CN102030361B - Method for preparing pine-like cadmium sulfide from ethylenediamine type ionic liquid - Google Patents
Method for preparing pine-like cadmium sulfide from ethylenediamine type ionic liquid Download PDFInfo
- Publication number
- CN102030361B CN102030361B CN 201010555278 CN201010555278A CN102030361B CN 102030361 B CN102030361 B CN 102030361B CN 201010555278 CN201010555278 CN 201010555278 CN 201010555278 A CN201010555278 A CN 201010555278A CN 102030361 B CN102030361 B CN 102030361B
- Authority
- CN
- China
- Prior art keywords
- ionic liquid
- cadmium sulfide
- quadrol
- sulfide
- deionized water
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
Images
Landscapes
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention relates to the field of preparation methods of cadmium sulfide (CdS) as an inorganic material, in particular to a method for preparing pine-like cadmium sulfide, which comprises the following steps of: (1) dissolving ethylenediamine into deionized water, then adding fluoboric acid, steaming water in the mixed liquid to obtain an ethylenediamine type ionic liquid; (2) mixing the ethylenediamine type ionic liquid prepared in the step (1) with the deionized water, adding a sulfide and cadmium chloride dihydrate to form a transparent solution; and (3) heating in a high-pressure autoclave to react, and then separating to obtain the target product. The heating temperature in the step (3) is 180-200 DEG C; the volume ratio of the ethylenediamine type ionic liquid to the deionized water in the step (2) is 3:1; and the sulfide in the step (2) is sulfourea. In the invention, the pine-like cadmium sulfide is prepared with a hydrothermal synthesis method with simple and easy operation, low cost, high product purity and possibility for mass production.
Description
Technical field
the present invention relates to preparation method field, the especially preparation method of the dendritic Cadmium Sulfide of pine tree of inorganic materials Cadmium Sulfide (CdS).
Background technology
are as important semiconductor material; Cadmium Sulfide is at photocatalyst, gas sensor, laser and infrared eye, solar cell; Fields such as photodiode and other optics are widely used; At present, its preparation method mainly contains template, thermal evaporation, chemical solution method etc.Chemical synthesis is simple, effective, is that the synthesizing cadmium sulfide nano material is used maximum methods.When nano materials, often to use some deleterious reagent, such as quadrol etc.Synthesized a lot of novel nano materials although use quadrol,, from the angle of Green Chemistry, should avoid the use of extreme conditions such as high temperature, anhydrous and oxygen-free, poisonous atmosphere as far as possible.
ionic liquid has a lot of advantages such as non-volatile, lower melting point, wide liquid journey, strong electrostatic field, wide electrochemical window, favorable conductive and thermal conductivity, good light transmittance and high refractive index, high heat capacity, high stability, selective dissolution power and designability; Received widely and having paid close attention to; People begin ionic liquid is combined with inorganics in recent years; Prepare the property material; This method has overcome high-temperature cracking method commonly used at present to a certain extent and has prepared nanocrystalline defective, is therefore developed fast.For example, Chinese patent: publication number is: 200510048415.7, and application number: 200510107214.X; 200610016252.9,200610053688.5,200710036633.8; 200710056250.7 patents such as 200810013390.0 all adopt ionic liquid to prepare nano material.But many employing positively charged ions are the ionic liquid of imidazoles in the preparation of these nano materials, and this kind ionic liquid preparation procedure is complicated, and cost is higher, is unfavorable for that ionic liquid prepares the industriallization of nano material.
Summary of the invention
the present invention be intended to overcome the weak point of prior art and provide a kind of program simple, and cost is low, and product purity is high, but the dendritic Cadmium Sulfide preparation method of the pine tree of suitable for mass production.
are for achieving the above object; The present invention is achieved in that a kind of quadrol type ionic liquid prepares the method for the dendritic Cadmium Sulfide of pine tree; Can carry out successively as follows: (1) is dissolved into quadrol in the deionized water; Add fluoroboric acid then, the water in the gained mixed solution is steamed, promptly get quadrol type ionic liquid; (2) get the said quadrol type of step (1) ionic liquid and mix, add sulfide and two water Cadmium chloride fine powdeies, form clear solution with deionized water; (3) in autoclave, heating, reaction promptly gets the purpose product after the separation.
