CN102139910A - Method for preparing dandelion-shaped copper oxide hollow micrometer balls - Google Patents
Method for preparing dandelion-shaped copper oxide hollow micrometer balls Download PDFInfo
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- CN102139910A CN102139910A CN 201110075748 CN201110075748A CN102139910A CN 102139910 A CN102139910 A CN 102139910A CN 201110075748 CN201110075748 CN 201110075748 CN 201110075748 A CN201110075748 A CN 201110075748A CN 102139910 A CN102139910 A CN 102139910A
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Abstract
The invention discloses a method for preparing an inorganic material, namely copper oxide (CuO), in particular a method for preparing dandelion-shaped copper oxide hollow micrometer balls. The method comprises the following steps of: dissolving copper nitrate and urea in distilled water to form mixed solution; adding cetyl trimethyl ammonium bromide (CTAB) into the mixed solution to obtain a uniform jelly; moving the jelly into a reaction kettle, sealing the reaction kettle and reacting for a period of time; naturally cooling to room temperature; and precipitating reactants and performing centrifugal separation to obtain a black product, namely the dandelion-shaped CuO hollow micrometer balls. The method has the advantages of high controllability and low cost and is easy to operate; the prepared product has high purity; and the used reagents are commercial products and are not required to be prepared complexly. The dandelion-shaped copper oxide hollow micrometer balls can be widely applied to the semiconductor industry.
Description
Technical field
The present invention relates to the preparation method of inorganic materials cupric oxide (CuO), refer in particular to the preparation method of cupric oxide hollow micron ball.
Technical background
Cupric oxide (CuO) is a kind of important semi-conductor transition metal oxide, possesses excellent electric property, in fields such as catalyzer, gas sensor, lithium ion battery material, an emission projector and superconductors good prospects for application is arranged, can also form mixture oxide material improving its catalytic performance with other oxide compound, thereby more and more receive publicity in the materials chemistry field.The method for preparing at present cupric oxide (CuO) hollow micron ball mainly contains hard template method, soft template method, difference diffusion process (Kirkendall effect), formula slaking method difficult to understand (Ostwald ripening), chemical self-assembly method.Soft template method (soft template method) is metal-salt (water-soluble) directly to be added contain in the aqueous solution of soft template such as bubble, milk sap or micella, directly by hydrothermal treatment consists, just obtains inorganic oxide nanometer (micron) hollow ball.The product size of soft template method preparation is even, pattern and Stability Analysis of Structures, and template is easily removed, and is a kind of effective ways of synthetic hollow ball.But utilize cetyl trimethylammonium bromide (CTAB) to be soft template, urea is precipitation agent, and preparation taraxacum shape CuO hollow micron ball is not also reported.
Summary of the invention
The present invention is directed to deficiency of the prior art, proposed a kind of convenience, effective preparation method.
The present invention is achieved by following technical proposals:
A kind of method for preparing taraxacum shape cupric oxide hollow micron ball is characterized in that comprising the steps:
(1) cupric nitrate, urea are dissolved in the distilled water, form mixing solutions, in mixing solutions, add cetyl trimethylammonium bromide then, make it form uniform jelly; Wherein the mol ratio of cupric nitrate and urea is 1: 2～4; The total moles of cupric nitrate and urea and the mol ratio of distilled water are 1: 100～105; The cetyl trimethylammonium bromide quality that adds accounts for 4～10% of mixing solutions quality;
(2) then jelly is moved in the reactor, after the sealing reactant is heated to 180～190 ℃ and is incubated 6～8 hours respectively, naturally cool to room temperature then;
(3) reactant is precipitated, centrifugation, respectively wash 3 times with deionized water and dehydrated alcohol successively, obtaining the black product in 4 hours in 80 ℃ of dryings is taraxacum shape CuO hollow micron ball.
As preferably, the mol ratio of cupric nitrate and urea is 1: 3 among the above-mentioned preparation method.
As preferably, the cetyl trimethylammonium bromide quality that adds among the above-mentioned preparation method accounts for 5～7% of mixing solutions quality.
As preferably, the filling degree among the above-mentioned preparation method in reactor is 75%, and the filling degree is meant that the volume of reaction mass accounts for the per-cent of reactor volume.
The method for preparing taraxacum shape CuO hollow micron ball among the present invention is to adopt the template hydrothermal method, as cupric nitrate Cu (NO
3)
23H
2O, urea CO (NH
2)
2Be dissolved in and form mixing solutions in the distilled water, add cetyl trimethylammonium bromide (CTBA) then, under magnetic agitation, make it form uniform jelly; Reactor among the present invention is the stainless steel autoclave of inner liner polytetrafluoroethylene.
Beneficial effect: in the preparation process of the present invention, agents useful for same is commerical prod, need not loaded down with trivial details preparation; Process controllability of the present invention is strong, and is easy to operate, and cost is low, the product purity height that makes.
