CN103408056A - Method for preparing nanometer copper oxide by adopting liquid phase precipitation method - Google Patents
Method for preparing nanometer copper oxide by adopting liquid phase precipitation method Download PDFInfo
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- CN103408056A CN103408056A CN2013103427752A CN201310342775A CN103408056A CN 103408056 A CN103408056 A CN 103408056A CN 2013103427752 A CN2013103427752 A CN 2013103427752A CN 201310342775 A CN201310342775 A CN 201310342775A CN 103408056 A CN103408056 A CN 103408056A
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Abstract
The invention discloses a method for preparing nanometer copper oxide by adopting a liquid phase precipitation method, and particularly relates to a method for preparing nanometer copper oxide by taking calcium lignosulphonate as a surfactant. The method comprises the following steps: by changing adding amount of a NaOH solution, taking the calcium lignosulphonate as the surfactant and utilizing the liquid phase precipitation method, nanometer copper oxide is prepared. The lignosulfonate, which is low in cost, non-toxic and easy to obtain, is taken as the surfactant, so that the technology for controllable preparation of nanometer copper oxide is achieved, the dispersibility problem existing widely in nanometer materials is solved, and application performance and catalytic performance of nanometer copper oxide are improved. The method prepares nanometer copper oxide by adopting the liquid phase precipitation method, and has the advantages of simple equipment, easily available raw materials, high purity, good uniformity, control accuracy in chemical composition and the like as compared with other methods.
Description
Technical field
The present invention relates to a kind of method that liquid-phase precipitation method prepares nano cupric oxide, the sulfonated lignin of particularly take prepare the method for nano cupric oxide as tensio-active agent.
Background technology
Calcium lignin sulphonate is a kind of polycomponent high molecular polymer anion surfactant, and molecular weight generally, between 800 ~ 10000, has very strong dispersiveness, cohesiveness, chelating.Water-soluble, but be insoluble to any common organic solvent.The lignosulfonic acid calcium product extensively has been used as cement water reducing agent, agricultural chemicals suspension agent, ceramic idiosome toughener, coal water slurry dispersing agent, leather tanning agent, binder for fire-resistant materials, pelletizing of carbon black agent etc.
Nano cupric oxide is a kind of very important inorganic nano material, and in recent years, people are growing on and on to its research.This is mainly because cupric oxide has the property that some other metal oxides do not have.Its band gap is approximately 1.4ev, is a kind of good semiconductor material.Therefore copper oxide nano material can be used as catalyzer, battery material, high temperature superconducting materia, photochromics, gas sensor, magnetic and deposits equipment etc.
Liquid phase method is to select one or more suitable soluble metal salts, by prepared material, form metering and be mixed with solution, make each element be the lewis' acid state, select again a kind of suitable precipitation agent or by operations such as evaporation, distillation, hydrolysis, make the metal ion precipitation from homogeneous solution or crystallize out, finally precipitation or exsiccation or thermal degradation being obtained to required material powder.The present invention uses the Liquid preparation methods nano cupric oxide, compares with additive method that to have equipment simple, and raw material easily obtains, and purity is high, good uniformity, the advantages such as chemical constitution precise control.
Summary of the invention
The objective of the invention is to adopt sulfonated lignin is tensio-active agent, synthesizes and calcines to prepare nano cupric oxide through differing temps by liquid phase method, and technique is simple, and raw material is easy to obtain, with low cost, of reduced contamination, is suitable for suitability for industrialized production.
Technical scheme of the present invention is as follows:
Under A, room temperature, getting concentration is 0.1-0.4 mol ﹒ L
-1CuSO
4Solution, by every 100mL CuSO
4Solution adds the 0.5-2g sulfonated lignin, and stirring and dissolving, under continuously stirring, by every 100mLCuSO
4Solution splashes into 10-40mL 2 mol ﹒ L
-1NaOH solution;
B, above-mentioned solution is refluxed at 50-90 ℃ of temperature 6-10h, be cooled to room temperature;
C, by the centrifugation of gained precipitation mixture, precipitate with deionized water is cleaned 3 times, then with dehydrated alcohol, cleans 3 times centrifugation;
D, the solid after separating are put into the dry 12h of thermostatic drying chamber, and the temperature of described thermostatic drying chamber is 60 ℃;
E, finally by dried solid in 300-500 ℃ of roasting temperature 2-3h.
In a more excellent open example of the present invention, described mantoquita is CuSO
4.
In a more excellent open example of the present invention, described sulfonated lignin are calcium lignin sulphonates.
In a more excellent open example of the present invention, step B, for above-mentioned solution is refluxed at 60-80 ℃ of temperature 6-10h, is cooled to room temperature.
