CN100376482C - Method for preparing nanometer copper nickel compoilite oxide - Google Patents
Method for preparing nanometer copper nickel compoilite oxide Download PDFInfo
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- CN100376482C CN100376482C CNB200610025292XA CN200610025292A CN100376482C CN 100376482 C CN100376482 C CN 100376482C CN B200610025292X A CNB200610025292X A CN B200610025292XA CN 200610025292 A CN200610025292 A CN 200610025292A CN 100376482 C CN100376482 C CN 100376482C
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Abstract
The present invention discloses a preparation method of nanometer copper-nickel composite oxide, which comprises the following steps: adopting copper acetate, nickelous acetate, citric acid and polyethylene glycol as principal raw materials; preparing sol and gel with a sol-gel method; preparing nanometer composite oxide by treating the sol and gel with the processes of solvent elimination, drying, high temperature roasting, etc. The chemical elements in the whole raw materials selected by the present invention only contain C, H, O instead of N element contained in the raw materials with other methods so as to avoid the formation of oxynitride in the preparation process, thereby having an environment-friendly preparation process.
Description
Technical field
The present invention relates to the preparation method of nanometer copper nickel oxide compound, relate in particular to a kind of method that adopts with the feedstock production nanometer copper nickel compoilite oxide of nonnitrogenous element.
Background technology
Nano material is because the designability of its excellent comprehensive performances and performance is widely used in a plurality of fields of the daily production of people, life, especially at catalytic field.The copper base oxide catalyst is the custom catalysts of CO, hydro carbons complete oxidation, because its good catalytic performance might replace noble metal catalyst.The copper-base composite oxidate recent researches is also more, the Cu-Ni-O composite oxides, and being applied in the reactions such as 1-methoxyl group-2-propyl alcohol oxidation synthesizing methoxy acetone, the synthetic n-Butyl Amine 99 of propyl carbinol, hydramine catalytic oxidative dehydrogenation all has greater activity.
The nano-copper base composite oxides are owing to possess the distinctive effect of nanometer, and are better than traditional copper nickel oxide performance, can prepare more efficiently catalyzer etc., have wide range of applications, and have good market outlook.The sol-gel method of making part with citric acid is the method that development in recent years plays the new synthesis of nano ultrafine particle of rice, with this method synthesizing composite oxide particulate, because each component is mixed mutually with solution state, at a lower temperature, can make by the oxide network micro-area composition cloth of the whole process of solution-sol-gel even, be the preparation composite oxides proper method.The report of relevant both at home and abroad preparation nanometer copper nickel compoilite oxide is less, and CN1594110 has reported the preparation method of the oxide compound of nickel.Method described in the relevant document exist desired raw material wide in variety, in preparation process, easily produce deficiency such as oxynitrides.
Summary of the invention
The technical issues that need to address of the present invention are the methods that disclose the feedstock production nanometer copper nickel compoilite oxide of the nonnitrogenous element of a kind of usefulness, to overcome the defective that prior art exists, satisfy the needs of the parties concerned.
Method of the present invention comprises the steps:
Add Cu (Ac) in the solvent
23H
2O and Ni (Ac)
24H
2O, Cu, Ni mol ratio are 1/0.01～100, the control solution temperature is 40～60 ℃, adds polyglycol surfactants then, stirring and dissolving;
In solution, add weight concentration again and be 0.5～5% citric acid ethanolic soln, stir 1～3h, form colloidal sol, filtrations, room temperature ageing, 100～110 ℃ of oven dry, 230～400 ℃ of roasting 1～5h, grind after acquisition Cu-Ni composite oxides;
Said solvent comprises methyl alcohol, ethanol, propyl alcohol, Virahol is a kind of or its combination;
In the solvent, Cu (Ac)
23H
2The bulking value concentration of O is 0.01～1.0g/ml;
The add-on of polyoxyethylene glycol is Cu (Ac)
23H
210～60% of O weight;
The add-on of citric acid ethanolic soln is 10～200% of a solvent volume;
All nonnitrogenous element in the various raw materials involved in the present invention has been avoided producing waste gas or the waste liquid that contains oxynitrides in preparation process, helps environment protection, and preparation process is environmentally friendly.
Description of drawings
Fig. 1 is the electromicroscopic photograph of embodiment.