as a kind of preferred version, the Heating temperature in the step according to the invention (3) is: 180～200 ℃.
as another kind of preferred version, the volume ratio of quadrol type ionic liquid and deionized water is 3:1 in the step according to the invention (2).
further, the sulfide in the step according to the invention (2) is thiocarbamide.
further, the add-on of thiocarbamide according to the invention and two water Cadmium chloride fine powdeies is 0.3g.
in addition, the time of the reaction in the step according to the invention (3) is 12 hours.
secondly, the volume ratio of quadrol and fluoroboric acid is 1:1 in the step according to the invention (1).
adopt quadrol to be the synthetic ionic liquid of positively charged ion single stage method in the present invention, and its program is simple and cost is lower, can be the industriallization that ionic liquid prepares nano material foundation is provided.
the present invention adopts hydrothermal synthesis method to prepare dendritic cadmium sulfide, and simple to operation, cost is low, and the product purity that makes is high, is expected to produce in enormous quantities.
Description of drawings
are described further the present invention below in conjunction with accompanying drawing and embodiment.Protection scope of the present invention not only is confined to the statement of following content.
Fig. 1 is field emission scanning electron microscope (SEM) photo of the dendritic cadmium sulfide that makes with the inventive method.
Fig. 2 is X-ray diffraction (XRD) spectrogram of the dendritic cadmium sulfide that makes with the inventive method.
The bar-shaped Cadmium Sulfide SEM photo of
Fig. 3 for preparing in quadrol and the water mixed solution.
Embodiment
method for preparing dendritic cadmium sulfide of the present invention; What adopt is hydrothermal synthesis method; Its step is following: quadrol is added dropwise in the 80mL deionized water while stirring, and the fluoroboric acid of getting with the quadrol equal volume joins in the above-mentioned mixed solution lentamente, continues to stir 6 hours; Adopt Rotary Evaporators to steam the water in the mixed solution then, obtain quadrol type ionic liquid.Get the ionic liquid of 30ml and mix, add the thiocarbamide of 0.3g and the two water Cadmium chloride fine powdeies of 0.3g and stir until forming transparent solution with the deionized water of 10ml.Transfer to then in the autoclave of 50ml,, after reaction finishes, separate obtaining product, flush away impurity, 80 ℃ of dry 6h down at 180 ℃～200 ℃ following heating 12h.The present invention prepares in the process, and all reagent are commerical prod, need not loaded down with trivial details preparation; The present invention prepares in the process, and the heat-up time in autoclave should be greater than 12h.
embodiment 1.
are got the quadrol type ionic liquid of 30ml and are mixed with the deionized water of 10ml, add the thiocarbamide of 0.3g and the two water Cadmium chloride fine powdeies of 0.3g and stir until the transparent solution of formation.Transfer to then in the autoclave of 50ml,, after reaction finishes, separate obtaining product, flush away impurity, 80 ℃ of dry 6h down at 180 ℃～200 ℃ following heating 12h.
are directly observed under field emission scanning electron microscope like Fig. 1, and as can be seen from the figure, the whole pattern of product is the pine branch shape, and purity is very high, do not have any other shape.Each branch is a club shaped structure, and the top of rod is point, but the length and the thickness of rod have bigger difference.
Fig. 2 is the XRD figure spectrum of sample.Through demarcating, all diffraction peaks are all consistent with standard diagram (PDF.No 41-4019), do not find other impurity peaks.Through analyzing, products therefrom belongs to the hexagonal crystal phase of Cadmium Sulfide, and its lattice parameter is: a=0.4119nm, c=0.6723nm.The intensity of sample diffraction peak is stronger among the figure, and the halfwidth broad, shows that gained cadmium sulfide nano material crystallinity is better.
embodiment 2.
are got the quadrol type ionic liquid of 30ml and are mixed with the deionized water of 10ml, add the thiocarbamide of 0.3g and the two water Cadmium chloride fine powdeies of 0.3g and stir until the transparent solution of formation.Transfer to then in the autoclave of 50ml,, after reaction finishes, separate obtaining product, flush away impurity, 80 ℃ of dry 6h down at 180 ℃～200 ℃ following heating 14h.