Description of drawings
Fig. 1 is scanning electron microscope (SEM) photo of the taraxacum shape CuO hollow micron ball that makes with the inventive method;
Fig. 2 is the SEM photo of the taraxacum shape CuO hollow micron ball that makes with the inventive method;
Fig. 3 is X-ray diffraction (XRD) spectrogram of the taraxacum shape CuO hollow micron ball that makes with the inventive method;
Fig. 4 is fourier infrared (FTIR) spectrogram of the taraxacum shape CuO hollow micron ball that makes with the inventive method.
Embodiment
Further specify the present invention below in conjunction with example.
Embodiment 1
With 2mmol cupric nitrate Cu (NO
3)
23H
2O, 6mmol urea CO (NH
2)
2Be dissolved in the 15mL distilled water, add 1g CTAB then, under magnetic agitation, make it form uniform jelly, jelly is moved in the stainless steel autoclave that volume is the 20mL inner liner polytetrafluoroethylene, the filling degree is 75%, is heated to 180 ℃ after the sealing and is incubated 6 hours respectively, naturally cools to room temperature then.With wherein black precipitate centrifugation, respectively wash 3 times with deionized water and dehydrated alcohol successively, obtained product in 4 hours in 80 ℃ of dryings.The product of gained black is directly observed (as Fig. 1) under scanning electron microscope, can find that a large amount of diameters generate at 5 to 10 microns left and right sides hollow balls.Can find out significantly that from the SEM photo of Fig. 2 this taraxacum inside configuration has a hollow cave, and these microns ball is assembled into by many small crystal zones.These crystal zone arranged verticals are pointed to same center in spherical surface.The XRD analysis of Fig. 3 shows that product is pure phase CuO.The FTIR collection of illustrative plates of Fig. 4 clearlys show the existence of CuO absorption peak.At 3455cm
-1And 1634cm
-1The absorption peak at place is respectively owing to the stretching vibration of product surface water molecule, the oh group on flexural vibration and surface.Do not detect other absorption peak, show that utilizing the prepared product of template hydrothermal method is pure CuO.
Embodiment 2
With 2mmol cupric nitrate Cu (NO
3)
23H
2O, 5mmol urea CO (NH
2)
2Be dissolved in the 15mL distilled water, add 1g CTAB then, under magnetic agitation, make it form uniform jelly, jelly is moved in the stainless steel autoclave that volume is the 20mL inner liner polytetrafluoroethylene, the filling degree is 75%, is heated to 180 ℃ after the sealing and is incubated 8 hours respectively, naturally cools to room temperature then.With wherein black precipitate centrifugation, respectively wash 3 times with deionized water and dehydrated alcohol successively, obtained product in 4 hours in 80 ℃ of dryings.The pattern of product, structure is all similar to embodiment 1 with the characteristic that becomes to grade.
With 2mmol cupric nitrate Cu (NO
3)
23H
2O, 7mmol urea CO (NH
2)
2Be dissolved in the 15mL distilled water, add 1g CTAB then, under magnetic agitation, make it form uniform jelly, jelly is moved in the stainless steel autoclave that volume is the 20mL inner liner polytetrafluoroethylene, the filling degree is 75%, is heated to 190 ℃ after the sealing and is incubated 6 hours respectively, naturally cools to room temperature then.With wherein black precipitate centrifugation, respectively wash 3 times with deionized water and dehydrated alcohol successively, obtained product in 4 hours in 80 ℃ of dryings.The pattern of product, structure is all similar to embodiment 1 with the characteristic that becomes to grade.
Embodiment 4
With 2mmol cupric nitrate Cu (NO
3)
23H
2O, 6mmol urea CO (NH
2)
2Be dissolved in the 15mL distilled water, add 1g CTAB then, under magnetic agitation, make it form uniform jelly, jelly is moved in the stainless steel autoclave that volume is the 20mL inner liner polytetrafluoroethylene, the filling degree is 75%, is heated to 190 ℃ after the sealing and is incubated 8 hours respectively, naturally cools to room temperature then.With wherein black precipitate centrifugation, respectively wash 3 times with deionized water and dehydrated alcohol successively, obtained product in 4 hours in 80 ℃ of dryings.The pattern of product, structure is all similar to embodiment 1 with the characteristic that becomes to grade.
