CN105645456B - A kind of preparation method of CuI nano-powders - Google Patents
A kind of preparation method of CuI nano-powders Download PDFInfo
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- CN105645456B CN105645456B CN201610200980.9A CN201610200980A CN105645456B CN 105645456 B CN105645456 B CN 105645456B CN 201610200980 A CN201610200980 A CN 201610200980A CN 105645456 B CN105645456 B CN 105645456B
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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
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- 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
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- 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
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- 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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Abstract
It is that at ambient temperature, one pot of iodine, copper sulphate, acetone, water and ethyl alcohol mixing are stirred to react the invention discloses a kind of preparation method of CuI nano-powders；Then reaction product centrifuged, distillation water washing, be dried in vacuo, obtain CuI nano-powders.The preparation process of CuI nano-powders of the present invention uses reaction raw materials one kettle way technology of preparing, and preparation process is simple, and reaction temperature is low, has energy conservation and environmental protection, the advantage of highly effective and safe.
Description
Technical field
The invention belongs to nano material and its preparation field, more particularly to a kind of preparation method of CuI nano-powders.
Background technology
CuI is a kind of substance that purposes is very extensive, can be used as organic catalyst compound, modifier, rain making
Iodine source in agent and iodizedsalt.Wherein, it is anti-can to be catalyzed a series of coupling that halogenated hydrocarbons participate in as catalyst by CuI
It answers, such as Heck reactions, Suzuki reactions and Ullmann reactions etc..
Currently, the preparation method of CuI is more.Such as：Elemental direct reaction method (Yaqing Liu, et.al.Synthesis
of nano-CuI and its catalytic activity in the thermal decomposition of
Ammonium perchlorate, Res.Chem.Intermed., 2015,41:3885-3892), electrodeposition process (Takeshi
Takeda,et.al.Copper(I)iodide-catalyzed regioselective allylation of α-(2-
pyridylthio)allylstannanes.A new route to δ,ε-unsaturated ketones,Tetrahedron
Lett., 1997,38,2879-2882), hydro-thermal method (L.P.Zhang, et.al.Growth and shape evolution of
Octahedral CuI crystal by a SC-assisted hydrothermal method, Mater.Res.Bull.,
2006,41,905-908), pulsed laser deposition (P.M.Sirimanne, et.al.Characterization of
transparent conducting CuI thin films prepared by pulse laser deposition
Technique, Chem.Phys.Lett., 2002,366,485-489), be evaporated in vacuo (K.Tennakone,
Et.al.Deposition of thin conducting films of CuI on glass, Sol.Energy
Mater.Sol.Cells, 1998,55,283-289), etc..
Although existing preparation method can prepare CuI, but still come with some shortcomings, such as：In preparation process, have
The equipment needed using complex and expensive, some need uses additive, some need hot conditions, some generations to be more toxic
By-product, or the products therefrom particle size distribution range having is wider.
Invention content
The present invention is provided a kind of simple and practicable, cost-effective, energy-saving and environment-friendly to avoid above-mentioned the deficiencies in the prior art
CuI nano-powder preparation methods.
The present invention solves technical problem, adopts the following technical scheme that：
The preparation method of CuI nano-powders of the present invention, be at ambient temperature, by iodine, copper sulphate, acetone, water and
One pot of mixing of ethyl alcohol, is stirred to react；Then reaction product centrifuged, distillation water washing, be dried in vacuo, obtain CuI nanometers
Powder；Specifically comprise the following steps：
(1) iodine is dissolved in the mixed solvent of second alcohol and water (volume ratio of second alcohol and water is preferably 1:1) it in, is made
A concentration of 0.075~0.30molL-1Iodine solution；
(2) copper sulphate is dissolved in the mixed solvent of acetone and water (volume ratio of acetone and water is preferably 1:4) it in, is made
A concentration of 0.050~0.20molL-1Copper-bath；
(3) iodine solution and the copper-bath are mixed in equal volume, obtains mixed solution (wherein, copper sulphate
A concentration of 0.025~0.10molL-1, a concentration of 0.0375~0.15molL of iodine-1)；In the mixed solution
The molar ratio of copper sulphate and iodine is 2:3；
(4) mixed solution for obtaining step (3) is added in closed container, continuously stirs 24 hours at room temperature, gained
Product is by centrifuging, distilling water washing, vacuum drying (being dried in vacuo 4 hours at preferably 80 DEG C) to get to CuI nanometers
Powder.