It is basic identical that
field emission scanning electron microscope is observed pattern and Fig. 1 down.
embodiment 3.
are got the quadrol type ionic liquid of 30ml and are mixed with the deionized water of 10ml, add the thiocarbamide of 0.3g and the two water Cadmium chloride fine powdeies of 0.3g and stir until the transparent solution of formation.Transfer to then in the autoclave of 50ml,, after reaction finishes, separate obtaining product, flush away impurity, 80 ℃ of dry 6h down at 180 ℃～200 ℃ following heating 16h.
It is basic identical that
field emission scanning electron microscope is observed pattern and Fig. 1 down.
comparative example.
The ethylenediamine ion liquid that 30ml is got in
mixes with the deionized water of 10ml, adds the thiocarbamide of 0.3g and the two water Cadmium chloride fine powdeies of 0.3g and stirs until forming transparent solution.Transfer to then in the autoclave of 50ml,, after reaction finishes, separate obtaining product, flush away impurity, 80 ℃ of dry 6h down at 180 ℃～200 ℃ following heating 16h.Shape characteristic is seen Fig. 3.
The above is merely the preferred embodiments of the present invention
, is not limited to the present invention, and for a person skilled in the art, the present invention can have various changes and variation.All within spirit of the present invention and principle, any modification of being done, be equal to replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (6)
1. a quadrol type ionic liquid prepares the method for the dendritic Cadmium Sulfide of pine tree, it is characterized in that, carries out successively as follows:
(1) quadrol is dissolved in the deionized water, adds fluoroboric acid then, the water in the gained mixed solution is steamed, promptly get quadrol type ionic liquid;
(2) get the said quadrol type of step (1) ionic liquid and mix, add sulfide and two water Cadmium chloride fine powdeies, form clear solution with deionized water; Said sulfide is thiocarbamide;
(3) in autoclave, heating, reaction promptly gets the purpose product after the separation.
2. prepare the method for the dendritic Cadmium Sulfide of pine tree according to the described quadrol type of claim 1 ionic liquid, it is characterized in that: the Heating temperature in the step (3) is: 180～200 ℃.
3. prepare the method for the dendritic Cadmium Sulfide of pine tree according to the described quadrol type of claim 2 ionic liquid, it is characterized in that: the volume ratio of quadrol type ionic liquid and deionized water is 3:1 in the said step (2).
4. prepare the method for the dendritic Cadmium Sulfide of pine tree according to the described quadrol type of claim 3 ionic liquid, it is characterized in that: the add-on of said thiocarbamide and two water Cadmium chloride fine powdeies is 0.3g.
5. prepare the method for the dendritic Cadmium Sulfide of pine tree according to the described quadrol type of claim 4 ionic liquid, it is characterized in that: the time of the reaction in the said step (3) is 12 hours.
6. prepare the method for the dendritic Cadmium Sulfide of pine tree according to the arbitrary described quadrol type ionic liquid of claim 1～5, it is characterized in that: the volume ratio of quadrol and fluoroboric acid is 1:1 in the said step (1).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201010555278 CN102030361B (en) | 2010-11-23 | 2010-11-23 | Method for preparing pine-like cadmium sulfide from ethylenediamine type ionic liquid |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201010555278 CN102030361B (en) | 2010-11-23 | 2010-11-23 | Method for preparing pine-like cadmium sulfide from ethylenediamine type ionic liquid |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN102030361A CN102030361A (en) | 2011-04-27 |
| CN102030361B true CN102030361B (en) | 2012-11-14 |
Family
ID=43883887
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 201010555278 Expired - Fee Related CN102030361B (en) | 2010-11-23 | 2010-11-23 | Method for preparing pine-like cadmium sulfide from ethylenediamine type ionic liquid |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102030361B (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103708532B (en) * | 2014-01-02 | 2015-09-30 | 天津大学 | Dendritic cadmium sulfide superfine nanorod grade structural material and preparation method thereof |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105399136B (en) * | 2015-12-18 | 2017-05-10 | 济南大学 | Preparation method for CdS flower-shaped self-assembly structure and obtained product |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1818153A (en) * | 2006-01-18 | 2006-08-16 | 浙江大学 | Production of nanometer wire with cadmium sulfide |