Claims (4)
1. a method for preparing taraxacum shape cupric oxide hollow micron ball is characterized in that comprising the steps:
(1) cupric nitrate, urea are dissolved in the distilled water, form mixing solutions, in mixing solutions, add cetyl trimethylammonium bromide then, make it form uniform jelly; Wherein the mol ratio of cupric nitrate and urea is 1: 2～4; The total moles of cupric nitrate and urea and the mol ratio of distilled water are 1: 100～105; The cetyl trimethylammonium bromide quality that adds accounts for 4～10% of mixing solutions quality;
(2) then jelly is moved in the reactor, after the sealing reactant is heated to 180～190 ℃ and is incubated 6～8 hours respectively, naturally cool to room temperature then;
(3) reactant is precipitated, centrifugation, respectively wash 3 times with deionized water and dehydrated alcohol successively, obtaining the black product in 4 hours in 80 ℃ of dryings is taraxacum shape CuO hollow micron ball.
2. preparation method according to claim 1, the mol ratio that it is characterized in that cupric nitrate and urea is 1: 3.
3. preparation method according to claim 1 is characterized in that the cetyl trimethylammonium bromide quality that adds accounts for 5～7% of mixing solutions quality.
4. preparation method according to claim 1 is characterized in that the filling degree in reactor is 75%.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102641736A (en) * | 2012-03-19 | 2012-08-22 | 中国科学院过程工程研究所 | Sea urchin shaped copper oxide catalyst, as well as preparation method and application thereof |
| CN104108739A (en) * | 2013-04-22 | 2014-10-22 | 广东致卓精密金属科技有限公司 | Preparation method of particle size-controllable spherical copper oxide |
| CN104108738A (en) * | 2013-04-22 | 2014-10-22 | 广东致卓精密金属科技有限公司 | Method for using copper sulfate waste liquid to prepare high-purity spherical copper oxide |
| CN105396546A (en) * | 2015-12-16 | 2016-03-16 | 哈尔滨工业大学 | Method used for preparing inorganic hollow porous material based on water-ethanol or acetone two-phase interface |
| CN106698499A (en) * | 2017-01-20 | 2017-05-24 | 江苏先丰纳米材料科技有限公司 | Nano-spherical chain structure copper oxide and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1462720A (en) * | 2003-06-10 | 2003-12-24 | 东北师范大学 | Method for preparing nano tube of some metalloid oxides and metals with size and shape being controllable |
| CN101274749A (en) * | 2008-03-25 | 2008-10-01 | 大连理工大学 | Universal synthesis method for porous hollow metallic oxide |
| CN101332999A (en) * | 2008-07-30 | 2008-12-31 | 江南大学 | Method for preparing Cu2O or CuO hollow submicrospheres with particle diameter controllable by water phase soft template method |
-
2011
- 2011-03-28 CN CN 201110075748 patent/CN102139910A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1462720A (en) * | 2003-06-10 | 2003-12-24 | 东北师范大学 | Method for preparing nano tube of some metalloid oxides and metals with size and shape being controllable |
| CN101274749A (en) * | 2008-03-25 | 2008-10-01 | 大连理工大学 | Universal synthesis method for porous hollow metallic oxide |
| CN101332999A (en) * | 2008-07-30 | 2008-12-31 | 江南大学 | Method for preparing Cu2O or CuO hollow submicrospheres with particle diameter controllable by water phase soft template method |
Non-Patent Citations (1)
| Title |
|---|
| 《Journal of Solid State Chemistry》 20090212 Shunli Wang et al CTAB-assisted synthesis and photocatalytic property of CuO hollow microspheres 第1088-1089页 1-4 , 第182期 * |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102641736A (en) * | 2012-03-19 | 2012-08-22 | 中国科学院过程工程研究所 | Sea urchin shaped copper oxide catalyst, as well as preparation method and application thereof |
| CN104108739A (en) * | 2013-04-22 | 2014-10-22 | 广东致卓精密金属科技有限公司 | Preparation method of particle size-controllable spherical copper oxide |
| CN104108738A (en) * | 2013-04-22 | 2014-10-22 | 广东致卓精密金属科技有限公司 | Method for using copper sulfate waste liquid to prepare high-purity spherical copper oxide |
| CN104108738B (en) * | 2013-04-22 | 2015-08-19 | 广东致卓精密金属科技有限公司 | A kind of method being prepared high pure spherical cupric oxide by bluestone waste |
| CN105396546A (en) * | 2015-12-16 | 2016-03-16 | 哈尔滨工业大学 | Method used for preparing inorganic hollow porous material based on water-ethanol or acetone two-phase interface |
| CN105396546B (en) * | 2015-12-16 | 2018-01-30 | 哈尔滨工业大学 | A kind of method that inorganic hollow porous material is prepared based on water/ethanol or acetone two-phase interface |
| CN106698499A (en) * | 2017-01-20 | 2017-05-24 | 江苏先丰纳米材料科技有限公司 | Nano-spherical chain structure copper oxide and preparation method thereof |
| CN106698499B (en) * | 2017-01-20 | 2018-02-06 | 江苏先丰纳米材料科技有限公司 | A kind of nanosphere chain structure cupric oxide and preparation method thereof |
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Application publication date: 20110803 |