CN100385037C - Method for preparing nano copper oxide on surface of SiO2 - Google Patents
Method for preparing nano copper oxide on surface of SiO2 Download PDFInfo
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- CN100385037C CN100385037C CNB2005100616692A CN200510061669A CN100385037C CN 100385037 C CN100385037 C CN 100385037C CN B2005100616692 A CNB2005100616692 A CN B2005100616692A CN 200510061669 A CN200510061669 A CN 200510061669A CN 100385037 C CN100385037 C CN 100385037C
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- cupric oxide
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Abstract
The present invention discloses a method for preparing nanometer copper oxide on the surface of SiO2, which comprises the following steps that step 1, lower alcohol solution which has water volume fraction of 0.1 to 20% is prepared, and 0.1 to 25g of SiO2 and 0.005 to 10g of compounds of Cu are orderly added to every 100 mls of the lower alcohol solution during stirring, and fully and uniformly mixed; step 2, water solution or alcohol solution of inorganic bases with concentration of 1 to 300 g/L is prepared, dripped into the reaction system obtained in step 1 under the stirring condition to react for 10 minutes to 10 hours at a temperature of minus 5 to 70 DEG C, separated by centrifugation and dried to obtain the composite materials of the copper oxide on the surface of the SiO2. In the present invention, the nanometer CuO crystalline particles are prepared on the surface of the SiO2 through the reaction in binary mixed solution, and the agglomeration phenomenon of CuO particles is effectively avoided or reduced by utilizing the stabilization effect of the surface of the SiO2 on the CuO crystalline particles.
Description
Technical field
The present invention relates at SiO
2The method of surface preparation nano cupric oxide belongs to the nano composite material preparation field.
Background technology
Cupric oxide is a kind of broad-spectrum material, has been applied to fields such as catalyzer, superconducting material, thermoelectric material, sensing material, glass, pottery.In addition, cupric oxide also can be used as the burningrate catalyst of rocket propellant, and it not only can obviously improve combustion speed, the reduction pressure index of homogeneous propellant, and the AP compositepropellent is had catalytic effect preferably.A large amount of experiments show that cupric oxide has very big relation with its particle diameter on effect, and the more little then effect of its particle diameter is good more.Therefore, the preparation of nano cupric oxide has become one of focus of current functional materials research.
The preparation method of nano cupric oxide can be divided into physics method and chemical method two classes by character.Chemical method is a method commonly used in the nano powder preparation technology, and it is simple that it has equipment, is easy to amplify characteristics such as carrying out suitability for industrialized production.Chemical method is divided into the precipitator method, microemulsion method, hydrothermal method, solid reaction process, spray pyrolysis, microwave method, electrochemical process, laser steaming method, pure hot method etc. with fixed attention again.
Often there are serious, the deficiencies such as energy consumption is high, process complexity of reuniting in these methods, and simultaneously, these methods neither directly prepare cupric oxide on existing carrier, need follow-up recombining process.
Summary of the invention
The purpose of this invention is to provide a kind of particle diameter controlled at SiO
2The method of surface preparation nano cupric oxide.
Of the present invention at SiO
2The method of surface preparation nano cupric oxide may further comprise the steps:
1) volume fraction of preparation water is the low-alcohol solution of 0.1%-20%, stirs the SiO that adds 0.1-25g down by every 100ml low-alcohol solution successively
2With the compound of the Cu of 0.005-10g, thorough mixing is even;
2) compound concentration is the aqueous solution or the alcoholic solution of the mineral alkali of 1-300g/L, drop under the agitation condition in the reaction system that step 1) obtains, and reaction 10min-10hr, temperature of reaction is-5 ℃～70 ℃, centrifugation, drying obtains at SiO
2The matrix material of area load cupric oxide.
Among the present invention, said lower alcohol can be a kind of or its mixture in the alcohols isomers of methyl alcohol, ethanol, propyl alcohol, butanols and propyl alcohol, butanols; The compound of said Cu can be inorganic salt or the organic salt of Cu, as Cu (NO
3)
2, CuSO
4, CuCl
2, neutralized verdigris etc.; Mineral alkali can be NaOH, KOH etc.;
The present invention is by the reaction in the binary mixing solutions, at SiO
2Surface preparation nanometer CuO crystal grain utilizes SiO
2The agglomeration of CuO particle is effectively avoided or reduced in the surface to the stabilization of CuO crystal grain, and can pass through the crystallite size of parameter control CuO such as conditioned reaction temperature, each concentration of component, reaction times, feed rate.Characteristics such as this method has easy to operate, and synthesis technique is simple, and is pollution-free, product have that particle diameter is little, and the product purity height is evenly distributed, the advantage that specific surface area is big.
