroimidazole ionic liquid into the nanoflower, mixing, and stirring for 15 minutes;
(2) transferring the mixture obtained in the step (1) into a 200 ml reaction bottle, adding concentrated nitric acid with the mass fraction of 68%, and reacting the nitric acid with CuB 23The molar ratio of the nanoflower is 50-100;
(3) starting liquid phase plasma with the power of 400-800 watts, and treating the mixed solution in the reaction bottle in the step (2) at room temperature for 30-90 minutes to obtain a crude product of the boron nitride nanoflower;
(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 an oxygen-containing boron nitride nanoflower according to claim 1, wherein: in the step (1), the volume of the nitroimidazole ionic liquid is 30 ml.
3. The method for preparing an oxygen-containing boron nitride nanoflower according to claim 1, wherein: in the step (2), nitric acid and CuB 23The molar ratio of the nanoflower is 75.
4. The method for preparing an oxygen-containing boron nitride nanoflower according to claim 1, wherein: in the step (3), the power of the liquid phase plasma is 600 watts.
5. The method for preparing an oxygen-containing boron nitride nanoflower according to claim 1, wherein: in the step (3), the reaction time was 60 minutes.
CN201911057533.2A 2019-11-01 2019-11-01 Preparation method of boron nitride nanoflower Pending CN110773109A (en)

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