CN105645456A - Preparation method of CuI nano-powder - Google Patents

Preparation method of CuI nano-powder Download PDF

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CN105645456A
CN105645456A CN201610200980.9A CN201610200980A CN105645456A CN 105645456 A CN105645456 A CN 105645456A CN 201610200980 A CN201610200980 A CN 201610200980A CN 105645456 A CN105645456 A CN 105645456A
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powder
cui
preparation
iodine
nano
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CN105645456B (en
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李龙凤
张茂林
刘明珠
付先亮
肖培培
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Huaibei Normal University
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Huaibei Normal University
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G3/00—Compounds of copper
    • C01G3/04—Halides
    • 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

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Manufacture Of Metal Powder And Suspensions Thereof (AREA)

Abstract

The invention discloses a preparation method of CuI nano-powder, comprising: at room temperature, mixing elemental iodine, copper sulfate, acetone, water and ethyl alcohol in a pot, and stirring for reacting; subjecting a reaction product to centrifugal separation, distilled water washing and vacuum drying to obtain the CuI nano-powder. In the preparation process of the CuI nano-powder, one-pot production technology of reaction materials is used, the preparation process is simple, reaction temperature is low, and the preparation method has the advantages of energy efficiency, environmental friendliness, high efficiency and safety.

Description

A kind of preparation method of CuI nano-powder
Technical field
The invention belongs to nano material and preparation field thereof, particularly to the preparation method of a kind of CuI nano-powder.
Background technology
CuI is a kind of purposes material very widely, can be used as organic catalyst compound, modifier, rain making agent and the iodine source in iodized salt. Wherein, CuI is as catalyst, it is possible to the coupling reaction that a series of halogenated hydrocarbons of catalysis participates in, for instance Heck reaction, Suzuki reaction and Ullmann reaction etc.
At present, the preparation method of CuI is more. such as: elemental direct reaction method (YaqingLiu, et.al.Synthesisofnano-CuIanditscatalyticactivityinthethe rmaldecompositionofammoniumperchlorate, Res.Chem.Intermed., 2015, 41:3885 3892), electrodeposition process (TakeshiTakeda, et.al.Copper (I) iodide-catalyzedregioselectiveallylationof ��-(2-pyridylthio) allylstannanes.Anewrouteto ��, ��-unsaturatedketones, TetrahedronLett., 1997, 38, 2879 2882), hydro-thermal method (L.P.Zhang, et.al.GrowthandshapeevolutionofoctahedralCuIcrystalbyaSC-assistedhydrothermalmethod, Mater.Res.Bull., 2006, 41, 905 908), pulsed laser deposition (P.M.Sirimanne, et.al.CharacterizationoftransparentconductingCuIthinfilm spreparedbypulselaserdepositiontechnique, Chem.Phys.Lett., 2002, 366, 485 489), vacuum evaporation (K.Tennakone, et.al.DepositionofthinconductingfilmsofCuIonglass, Sol.EnergyMater.Sol.Cells, 1998, 55, 283 289), etc..
Although existing preparation method can prepare CuI, but still come with some shortcomings, as: in preparation process, the equipment needing to use complex and expensive having, what have needs use additive, what have needs hot conditions, the by-product that some generation toxicity is bigger, or the products therefrom particle size distribution range having is wider.
Summary of the invention
The present invention is for avoiding above-mentioned the deficiencies in the prior art, it is provided that a kind of simple, save cost, energy-conserving and environment-protective CuI nano-powder preparation method.
This invention address that technical problem, adopt the following technical scheme that
The preparation method of CuI nano-powder of the present invention, is at ambient temperature, by iodine, copper sulfate, acetone, water and ethanol one pot mixing, stirring reaction;Then to product centrifugation, distilled water wash, vacuum drying, CuI nano-powder is obtained; Specifically include following steps:
(1) being dissolved in by iodine in the mixed solvent (volume ratio of second alcohol and water is preferably 1:1) of second alcohol and water, prepared concentration is 0.075��0.30mol L-1Iodine solution;
(2) being dissolved in by copper sulfate in the mixed solvent (volume ratio of acetone and water is preferably 1:4) of acetone and water, prepared concentration is 0.050��0.20mol L-1Copper-bath;
(3) described iodine solution and described copper-bath equal-volume are mixed, it is thus achieved that (wherein, the concentration of copper sulfate is 0.025��0.10mol L to mixed solution-1, the concentration of iodine is 0.0375��0.15mol L-1); In described mixed solution, the mol ratio of copper sulfate and iodine is 2:3;
(4) mixed solution step (3) obtained adds in hermetic container, at room temperature continuous stirring 24 hours, products therefrom, by centrifugation, distilled water wash, vacuum drying (at being preferably 80 DEG C vacuum drying 4 hours), namely obtains CuI nano-powder.
The present invention utilizes the iodination reaction original position of acetone to produce iodide ion at ambient temperature, it is achieved precipitation from homogeneous solution, prepares CuI nanoparticle, the reaction of generation such as equation (1) and shown in equation (2). This preparation method is simple to operate, and reaction temperature is low, product CuI particle diameter of nanometer powder narrow distribution range, is a kind of simplicity and the preparation method that will not produce the CuI nano-powder polluted.
CH3-CO-CH3+I2��CH3-CO-CH2I+I-+H+(1)
Beneficial effects of the present invention is embodied in:
(1) in the preparation method of CuI nano-powder of the present invention, with copper ion (Cu2+) there is the iodide ion (I required for precipitation-) it not external addition, but produced by the iodination reaction original position of acetone, it is achieved that homogeneous precipitation method prepares CuI, it is ensured that particle size narrow distribution range, good dispersion, regular shape; And the preparation method of the present invention need not add surfactant, template etc., improve product purity.
(2) preparation process of CuI nano-powder of the present invention, have employed reaction raw materials one kettle way technology of preparing, and preparation process is simple, and reaction temperature is low, has the advantage of energy-conserving and environment-protective, highly effective and safe.
Accompanying drawing explanation
Fig. 1 is the XRD figure of the CuI nano-powder of the embodiment of the present invention 1,2,3 and 4 preparation.
Fig. 2 is the TEM image of the CuI nano-powder of the embodiment of the present invention 2 preparation.
Detailed description of the invention
Detailed description of the invention prepared by CuI nano-powder of the present invention presented below.
Embodiment 1
The present embodiment prepares CuI nano-powder as follows:
(1) 1.50mmol iodine is dissolved in the mixed solvent of the second alcohol and water that 20mL volume ratio is 1:1, prepares 0.075mol L-1Iodine solution.
(2) 1.0mmol copper sulfate is dissolved in the mixed solvent of acetone that 20mL volume ratio is 1:4 and water, prepares 0.050mol L-1Copper-bath.
(3) iodine solution and copper-bath are merged mixing in iodine flask, it is thus achieved that (wherein, the concentration of copper sulfate is 0.025mol L to mixed solution-1, the concentration of iodine is 0.0375mol L-1)��
(4) by mixed solution at room temperature continuous magnetic agitation 24 hours, products therefrom passes through centrifugation, distilled water wash, then at 80 DEG C vacuum drying 4 hours, obtain CuI nano-powder.
Product being carried out X-ray diffraction analysis, is calculated by Scherrer formula, obtaining CuI average grain size is 48.7nm.
Embodiment 2
The present embodiment prepares CuI nano-powder as follows:
(1) 6.0mmol iodine is dissolved in the mixed solvent of the second alcohol and water that 20mL volume ratio is 1:1, prepares 0.30mol L-1Iodine solution.
(2) 4.0mmol copper sulfate is dissolved in the mixed solvent of acetone that 20mL volume ratio is 1:4 and water, prepares 0.20mol L-1Copper-bath.
(3) iodine solution and copper-bath are merged mixing in iodine flask, it is thus achieved that (wherein, the concentration of copper sulfate is 0.10mol L to mixed solution-1, the concentration of iodine is 0.15mol L-1)��
(4) by mixed solution at room temperature continuous magnetic agitation 24 hours, products therefrom passes through centrifugation, distilled water wash, then at 80 DEG C vacuum drying 4 hours, obtain CuI nano-powder.
Product being carried out X-ray diffraction analysis, is calculated by Scherrer formula, obtaining CuI average grain size is 38.1nm.
Embodiment 3
The present embodiment prepares CuI nano-powder as follows:
(1) 3.0mmol iodine is dissolved in the mixed solvent of the second alcohol and water that 20mL volume ratio is 1:1, prepares 0.15mol L-1Iodine solution.
(2) 2.0mmol copper sulfate is dissolved in the mixed solvent of acetone that 20mL volume ratio is 1:4 and water, prepares 0.10mol L-1Copper-bath.
(3) iodine solution and copper-bath are merged mixing in iodine flask, it is thus achieved that (wherein, the concentration of copper sulfate is 0.050mol L to mixed solution-1, the concentration of iodine is 0.075mol L-1)��
(4) by mixed solution at room temperature continuous magnetic agitation 24 hours, products therefrom passes through centrifugation, distilled water wash, then at 80 DEG C vacuum drying 4 hours, obtain CuI nano-powder.
Product being carried out X-ray diffraction analysis, is calculated by Scherrer formula, obtaining CuI average grain size is 44.3nm.
Embodiment 4
The present embodiment prepares CuI nano-powder as follows:
(1) 4.5mmol iodine is dissolved in the mixed solvent of the second alcohol and water that 20mL volume ratio is 1:1, prepares 0.225mol L-1Iodine solution.
(2) 3.0mmol copper sulfate is dissolved in the mixed solvent of acetone that 20mL volume ratio is 1:4 and water, prepares 0.15mol L-1Copper-bath.
(3) iodine solution and copper-bath are merged mixing in iodine flask, it is thus achieved that (wherein, the concentration of copper sulfate is 0.075mol L to mixed solution-1, the concentration of iodine is 0.1125mol L-1)��
(4) by mixed solution at room temperature continuous magnetic agitation 24 hours, products therefrom passes through centrifugation, distilled water wash, then at 80 DEG C vacuum drying 4 hours, obtain CuI nano-powder. Product being carried out X-ray diffraction analysis, is calculated by Scherrer formula, obtaining CuI average grain size is 40.9nm.
Performance test:
X-ray diffraction analyzes (XRD analysis): respectively the CuI nano-powder that embodiment 1,2,3 and 4 prepares being carried out XRD analysis, result is shown in Fig. 1. Calculated by Scherrer formula and obtain: the concentration of copper sulfate (iodine) respectively 0.025 (0.0375), 0.050 (0.075), 0.075 (0.1125), 0.10 (0.15) mol L in reaction raw materials-1Time, the average grain size of gained CuI particle respectively 48.7,44.3,40.9,38.1nm, show that in reaction raw materials, the average grain size of CuI is had a certain impact by the change of copper sulfate and iodine concentration, along with the increase of copper sulfate and iodine concentration, the average crystal grain size of product CuI is gradually reduced. In preparation process, it is possible to control the average grain size of CuI particle by controlling the concentration of reaction raw materials.
Tem study (tem analysis): the CuI nano-powder that embodiment 2 prepares is carried out tem analysis, and result is Fig. 2 such as.CuI nano particle diameter narrow distribution range as can be seen from Figure 2, its granular size is at about 40nm.