Description of drawings
Fig. 1 is the X ray diffracting spectrum of the sample that makes of the inventive method;
Fig. 2 is the electromicroscopic photograph of the sample that makes of the inventive method.
Embodiment
Further specify the present invention below in conjunction with example.
Embodiment 1
NaOH is dissolved in the ethanol, is mixed with the solution that concentration is 0.008g/ml.200ml dehydrated alcohol, 1.0ml water are added in the there-necked flask, add 0.5g SiO
2, under 25 ℃ water bath with thermostatic control environment, stir into uniform suspension.Add the 0.6g neutralized verdigris, constant temperature stirs 6hr.Under the agitation condition, 15ml NaOH ethanolic soln average rate is dripped in the there-necked flask, after continuing to stir 10hr, obtain solid precipitation by centrifugation with the speed of 1ml/min.Through after the washing with alcohol repeatedly, oven dry obtains product.Fig. 1 is the sample X ray diffracting spectrum, calculates as can be known according to the Scherrer formula, and its median size is 10nm.Fig. 2 is the electromicroscopic photograph of product, and as seen from the figure, the CuO particle is scattered in network-like silica gel surface well.
Embodiment 2
NaOH is dissolved in the methyl alcohol, is mixed with the solution that concentration is 0.008g/ml.200ml anhydrous methanol, 1.0ml water are added in the there-necked flask, add 0.5g SiO
2, under 40 ℃ water bath with thermostatic control environment, stir into uniform suspension.Add 0.6g Cu (NO
3)
2, constant temperature stirs 6hr.Under the agitation condition, 15ml NaOH methanol solution average rate is dripped in the there-necked flask, after continuing to stir 2hr, obtain solid precipitation by centrifugation with the speed of 1ml/min.Through after the washing with alcohol repeatedly, oven dry obtains product.X-ray diffraction analysis calculates as can be known according to the Scherrer formula, and its median size is 8nm.
Embodiment 3
NaOH is dissolved in the Virahol, is mixed with the solution that concentration is 0.001g/ml.200ml anhydrous isopropyl alcohol, 2ml water are added in the there-necked flask, add 0.5g SiO
2, under-5 ℃ water bath with thermostatic control environment, stir into uniform suspension.Add 0.01g CuCl
2, constant temperature stirs 48hr.Under the agitation condition, 40ml NaOH aqueous isopropanol average rate is dripped in the there-necked flask, after continuing to stir 2hr, obtain solid precipitation by centrifugation with the speed of 1ml/min.Through after the washing with alcohol repeatedly, oven dry obtains product.X-ray diffraction analysis calculates as can be known according to the Scherrer formula, and its median size is 6nm.
Embodiment 4
NaOH is dissolved in the ethanol, is mixed with the solution that concentration is 0.3g/ml.200ml dehydrated alcohol, 2ml water are added in the there-necked flask, add 50g SiO
2, under 20 ℃ water bath with thermostatic control environment, stir into uniform suspension.Add the 20g neutralized verdigris, constant temperature stirs 6hr.Under the agitation condition, 15ml NaOH ethanolic soln average rate is dripped in the there-necked flask, after continuing to stir 10hr, obtain solid precipitation by centrifugation with the speed of 1ml/min.Through after the washing with alcohol repeatedly, oven dry obtains product.X-ray diffraction analysis calculates as can be known according to the Scherrer formula, and its median size is 22nm.
Embodiment 5
KOH is dissolved in the water, is mixed with the solution that concentration is 0.1g/ml.200ml dehydrated alcohol, 0.2ml water are added in the there-necked flask, add 1g SiO
2, under 70 ℃ water bath with thermostatic control environment, stir into uniform suspension.Add 1.0g CuSO
4, constant temperature stirs 10min.Under the agitation condition, 3ml KOH aqueous solution average rate is dripped in the there-necked flask, after continuing to stir 10min, obtain solid precipitation by centrifugation with the speed of 1ml/min.Through after the washing with alcohol repeatedly, oven dry obtains product.X-ray diffraction analysis calculates as can be known according to the Scherrer formula, and its median size is 17nm.