The present invention utilizes the iodination reaction of acetone to generate iodide ion in situ at ambient temperature, realizes precipitation from homogeneous solution, prepares
Go out CuI nano-particles, shown in the reaction such as equation (1) and equation (2) of generation.The preparation method is easy to operate, and reaction temperature is low,
Product CuI particle diameter of nanometer powder narrow distribution ranges are the preparation sides of CuI nano-powders that are a kind of easy and not will produce pollution
Method.
CH3-CO-CH3+I2→CH3-CO-CH2I+I-+H+ (1)
Beneficial effects of the present invention are embodied in：
(1) in the preparation method of CuI nano-powders of the present invention, with copper ion (Cu2+) the required iodine of precipitation reaction occurs
Ion (I-) not external addition, it is generated in situ by the iodination reaction of acetone, realizes homogeneous precipitation method preparation
CuI ensure that particle size narrow distribution range, good dispersion, regular shape；And the preparation method of the present invention need not add table
Face activating agent, template etc., improve product purity.
(2) preparation process of CuI nano-powders of the present invention uses reaction raw materials one kettle way technology of preparing, preparation process
Simply, reaction temperature is low, has energy conservation and environmental protection, the advantage of highly effective and safe.
Description of the drawings
Fig. 1 is the XRD diagram of CuI nano-powders prepared by the embodiment of the present invention 1,2,3 and 4.
Fig. 2 is the TEM image of CuI nano-powders prepared by the embodiment of the present invention 2.
Specific implementation mode
Specific implementation mode prepared by CuI nano-powders of the present invention presented below.
Embodiment 1
The present embodiment prepares CuI nano-powders as follows：
(1) it is 1 1.50mmol iodines to be dissolved in 20mL volume ratios:The in the mixed solvent of 1 second alcohol and water is made
0.075mol·L-1Iodine solution.
(2) it is 1 1.0mmol copper sulphate to be dissolved in 20mL volume ratios:4 acetone and the in the mixed solvent of water are made
0.050mol·L-1Copper-bath.
(3) iodine solution and copper-bath merge to mixing in iodine flask, obtains mixed solution (wherein, copper sulphate
A concentration of 0.025molL-1, a concentration of 0.0375molL of iodine-1)。
(4) by mixed solution continuous magnetic agitation 24 hours at room temperature, products therefrom is by centrifuging, distilling washing
It washs, then is dried in vacuo 4 hours at 80 DEG C, obtain CuI nano-powders.
X-ray diffraction analysis is carried out to product, is calculated by Scherrer formula, has obtained CuI average crystal grain rulers
Very little is 48.7nm.
Embodiment 2
The present embodiment prepares CuI nano-powders as follows：
(1) it is 1 6.0mmol iodines to be dissolved in 20mL volume ratios:The in the mixed solvent of 1 second alcohol and water is made
0.30mol·L-1Iodine solution.
(2) it is 1 4.0mmol copper sulphate to be dissolved in 20mL volume ratios:4 acetone and the in the mixed solvent of water are made
0.20mol·L-1Copper-bath.
(3) iodine solution and copper-bath merge to mixing in iodine flask, obtains mixed solution (wherein, copper sulphate
A concentration of 0.10molL-1, a concentration of 0.15molL of iodine-1)。
(4) by mixed solution continuous magnetic agitation 24 hours at room temperature, products therefrom is by centrifuging, distilling washing
It washs, then is dried in vacuo 4 hours at 80 DEG C, obtain CuI nano-powders.
X-ray diffraction analysis is carried out to product, is calculated by Scherrer formula, has obtained CuI average crystal grain rulers
Very little is 38.1nm.
Embodiment 3
The present embodiment prepares CuI nano-powders as follows：
(1) it is 1 3.0mmol iodines to be dissolved in 20mL volume ratios:The in the mixed solvent of 1 second alcohol and water is made
0.15mol·L-1Iodine solution.
(2) it is 1 2.0mmol copper sulphate to be dissolved in 20mL volume ratios:4 acetone and the in the mixed solvent of water are made
0.10mol·L-1Copper-bath.
(3) iodine solution and copper-bath merge to mixing in iodine flask, obtains mixed solution (wherein, copper sulphate
A concentration of 0.050molL-1, a concentration of 0.075molL of iodine-1)。
(4) by mixed solution continuous magnetic agitation 24 hours at room temperature, products therefrom is by centrifuging, distilling washing
It washs, then is dried in vacuo 4 hours at 80 DEG C, obtain CuI nano-powders.