This experiment reagent used is all analytical pure, is commercially available.
Beneficial effect
The present invention utilizes, and sulfonated lignin inexpensive, nontoxic, that be easy to get are tensio-active agent, realize the controlled technology of preparing of nano cupric oxide, solve the ubiquitous dispersion problem of nano material, improved application performance and the catalytic performance of nano cupric oxide, the present invention uses the Liquid preparation methods nano cupric oxide, compares with additive method that to have equipment simple, raw material easily obtains, purity is high, good uniformity, the advantages such as chemical constitution precise control.
The accompanying drawing explanation
The X ray diffracting spectrum of Fig. 1 sample (XRD), be the XRD figure spectrum of embodiment 1 sample.
Embodiment
The present invention will be further described below in conjunction with concrete embodiment, so that those skilled in the art understand the present invention better, but the present invention is not limited to following examples.
Embodiment 1
Under room temperature, getting concentration is 0.1 mol ﹒ L
-1CuSO
4Solution 100mL, add calcium lignin sulphonate 1g, and stirring and dissolving, under continuously stirring, dropwise splashes into 2 mol ﹒ L
-1NaOH solution 10mL, at 50 ℃ of lower reflux 6h, be cooled to room temperature, by the centrifugation of gained precipitation mixture, precipitate with deionized water is cleaned 3 times, then cleans 3 times with dehydrated alcohol, centrifugation, solid after separation is put into 60 ℃ of dry 12h of thermostatic drying chamber, then by dried solid in 300 ℃ of roasting temperature 2h, namely obtain black nano oxidation zinc-copper.Sample XRD figure such as Fig. 1.
Embodiment 2
Under room temperature, getting concentration is 0.4mol ﹒ L
-1CuSO
4Solution 100mL, add calcium lignin sulphonate 2g, and stirring and dissolving, under continuously stirring, dropwise splashes into 2 mol ﹒ L
-1NaOH solution 40 mL, at 90 ℃ of lower reflux 10h, be cooled to room temperature, by the centrifugation of gained precipitation mixture, precipitate with deionized water is cleaned 3 times, then cleans 3 times with dehydrated alcohol, centrifugation, solid after separation is put into 60 ℃ of dry 12h of thermostatic drying chamber, then by dried solid in 300 ℃ of roasting temperature 3h, namely obtain black nano oxidation zinc-copper.
Embodiment 3
Under room temperature, getting concentration is 0.1 mol ﹒ L
-1CuSO
4Solution 100mL, add calcium lignin sulphonate 0.5g, and stirring and dissolving, under continuously stirring, dropwise splashes into 2 mol ﹒ L
-1NaOH solution 20 mL, at 80 ℃ of lower reflux 10h, be cooled to room temperature, by the centrifugation of gained precipitation mixture, precipitate with deionized water is cleaned 3 times, then cleans 3 times with dehydrated alcohol, centrifugation, solid after separation is put into 60 ℃ of dry 12h of thermostatic drying chamber, then by dried solid in 500 ℃ of roasting temperature 2h, namely obtain black nano oxidation zinc-copper.
Embodiment 4
Under room temperature, getting concentration is 0.4 mol ﹒ L
-1CuSO
4Solution 100mL, add calcium lignin sulphonate 1g, and stirring and dissolving, under continuously stirring, dropwise splashes into 2 mol ﹒ L
-1NaOH solution 40 mL, at 70 ℃ of lower reflux 10h, be cooled to room temperature, by the centrifugation of gained precipitation mixture, precipitate with deionized water is cleaned 3 times, then cleans 3 times with dehydrated alcohol, centrifugation, solid after separation is put into 60 ℃ of dry 12h of thermostatic drying chamber, then by dried solid in 300 ℃ of roasting temperature 3h, namely obtain black nano oxidation zinc-copper.
Embodiment 5
Under room temperature, getting concentration is 0.2 mol ﹒ L
-1CuSO
4Solution 100mL, add calcium lignin sulphonate 0.5g, and stirring and dissolving, under continuously stirring, dropwise splashes into 2 mol ﹒ L
-1NaOH solution 30 mL, at 60 ℃ of lower reflux 6h, be cooled to room temperature, by the centrifugation of gained precipitation mixture, precipitate with deionized water is cleaned 3 times, then cleans 3 times with dehydrated alcohol, centrifugation, solid after separation is put into 60 ℃ of dry 12h of thermostatic drying chamber, then by dried solid in 300 ℃ of roasting temperature 2h, namely obtain black nano oxidation zinc-copper.