Claims (4)
1. at SiO
2The method of surface preparation nano cupric oxide may further comprise the steps:
1) volume fraction of preparation water is the low-alcohol solution of 0.1%-20%, stirs the SiO that adds 0.1-25g down by every 100ml low-alcohol solution successively
2With the compound of the Cu of 0.005-10g, thorough mixing is even;
2) compound concentration is the aqueous solution or the alcoholic solution of the mineral alkali of 1-300g/L, drop under the agitation condition in the reaction system that step 1) obtains, and reaction 10min-10hr, temperature of reaction is-5 ℃～70 ℃, centrifugation, drying obtains at SiO
2The matrix material of area load cupric oxide.
2. according to claim 1 at SiO
2The method of surface preparation nano cupric oxide is characterized in that said lower alcohol is a kind of or its mixture in the alcohols isomers of methyl alcohol, ethanol, propyl alcohol, butanols and propyl alcohol, butanols.
3. according to claim 1 at SiO
2The method of surface preparation nano cupric oxide, the compound that it is characterized in that said Cu are Cu (NO
3)
2, CuSO
4, CuCl
2Or neutralized verdigris.
4. according to claim 1 at SiO
2The method of surface preparation nano cupric oxide is characterized in that said mineral alkali is NaOH or KOH.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100616692A CN100385037C (en) | 2005-11-22 | 2005-11-22 | Method for preparing nano copper oxide on surface of SiO2 |
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| CNB2005100616692A CN100385037C (en) | 2005-11-22 | 2005-11-22 | Method for preparing nano copper oxide on surface of SiO2 |
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| CN1776012A CN1776012A (en) | 2006-05-24 |
| CN100385037C true CN100385037C (en) | 2008-04-30 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103170328A (en) * | 2013-03-04 | 2013-06-26 | 浙江大学 | Low-temperature denitration catalyst for smoke and preparation method thereof |
| CN104841429B (en) * | 2015-04-05 | 2017-12-26 | 浙江大学 | A kind of synthesising gas systeming carbinol carried copper-base catalyst and preparation method thereof |
| CN112279291A (en) * | 2020-11-11 | 2021-01-29 | 湖南师范大学 | Nano copper oxide and preparation method and application thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| SU437528A1 (en) * | 1973-03-09 | 1974-07-30 | Невиномысский Химический Комбинат | The method of preparation of the catalyst for the hydrogenation of crotonaldehyde to n-butyl alcohol |
| JPH03242543A (en) * | 1990-02-20 | 1991-10-29 | Seiko Epson Corp | Moisture sensor |
| CN1355138A (en) * | 2000-12-01 | 2002-06-26 | 朱强 | Process for preparing nano material |
| CN1539740A (en) * | 2003-04-22 | 2004-10-27 | 中南大学 | Method for preparing composite material of Nano crystal between copper oxide and indium oxide |
-
2005
- 2005-11-22 CN CNB2005100616692A patent/CN100385037C/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| SU437528A1 (en) * | 1973-03-09 | 1974-07-30 | Невиномысский Химический Комбинат | The method of preparation of the catalyst for the hydrogenation of crotonaldehyde to n-butyl alcohol |
| JPH03242543A (en) * | 1990-02-20 | 1991-10-29 | Seiko Epson Corp | Moisture sensor |
| CN1355138A (en) * | 2000-12-01 | 2002-06-26 | 朱强 | Process for preparing nano material |
| CN1539740A (en) * | 2003-04-22 | 2004-10-27 | 中南大学 | Method for preparing composite material of Nano crystal between copper oxide and indium oxide |
Non-Patent Citations (2)
| Title |
|---|
| SiO2/CuO复合纳米粒子添加剂的摩擦学和自修复性能研究. 董凌，陈国需，李华峰，方建华.润滑油，第20卷第5期. 2005 |
| SiO2/CuO复合纳米粒子添加剂的摩擦学和自修复性能研究. 董凌，陈国需，李华峰，方建华.润滑油，第20卷第5期. 2005 * |
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