X-ray diffraction analysis is carried out to product, is calculated by Scherrer formula, has obtained CuI average crystal grain rulers
Very little is 44.3nm.
Embodiment 4
The present embodiment prepares CuI nano-powders as follows：
(1) it is 1 4.5mmol iodines to be dissolved in 20mL volume ratios:The in the mixed solvent of 1 second alcohol and water is made
0.225mol·L-1Iodine solution.
(2) it is 1 3.0mmol copper sulphate to be dissolved in 20mL volume ratios:4 acetone and the in the mixed solvent of water are made
0.15mol·L-1Copper-bath.
(3) iodine solution and copper-bath merge to mixing in iodine flask, obtains mixed solution (wherein, copper sulphate
A concentration of 0.075molL-1, a concentration of 0.1125molL of iodine-1)。
(4) by mixed solution continuous magnetic agitation 24 hours at room temperature, products therefrom is by centrifuging, distilling washing
It washs, then is dried in vacuo 4 hours at 80 DEG C, obtain CuI nano-powders.X-ray diffraction analysis is carried out to product, is passed through
Scherrer formula are calculated, and it is 40.9nm to have obtained CuI average grain sizes.
Performance test：
X-ray diffraction analyzes (XRD analysis)：CuI nano-powders made from embodiment 1,2,3 and 4 are subjected to XRD respectively
Analysis, the result is shown in Figure 1.It is calculated by Scherrer formula：The concentration of copper sulphate (iodine) is respectively in reaction raw materials
0.025(0.0375)、0.050(0.075)、0.075(0.1125)、0.10(0.15)mol·L-1When, gained CuI particles are put down
Equal crystallite dimension is respectively 48.7,44.3,40.9,38.1nm, show the variation of copper sulphate and simple substance iodine concentration in reaction raw materials
It has a certain impact to the average grain size of CuI, with the increase of copper sulphate and simple substance iodine concentration, the average crystalline substance of product CuI
Grain size is gradually reduced.In preparation process, the average crystal grain of CuI particles can be controlled by controlling the concentration of reaction raw materials
Size.
Tem study (tem analysis)：CuI nano-powders made from embodiment 2 are subjected to tem analysis, knot
Fruit such as Fig. 2.CuI nano particle diameters narrow distribution range as can be seen from Figure 2, granular size is in 40nm or so.
Claims (4)
1. a kind of precipitation from homogeneous solution preparation method of CuI nano-powders, it is characterised in that include the following steps：
(1) iodine is dissolved in the in the mixed solvent of second alcohol and water, a concentration of 0.075~0.30molL is made-1Iodine it is molten
Liquid；
(2) copper sulphate is dissolved in the in the mixed solvent of acetone and water, a concentration of 0.050~0.20molL is made-1Sulfuric acid
Copper solution；
(3) iodine solution and the copper-bath are mixed in equal volume, obtains mixed solution；The sulphur in the mixed solution
The molar ratio of sour copper and iodine is 2:3；
(4) mixed solution for obtaining step (3) is added in closed container, continuously stirs 24 hours at room temperature, products therefrom
By centrifuging, distilling water washing, vacuum drying to get to CuI nano-powders, the particle diameter distribution of gained CuI nano-powders
Narrow range.
2. the precipitation from homogeneous solution preparation method of CuI nano-powders according to claim 1, it is characterised in that：Second in step (1)
The volume ratio of alcohol and water is 1:1.
3. the precipitation from homogeneous solution preparation method of CuI nano-powders according to claim 1, it is characterised in that：Third in step (2)
The volume ratio of ketone and water is 1:4.
4. the precipitation from homogeneous solution preparation method of CuI nano-powders according to claim 1, it is characterised in that：It is true in step (4)
Empty drying is dried in vacuo 4 hours at 80 DEG C.
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| CN106115764B (en) * | 2016-06-23 | 2017-12-12 | 淮北师范大学 | The method that one pot of ball milling solid phase method prepares CuI nano-powders |
| 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 |
| 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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| US3384450A (en) * | 1966-02-07 | 1968-05-21 | Eastman Kodak Co | Method for synthesizing cuprous iodide from a cupric salt |
| JPS55109226A (en) * | 1979-02-09 | 1980-08-22 | Ricoh Co Ltd | Preparing white copper iodide |
| CN1298632C (en) * | 2005-03-25 | 2007-02-07 | 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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