Claims (4)
1. a liquid-phase precipitation method prepares the method for nano cupric oxide, carries out according to following step:
Under A, room temperature, getting concentration is 0.1-0.4 mol ﹒ L
-1CuSO
4Solution, by every 100mL CuSO
4Solution adds the 0.5-2g sulfonated lignin, and stirring and dissolving, under continuously stirring, by every 100mLCuSO
4Solution splashes into 10-40mL 2 mol ﹒ L
-1NaOH solution;
B, above-mentioned solution is refluxed at 50-90 ℃ of temperature 6-10h, be cooled to room temperature;
C, by the centrifugation of gained precipitation mixture, precipitate with deionized water is cleaned 3 times, then with dehydrated alcohol, cleans 3 times centrifugation;
D, the solid after separating are put into the dry 12h of thermostatic drying chamber, and the temperature of described thermostatic drying chamber is 60 ℃;
E, finally by dried solid in 300-500 ℃ of roasting temperature 2-3h.
2. a kind of liquid-phase precipitation method according to claim 1 prepares the method for nano cupric oxide, it is characterized in that described mantoquita is CuSO
4.
3. a kind of liquid-phase precipitation method according to claim 1 prepares the method for nano cupric oxide, it is characterized in that described sulfonated lignin are calcium lignin sulphonates.
4. a kind of liquid-phase precipitation method according to claim 1 prepares the method for nano cupric oxide, it is characterized in that step B, for above-mentioned solution being refluxed to 6-10h at 60-80 ℃ of temperature, is cooled to room temperature.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103864134A (en) * | 2014-03-07 | 2014-06-18 | 上海交通大学 | Preparation method of chiral nanometer copper oxide with optical activity |
| CN104743610A (en) * | 2015-03-12 | 2015-07-01 | 江苏大学 | Method for preparing nano bismuth oxide by using liquid phase precipitation method |
| CN107381909A (en) * | 2017-09-14 | 2017-11-24 | 安徽工程大学 | A kind of processing method of aniline waste water |
| CN107413354A (en) * | 2017-09-12 | 2017-12-01 | 山东师范大学 | A kind of preparation method for the cupric oxide nano composite for loading silver |
| CN113603130A (en) * | 2021-08-17 | 2021-11-05 | 湖南德邦生物科技有限公司 | Preparation method for crystal modification in basic copper chloride synthesis |
| CN114291837A (en) * | 2021-12-30 | 2022-04-08 | 宁夏京成天宝科技有限公司 | Preparation method of antibiotic substitute |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101407332A (en) * | 2007-10-12 | 2009-04-15 | 新疆大学 | Hydro-thermal synthesis method for cupric oxide nano-rod |
| CN102941110A (en) * | 2012-11-16 | 2013-02-27 | 江苏大学 | Preparation method of nano-zinc oxide composite photocatalyst |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101407332A (en) * | 2007-10-12 | 2009-04-15 | 新疆大学 | Hydro-thermal synthesis method for cupric oxide nano-rod |
| CN102941110A (en) * | 2012-11-16 | 2013-02-27 | 江苏大学 | Preparation method of nano-zinc oxide composite photocatalyst |
Non-Patent Citations (2)
| Title |
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| DAQIANG GAO, ET AL.: "Vacancy-Mediated Magnetism in Pure Copper Oxide Nanoparticles", 《NANOSCALE RESEARCH LETTERS》 * |
| SATHISH REDDY, ET AL.: "CuO nanoparticle sensor for the electrochemical determination of dopamine", 《ELECTROCHIMICA ACTA》 * |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103864134A (en) * | 2014-03-07 | 2014-06-18 | 上海交通大学 | Preparation method of chiral nanometer copper oxide with optical activity |
| CN103864134B (en) * | 2014-03-07 | 2016-07-06 | 上海交通大学 | A kind of preparation method with optically active chirality nano cupric oxide |
| CN104743610A (en) * | 2015-03-12 | 2015-07-01 | 江苏大学 | Method for preparing nano bismuth oxide by using liquid phase precipitation method |
| CN107413354A (en) * | 2017-09-12 | 2017-12-01 | 山东师范大学 | A kind of preparation method for the cupric oxide nano composite for loading silver |
| CN107381909A (en) * | 2017-09-14 | 2017-11-24 | 安徽工程大学 | A kind of processing method of aniline waste water |
| CN113603130A (en) * | 2021-08-17 | 2021-11-05 | 湖南德邦生物科技有限公司 | Preparation method for crystal modification in basic copper chloride synthesis |
| CN114291837A (en) * | 2021-12-30 | 2022-04-08 | 宁夏京成天宝科技有限公司 | Preparation method of antibiotic substitute |
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