| US7547347B2 (en) * | 2005-05-13 | 2009-06-16 | University Of Rochester | Synthesis of nano-materials in ionic liquids |
| CN101559976A (en) * | 2009-05-27 | 2009-10-21 | 辽宁石油化工大学 | Method for preparing dendritic cadmium sulfide |
-
2010
- 2010-11-23 CN CN 201010555278 patent/CN102030361B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7547347B2 (en) * | 2005-05-13 | 2009-06-16 | University Of Rochester | Synthesis of nano-materials in ionic liquids |
| CN1818153A (en) * | 2006-01-18 | 2006-08-16 | 浙江大学 | Production of nanometer wire with cadmium sulfide |
| CN101559976A (en) * | 2009-05-27 | 2009-10-21 | 辽宁石油化工大学 | Method for preparing dendritic cadmium sulfide |
Non-Patent Citations (1)
| Title |
|---|
| 郭福强等.溶剂热合成CdS纳米棒及光学性能研究.《人工晶体学报》.2009,第38卷(第4期),第2页第2段. * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103708532B (en) * | 2014-01-02 | 2015-09-30 | 天津大学 | Dendritic cadmium sulfide superfine nanorod grade structural material and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN102030361A (en) | 2011-04-27 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Zhang et al. | Preparation of nano-Li2FeSiO4 as cathode material for lithium-ion batteries | |
| Long et al. | A novel solvent-free strategy for the synthesis of bismuth oxyhalides | |
| CN102491417B (en) | Method for preparing ball-flower-shaped gamma-bismuth trioxide powder | |
| CN106115654B (en) | A kind of three-dimensional porous carbon material of Heteroatom doping, preparation method and applications | |
| CN102923791B (en) | Method for preparing multi-tunnel cobaltosic oxide flower-like microspheres by solvothermal method | |
| CN104014356B (en) | A kind of preparation method of phosphorus doping bismuth phosphate photocatalyst | |
| França et al. | Rice husk ash as raw material for the synthesis of silicon and potassium slow-release fertilizer | |
| CN102030361B (en) | Method for preparing pine-like cadmium sulfide from ethylenediamine type ionic liquid | |
| CN102504820B (en) | Preparation method of up-conversion fluorescence/paramagnetic difunctional nanocrystal | |
| CN106542569A (en) | A kind of preparation method of flower ball-shaped tin ash | |
| CN103342396B (en) | Method for microwave liquid-phase synthesis of graphene-like two-dimensional nickel hydroxide nano material | |
| CN101559976A (en) | Method for preparing dendritic cadmium sulfide | |
| CN103071479A (en) | Preparation method for double-rare earth element lanthanum and gadolinium codoped titanium dioxide nanotube | |
| CN104192890A (en) | Method for preparing carbon-dope zinc oxide nanopillars | |
| CN104291278B (en) | A kind of method of hydrazine hydrate auxiliary polyhydric alcohol based sols synthesis β phase indium selenide flaky nanocrystalline | |
| CN109321948A (en) | A kind of method that quick Green Electrochemical prepares Silver nanorod | |
| Bankole et al. | Silicon exchange effects of glassware on the recovery of LiPF6: Alternative route to preparation of Li2SiF6 | |
| CN102745747A (en) | Preparation method for rod-like Sc2W3O12 negative thermal expansion material | |
| CN112158887B (en) | ZnMoO prepared by hydrothermal method4Method for introducing fluorine ions | |
| Qiu et al. | An optimized preparation procedure of tetrabasic lead sulfate for lead-acid batteries | |
| CN102618283B (en) | Method for preparing bowknot-shaped terbium-mixed Teflon gadolinium sodium green luminous nanometer materials | |
| CN103588180A (en) | Method for synthesis of CIASe (Cu-In-Al-Se) nanocrystalline by using triethylene tetramine auxiliary polyhydric alcohol solution | |
| CN101857568B (en) | Preparation method of 8-hydroxyquinoline zinc with shape of octahedron | |
| CN102786038A (en) | Hydro-thermal synthesis method of cubic phase InSe nano sheet | |
| CN101343041B (en) | Synthesis of three-component fluoride ABF3 at low-temperature |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C17 | Cessation of patent right | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20121114 Termination date: 20131123 |