CN110759349A - Porous CuB23Preparation method of (1) - Google Patents

Porous CuB23Preparation method of (1) Download PDF

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CN110759349A
CN110759349A CN201911041561.5A CN201911041561A CN110759349A CN 110759349 A CN110759349 A CN 110759349A CN 201911041561 A CN201911041561 A CN 201911041561A CN 110759349 A CN110759349 A CN 110759349A
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cub
porous
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copper sulfate
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童东革
傅仕艳
周瑞
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Chengdu Univeristy of Technology
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    • 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
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    • B—PERFORMING OPERATIONS; TRANSPORTING
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    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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    • C01P2006/12—Surface area
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    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/16—Pore diameter

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Abstract

The invention discloses a porous CuB23The preparation method of (1). The invention successfully prepares the porous CuB in the 1-butyl-3-methylimidazole triflate ionic liquid at room temperature by the liquid phase plasma technology23. With commercial CuB23Compared with the porous CuB prepared by the invention23The specific surface area is larger, and the bacteriostatic effect is stronger. Compared with amikacin and kanamycin, the porous CuB prepared by the invention23Has stronger antibacterial activity to pseudomonas aeruginosa. The excellent bacteriostatic property of pseudomonas aeruginosa is expected to expand CuB23The compound can be used in medical equipment coating, skin and subcutaneous tissue infection, otitis media, meningitis, and respiratory tract infectionThe application in the fields of infection, urinary tract infection, septicemia and the like.

Description

Porous CuB23Preparation method of (1)
Technical Field
The invention relates to the technical field of nano materials, in particular to a porous CuB23The preparation method of (1).
Background
CuB23Not only is an important catalyst, but also is an important gas-sensitive sensing material. With the development of science and technology, people find that the performance of materials is closely related to the shape and structure of the materials. But due to CuB23The synthesis of (A) is more challenging, with respect to CuB at present23Construct and imitate to closeThe research is not much. For example, only CuB has been studied23The structure-activity relationship of nano particles, nano sheets and the like greatly hinders the development and commercialization process of the application of the nano particles.
Therefore, the novel morphology structure CuB23The research on the preparation method of (2) is very meaningful. Currently, people have not synthesized CuB with porous morphology structure23. Recently, a liquid phase plasma technology using ionic liquid as a reaction medium is developed to synthesize metal boride nano-materials such as europium hexaboride and ytterbium hexaboride.
Disclosure of Invention
The invention synthesizes porous CuB by reducing copper sulfate with hydrazine borane at room temperature for the first time in 1-butyl-3-methylimidazole trifluoromethanesulfonate ionic liquid by using dioctyl sodium sulfosuccinate as a surfactant through a liquid phase plasma technology23The average pore diameter is about 50nm, and the pseudomonas aeruginosa activity is better.
The invention adopts the following technical scheme:
(1) mixing 2.4 mmol of copper sulfate and a proper amount of dioctyl sodium sulfosuccinate in 30 ml of 1-butyl-3-methylimidazole trifluoromethanesulfonate ionic liquid, and stirring for 10 minutes to form a solution, wherein the molar ratio of the copper sulfate to the dioctyl sodium sulfosuccinate is 5-10: 1;
(2) transferring the mixed solution obtained in the step (1) into a 100 ml reaction bottle, and adding hydrazine borane to ensure that the molar ratio of the hydrazine borane to the copper sulfate is 25-35;
(3) starting liquid phase plasma with the power of 100-23A crude product;
(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 preferred molar ratio of copper sulfate to sodium dioctyl sulfosuccinate is 8: 1.
In the step (2), the molar ratio of hydrazine borane to copper sulfate is preferably 30.
In the step (3), the power of the liquid phase plasma is preferably 300 watts.
In the step (3), the reaction time is preferably 30 minutes.
The invention has the following positive effects:
1) the invention successfully synthesizes the porous CuB at room temperature for the first time by using a liquid phase plasma technology and 1-butyl-3-methylimidazole triflate ionic liquid as a reaction medium23。
2) Commercial CuB23In contrast, the porous CuB synthesized by the present invention23Is larger than the specific surface area of (a).
3) With commercial CuB23In contrast, the porous CuB synthesized by the present invention23Shows stronger antibacterial activity.
4) Compared with amikacin and kanamycin, the porous CuB synthesized by the method23Has stronger antibacterial activity to the activity of pseudomonas aeruginosa.
Drawings
FIG. 1 is a porous CuB prepared in example 123TEM photograph of (a).
FIG. 2 is porous CuB prepared in example 123The selected area electron diffraction photograph of (1).
FIG. 3 is porous CuB prepared in example 123X-ray diffraction pattern of (a).
FIG. 4 is porous CuB prepared in example 123Cu2p3/2XPS spectra.
FIG. 5 is porous CuB prepared in example 123B1 xps spectrum of (a).
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) Mixing 2.4 mmol of copper sulfate and 0.3 mmol of sodium dioctyl sulfosuccinate in 30 ml of 1-butyl-3-methylimidazolium trifluoromethanesulfonate ionic liquid, and stirring for 10 minutes to form a solution;
(2) transferring the mixed solution obtained in the step (1) into a 100 ml reaction bottle, and adding hydrazine borane to ensure that the molar ratio of the hydrazine borane to the copper sulfate is 30;
(3) starting liquid phase plasma with the power of 300 watts, and treating the mixed solution in the reaction bottle in the step (2) at room temperature for 30 minutes to obtain porous CuB23A crude product;
(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) Mixing 2.4 mmol of copper sulfate and 0.3 mmol of sodium dioctyl sulfosuccinate in 30 ml of 1-butyl-3-methylimidazolium trifluoromethanesulfonate ionic liquid, and stirring for 10 minutes to form a solution;
(2) transferring the mixed solution obtained in the step (1) into a 100 ml reaction bottle, and adding hydrazine borane to ensure that the molar ratio of the hydrazine borane to the copper sulfate is 30;
(3) starting liquid phase plasma with the power of 300 watts, and treating the mixed solution in the reaction bottle in the step (2) at room temperature for 20 minutes to obtain porous CuB23A crude product;
(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) Mixing 2.4 mmol of copper sulfate and 0.3 mmol of sodium dioctyl sulfosuccinate in 30 ml of 1-butyl-3-methylimidazolium trifluoromethanesulfonate ionic liquid, and stirring for 10 minutes to form a solution;
(2) transferring the mixed solution obtained in the step (1) into a 100 ml reaction bottle, and adding hydrazine borane to ensure that the molar ratio of the hydrazine borane to the copper sulfate is 30;
(3) starting liquid phase plasma with the power of 300 watts, and treating the mixed solution in the reaction bottle in the step (2) at room temperature for 40 minutes to obtain porous CuB23A crude product;
(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.
Porous CuB of the invention23The performance of (A):
the sample prepared in example 1 was characterized by TEM, and fig. 1 is a TEM image of the sample. As can be seen in FIG. 1, porous CuB23Has been successfully prepared, and has an average particle size of about 50 nm. The prepared porous CuB23The amorphous nature of (2) can be confirmed from the halo of the selected area electron diffraction photograph (fig. 2).
The ICP-AES analysis test result shows that the prepared porous CuB23With commercial CuB23Has the same atomic composition (Cu)4.17B95.83). Example 1 porous CuB prepared23Has a specific surface area of 300.3m2g-1Much larger than commercial CuB23(5.5m2g-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 illustrates the prepared porous CuB23Is amorphous (fig. 3).
The results of XPS spectra (FIGS. 4 and 5) show that porous CuB was prepared23The surface of the nano material, Cu and B exist in an element state.
For the prepared porous CuB23The antibacterial activity of (2) was investigated (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, commercial CuB23The antibacterial activity of amikacin and kanamycin is also shown.
TABLE 1 antibacterial Activity of the samples
Figure BDA0002252977100000041
The invention successfully prepares the porous CuB by using 1-butyl-3-methylimidazole triflate ionic liquid as a reaction medium and adopting a liquid phase plasma technology23. With commercial CuB23In contrast, porous CuB23Has stronger antibacterial activity. Enhancement of antibacterial activityDue to its large specific surface area. Further, porous CuB23The antibacterial activity to pseudomonas aeruginosa is stronger than amikacin and kanamycin. CuB23The strong bacteriostatic function of the nano-flowers of the pseudomonas aeruginosa enables the pseudomonas aeruginosa to be expected to be widely applied to the fields of medical instrument coatings, skin and subcutaneous tissue infection, otitis media, meningitis, respiratory tract infection, urinary 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 (5)