Embodiment
Embodiment 1
In the 80ml dehydrated alcohol, add 1.50 gram Cu (Ac)
23H
2O and 1.87 gram Ni (Ac)
24H
2O, Cu, Ni mol ratio are 1/1, the control solution temperature is 50 ℃, adds 0.5 gram polyglycol surfactants then, by mechanical stirring and ultrasonicly make it abundant dissolving.
In solution, slowly add the 100ml weight concentration again and be 1% citric acid ethanolic soln, form colloidal sol after continuing to stir 2h, filtrations, room temperature ageing, 105 ℃ of oven dry, roasting 3h, grind after acquisition Cu-Ni combined oxidation matter sample.The sample that takes a morsel carries out TEM (transmission electron microscope) analysis, as Fig. 1.
Claims (5)
1. prepare the method for nanometer copper nickel compoilite oxide, it is characterized in that, comprise the steps:
Add Cu (Ac) in the solvent
23H
2O and Ni (Ac)
24H
2O, Cu, Ni mol ratio are 1/0.01～100, add polyglycol surfactants then, stirring and dissolving;
In solution, add weight concentration again and be 0.5～5% citric acid ethanolic soln, stir 1～3h, form colloidal sol, filtrations, room temperature ageing, 100～110 ℃ of oven dry, 230～400 ℃ of roasting 1～5h, grind after acquisition Cu-Ni composite oxides;
Said solvent is a kind of or its combination in methyl alcohol, ethanol, propyl alcohol or the Virahol.
2. method according to claim 1 is characterized in that, the control solution temperature is 40～60 ℃.
3. method according to claim 1 is characterized in that, in the solvent, and Cu (Ac)
23H
2The bulking value concentration of O is 0.01～1.0g/ml.
4. method according to claim 1 is characterized in that, the add-on of polyoxyethylene glycol is Cu (Ac)
23H
2O and Ni (Ac)
24H
210～60% of O gross weight.
5. method according to claim 1 is characterized in that, the add-on of citric acid ethanolic soln is 10～200% of a solvent volume.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB200610025292XA CN100376482C (en) | 2006-03-30 | 2006-03-30 | Method for preparing nanometer copper nickel compoilite oxide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB200610025292XA CN100376482C (en) | 2006-03-30 | 2006-03-30 | Method for preparing nanometer copper nickel compoilite oxide |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1830801A CN1830801A (en) | 2006-09-13 |
| CN100376482C true CN100376482C (en) | 2008-03-26 |
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ID=36993327
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB200610025292XA Expired - Fee Related CN100376482C (en) | 2006-03-30 | 2006-03-30 | Method for preparing nanometer copper nickel compoilite oxide |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106952828A (en) * | 2017-03-28 | 2017-07-14 | 青岛大学 | A kind of preparation method of p-type metal oxide thin-film transistor |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CZ302445B6 (en) * | 2010-01-07 | 2011-05-18 | Ceské vysoké ucení technické - FJFI-katedra jaderné chemie | Process for preparing nanoparticles of nickel monooxide of high catalytic activity |
| CN102557670A (en) * | 2010-12-24 | 2012-07-11 | 中国科学院兰州化学物理研究所 | Preparation method of aluminum oxide and titanium oxide compound nanometer powder body |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5955219A (en) * | 1996-11-29 | 1999-09-21 | Sharp Kabushiki Kaisha | Lithium nickel copper composite oxide and its production process and use |
| CN1513596A (en) * | 2003-07-07 | 2004-07-21 | 深圳大学 | Nano-copper-lead composite oxide powder and its preparation method |
-
2006
- 2006-03-30 CN CNB200610025292XA patent/CN100376482C/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5955219A (en) * | 1996-11-29 | 1999-09-21 | Sharp Kabushiki Kaisha | Lithium nickel copper composite oxide and its production process and use |
| CN1513596A (en) * | 2003-07-07 | 2004-07-21 | 深圳大学 | Nano-copper-lead composite oxide powder and its preparation method |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106952828A (en) * | 2017-03-28 | 2017-07-14 | 青岛大学 | A kind of preparation method of p-type metal oxide thin-film transistor |
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| CN1830801A (en) | 2006-09-13 |
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Granted publication date: 20080326 Termination date: 20120330 |