Claims (4)

1. the preparation method of a CuI nano-powder, it is characterised in that comprise the steps:
(1) being dissolved in by iodine in the mixed solvent of second alcohol and water, prepared concentration is 0.075��0.30mol L-1Iodine solution;
(2) being dissolved in by copper sulfate in the mixed solvent of acetone and water, prepared concentration is 0.050��0.20mol L-1Copper-bath;
(3) described iodine solution and described copper-bath equal-volume are mixed, it is thus achieved that mixed solution; In described mixed solution, the mol ratio of copper sulfate and iodine is 2:3;
(4) mixed solution step (3) obtained adds in hermetic container, at room temperature continuous stirring 24 hours, and products therefrom passes through centrifugation, distilled water wash, vacuum drying, namely obtains CuI nano-powder.
2. the preparation method of CuI nano-powder according to claim 1, it is characterised in that: in step (1), the volume ratio of second alcohol and water is 1:1.
3. the preparation method of CuI nano-powder according to claim 1, it is characterised in that: in step (2), the volume ratio of acetone and water is 1:4.
4. the preparation method of CuI nano-powder according to claim 1, it is characterised in that: in step (4), vacuum drying is vacuum drying 4 hours at 80 DEG C.
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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106115764A (en) * 2016-06-23 2016-11-16 淮北师范大学 The method that one pot of ball milling solid phase method prepares CuI nano-powder
CN107583656A (en) * 2017-09-14 2018-01-16 华中科技大学 A kind of self-supporting Cu/CuI catalysis materials and preparation method thereof
CN111606350A (en) * 2020-07-23 2020-09-01 山东博苑医药化学有限公司 Environment-friendly preparation process of cuprous iodide

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB1173334A (en) * 1966-02-07 1969-12-10 Eastman Kodak Co Method of Making Cuprous Iodide
JPS55109226A (en) * 1979-02-09 1980-08-22 Ricoh Co Ltd Preparing white copper iodide
CN1673091A (en) * 2005-03-25 2005-09-28 吉林大学 Prepn process of nano copper iodide powder
CN101045551A (en) * 2006-11-07 2007-10-03 郑直 Chemical method for preparing nano metal iodine compound film

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB1173334A (en) * 1966-02-07 1969-12-10 Eastman Kodak Co Method of Making Cuprous Iodide
JPS55109226A (en) * 1979-02-09 1980-08-22 Ricoh Co Ltd Preparing white copper iodide
CN1673091A (en) * 2005-03-25 2005-09-28 吉林大学 Prepn process of nano copper iodide powder
CN101045551A (en) * 2006-11-07 2007-10-03 郑直 Chemical method for preparing nano metal iodine compound film

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Title
尹立辉等: "《实验化学教程》", 30 June 2014 *
李宏涛等: ""纳米碘化银、纳米碘化亚铜及纳米银的制备及抗菌性能研究"", 《HANS JOURNAL OF NANOTECHNOLOGY》 *

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106115764A (en) * 2016-06-23 2016-11-16 淮北师范大学 The method that one pot of ball milling solid phase method prepares CuI nano-powder
CN107583656A (en) * 2017-09-14 2018-01-16 华中科技大学 A kind of self-supporting Cu/CuI catalysis materials and preparation method thereof
CN111606350A (en) * 2020-07-23 2020-09-01 山东博苑医药化学有限公司 Environment-friendly preparation process of cuprous iodide
CN111606350B (en) * 2020-07-23 2022-10-04 山东博苑医药化学股份有限公司 Environment-friendly preparation process of cuprous iodide

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