CN107243642B - The method for preparing antimony alkene using ionic liquid auxiliary - Google Patents

The method for preparing antimony alkene using ionic liquid auxiliary Download PDF

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Publication number
CN107243642B
CN107243642B CN201710470088.7A CN201710470088A CN107243642B CN 107243642 B CN107243642 B CN 107243642B CN 201710470088 A CN201710470088 A CN 201710470088A CN 107243642 B CN107243642 B CN 107243642B
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antimony
alkene
ionic liquid
antimony alkene
sample
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CN107243642A (en
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赵敏
王志元
曹海亮
张华�
郭俊杰
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Taiyuan University of Technology
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Taiyuan University of Technology
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00Making metallic powder or suspensions thereof
    • B22F9/02Making metallic powder or suspensions thereof using physical processes
    • B22F9/04Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00Manufacture or treatment of nanostructures

Abstract

The present invention relates to a kind of methods for preparing antimony alkene using -3 methylimidazole trifluoroacetate liquid phase auxiliary of 1- ethyl, belong to novel inorganic two-dimensional material preparation field.The method that the present invention utilizes simple ionic liquid liquid phase up-stripping, antimony powder is removed to have obtained few layer of antimony alkene.Preparation method of the invention has simple to operation, and the antimony alkene being prepared has the characteristics that quality is high, concentration is big, and the ionic liquid utilized have many advantages, such as it is environmentally protective, it is recyclable to reuse.

Description

The method for preparing antimony alkene using ionic liquid auxiliary
Technical field
The present invention relates to the preparation fields of New Two Dimensional material, specifically use the method for ionic liquid liquid phase up-stripping Prepare the New Two Dimensional antimony alkene of high concentration.
Background technique
In recent years, the appearance of grapheme two-dimension material has caused a series of scientific and technological revolution.It is some special that graphene has Physicochemical property and photoelectric characteristic, such as high conductivity, high-termal conductivity, high intensity and high light transmittance etc..With graphene Development, has also expedited the emergence of out a series of novel class grapheme two-dimension material, as transient metal sulfide, boron alkene, silene, two dimension are black Phosphorus etc., this greatly enriches the diversity of two-dimensional material, complementary some defects of graphene.But to large-scale application These two-dimensional materials, there is also lot of challenges, wherein high yield prepares height how within the scope of acceptable preparation cost The two-dimensional material of quality is undoubtedly the difficulty to overcome first.
Summary of the invention
Based on the above-mentioned prior art, the object of the present invention is to provide a kind of method systems using ionic liquid liquid phase up-stripping The method of the New Two Dimensional material antimony alkene of standby high concentration.Using the electrostatic interaction and Π-Π key on ionic liquid and antimony surface act on come Realize being effectively peeled off for antimony.
The present invention is achieved by the following technical scheme:
A method of antimony alkene being prepared using ionic liquid auxiliary, using ionic liquid liquid phase up-stripping antimony alkene:
A certain amount of antimony powder end is ground in the agate mortar, then takes appropriate ion liquid solvent, by the antimony after grinding Powder is placed in the antimony solution that saturation is made in ion liquid solvent, carries out ultrasonic removing to above-mentioned solution, ultrasonic time 4-7h surpasses Acoustical power is 500-700W, obtains the antimony alkene sample that concentration is 0.9 ± 0.2 g/L;The ion liquid solvent is 1- ethyl -3 Methylimidazole trifluoroacetate.
The invention proposes utilize -3 methylimidazole trifluoroacetate liquid phase up-stripping antimony alkene of ionic liquid 1- ethyl Method, antimony alkene concentration with higher (0.9 ± 0.2g/L) obtained, the features such as high quality and pattern are uniform;Utilize this method Obtained antimony alkene is better than existing report with a thickness of 1 ~ 3nm, and ion liquid solvent of the present invention have green, The advantages that environmental protection, higher boiling, high conductivity, antimony alkene material prepared by this method due to a certain amount of ionic liquid of adsorption, There is good application prospect in fields such as energy stores, solar battery, field effect transistor, nonlinear opticses.
Detailed description of the invention
Fig. 1 shows the ultraviolet-visible absorption spectroscopies of antimony alkene of the present invention.
Fig. 2 indicates the TEM figure of antimony alkene of the present invention.
Specific embodiment
A specific embodiment of the invention is further illustrated below.
A method of antimony alkene being prepared using ionic liquid auxiliary, is included the following steps:
(1) ionic liquid liquid phase up-stripping antimony alkene:
A certain amount of antimony powder end is ground in the agate mortar, then takes appropriate ion liquid solvent, by the antimony after grinding Powder is placed in the antimony solution that saturation is made in ion liquid solvent, carries out ultrasonic removing to above-mentioned solution, ultrasonic time 4-7h surpasses Acoustical power is 500-700W, obtains the antimony alkene sample that concentration is 0.9 ± 0.2g/L;The ion liquid solvent is -3 first of 1- ethyl Base imidazoles trifluoroacetate.
(2) characterization of sample:
Sample is centrifuged first, precipitating solvent is cleaned, to carry out ultraviolet-visible absorption spectroscopy and TEM to sample Characterization, the concentration of antimony alkene are 0.9 ± 0.2 g/L.
Attached drawing 1 is the ultraviolet-visible absorption spectroscopy that antimony alkene is prepared.The concentration of antimony alkene has been estimated using ultraviolet absorption method, Its concentration is 0.9 ± 0.2 g/L.Attached drawing 2 is that the TEM of antimony alkene schemes.
Based on above-mentioned test result, it can be seen that method of the invention can using the method for ionic liquid liquid phase up-stripping To prepare the antimony alkene of high concentration, high quality.In short, the present invention is prepared for antimony alkene using the method that simple liquid phase is removed, this The preparation method of invention has the features such as simple to operation, the antimony alkene quality being prepared is high, and concentration is high, and ionic liquid is with green The advantages that colour circle is protected, and recycling can be recycled.
Above embodiment is merely to illustrate the contents of the present invention, but this is not a limitation of the present invention, this field Related technical personnel can also make corresponding adjustment and modification, therefore all without departing from the scope of the invention The technical solution that the mode of equivalent replacement or equivalent variations is formed all belongs to the scope of protection of the present invention.