1. Porous CuB23The preparation method is characterized by comprising the following steps: the preparation method comprises the following specific steps:
(1) mixing 2.4 mmol of copper sulfate and a proper amount of dioctyl sodium sulfosuccinate in 30 ml of 1-butyl-3-methylimidazole trifluoromethanesulfonate ionic liquid, and stirring for 10 minutes to form a solution, wherein the molar ratio of the copper sulfate to the dioctyl sodium sulfosuccinate is 5-10: 1;
(2) transferring the mixed solution obtained in the step (1) into a 100 ml reaction bottle, and adding hydrazine borane to ensure that the molar ratio of the hydrazine borane to the copper sulfate is 25-35;
(3) starting liquid phase plasma with the power of 100-23A crude product;
(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 porous CuB of claim 123The preparation method is characterized by comprising the following steps: in the step (1), the molar ratio of copper sulfate to dioctyl sodium sulfosuccinate is 8: 1.
3. The porous CuB of claim 123Preparation method ofThe method is characterized in that: in the step (2), the molar ratio of hydrazine borane to copper sulfate is 30.
4. The porous CuB of claim 123The preparation method is characterized by comprising the following steps: in the step (3), the power of the liquid phase plasma is 300 watts.
5. The porous CuB of claim 123The preparation method is characterized by comprising the following steps: in the step (3), the reaction time was 30 minutes.
CN201911041561.5A 2019-10-30 2019-10-30 Porous CuB23Preparation method of (1) Pending CN110759349A (en)

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104561840A (en) * 2014-12-23 2015-04-29 成都理工大学 Method for simply preparing amorphous alloy CuB23 nano short tube and application thereof
CN108862299A (en) * 2018-08-08 2018-11-23 成都理工大学 A kind of amorphous state EuB6The preparation method of nano material
CN110092388A (en) * 2019-05-15 2019-08-06 成都理工大学 A kind of preparation method of six ytterbium borides alloy nano particle

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104561840A (en) * 2014-12-23 2015-04-29 成都理工大学 Method for simply preparing amorphous alloy CuB23 nano short tube and application thereof
CN108862299A (en) * 2018-08-08 2018-11-23 成都理工大学 A kind of amorphous state EuB6The preparation method of nano material
CN110092388A (en) * 2019-05-15 2019-08-06 成都理工大学 A kind of preparation method of six ytterbium borides alloy nano particle

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
FAN YANG ET AL: "Monodisperse amorphous CuB23 alloy short nanotubes: novel efficient catalysts for Heck coupling of inactivated alkyl halides and alkenes", 《RSC ADVANCES》 *
杨帆: "一维非晶态Co-B-N-H和CuB23催化剂的制备及其性能研究", 《中国优秀博硕士学位论文全文数据库（硕士）工程科技I辑》 *

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Application publication date: 20200207