Claims (2)

1. a kind of method for preparing antimony alkene using ionic liquid auxiliary, which is characterized in that use ionic liquid liquid phase up-stripping antimony Alkene:
A certain amount of antimony powder end is ground in the agate mortar, then takes appropriate ion liquid solvent, by the antimony powder end after grinding It is placed in the antimony solution that saturation is made in ion liquid solvent, ultrasonic removing, ultrasonic time 4-7h, ultrasonic function are carried out to above-mentioned solution Rate is 500-700W, obtains the antimony alkene sample that concentration is 0.9 ± 0.2g/L;The ion liquid solvent is -3 methyl miaow of 1- ethyl Azoles trifluoroacetate.
2. the method according to claim 1 for preparing antimony alkene using ionic liquid auxiliary, it is characterised in that: to antimony alkene obtained Sample is characterized: antimony alkene sample being centrifuged half an hour first, precipitating solvent is cleaned, then carries out UV, visible light to sample The characterization of absorption spectrum and transmission electron microscope.
CN201710470088.7A 2017-06-20 2017-06-20 The method for preparing antimony alkene using ionic liquid auxiliary Active CN107243642B (en)

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CN107243642B true CN107243642B (en) 2019-02-22

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Publication number Priority date Publication date Assignee Title
CN108237229B (en) * 2018-01-17 2021-02-19 深圳大学 Two-dimensional stibene with adjustable layer number and preparation method thereof
CN108574045B (en) * 2018-05-07 2021-10-26 太原理工大学 Organic photovoltaic cell with high photoelectric conversion efficiency
CN108588826A (en) * 2018-05-15 2018-09-28 中国工程物理研究院化工材料研究所 The liquid phase stripping means of antimony alkene, bismuth alkene based on ion insertion auxiliary
CN109648095B (en) * 2018-12-13 2021-12-14 兰州大学 Antimony nanosheet and stripping method thereof, and flexible photodetector and preparation method thereof
CN112320761A (en) * 2020-11-19 2021-02-05 太原理工大学 Preparation method of iodoene with controllable layer number
CN114433852B (en) * 2022-03-14 2023-05-19 清华大学 Method for preparing antimoney nanosheets by electrochemical stripping

Citations (5)

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CN101037388A (en) * 2007-04-17 2007-09-19 华东师范大学 Multifunctional ion liquid system, preparation and application thereof
WO2007105443A1 (en) * 2006-02-27 2007-09-20 National University Corporation Nagoya University Method for producing nanoparticle
CN101137437A (en) * 2005-01-04 2008-03-05 贝尔法斯特女王大学 Basic ionic liquids
CN105297133A (en) * 2015-10-28 2016-02-03 南京理工大学 Preparation method of single-crystal less-layer antimonene
CN106191999A (en) * 2016-09-19 2016-12-07 中国科学院物理研究所 A kind of antimony alkene two-dimensional atomic crystal material and preparation method thereof

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101137437A (en) * 2005-01-04 2008-03-05 贝尔法斯特女王大学 Basic ionic liquids
WO2007105443A1 (en) * 2006-02-27 2007-09-20 National University Corporation Nagoya University Method for producing nanoparticle
CN101037388A (en) * 2007-04-17 2007-09-19 华东师范大学 Multifunctional ion liquid system, preparation and application thereof
CN105297133A (en) * 2015-10-28 2016-02-03 南京理工大学 Preparation method of single-crystal less-layer antimonene
CN106191999A (en) * 2016-09-19 2016-12-07 中国科学院物理研究所 A kind of antimony alkene two-dimensional atomic crystal material and preparation method thereof

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