CN103408056B - A kind of liquid-phase precipitation method prepares the method for nano cupric oxide - Google Patents
A kind of liquid-phase precipitation method prepares the method for nano cupric oxide Download PDFInfo
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- CN103408056B CN103408056B CN201310342775.2A CN201310342775A CN103408056B CN 103408056 B CN103408056 B CN 103408056B CN 201310342775 A CN201310342775 A CN 201310342775A CN 103408056 B CN103408056 B CN 103408056B
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- cupric oxide
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Abstract
The invention discloses a kind of method that liquid-phase precipitation method prepares nano cupric oxide, in particular to taking calcium lignin sulphonate as the method that tensio-active agent liquid phase prepares nano cupric oxide, step is: by changing the difference of NaOH solution add-on, take calcium lignin sulphonate as tensio-active agent, use liquid-phase precipitation method to prepare nano cupric oxide.Be tensio-active agent with sulfonated lignin that are inexpensive, nontoxic, that be easy to get, realize the controlled synthesis technology of nano cupric oxide, solve the ubiquitous dispersion problem of nano material, improve application performance and the catalytic performance of nano cupric oxide.The present invention uses liquid-phase precipitation method to prepare nano cupric oxide, has equipment simple, the advantages such as raw material easily obtains, and purity is high, good uniformity, chemical constitution precise control compared with additive method.
Description
Technical field
The present invention relates to a kind of method that liquid-phase precipitation method prepares nano cupric oxide, is particularly the method that nano cupric oxide prepared by tensio-active agent with sulfonated lignin.
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, sequestering.Water-soluble, but be insoluble to any common organic solvent.Lignosulfonic acid calcium product has extensively 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, the research of people to it is growing on and on.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 well semiconductor material.Therefore copper oxide nano material can deposit equipment etc. as catalyzer, battery material, high temperature superconducting materia, photochromics, gas sensor, magnetic.
Liquid phase method selects one or more suitable soluble metal salts, solution is mixed with by the metering of prepared material composition, each element is made to be lewis' acid state, select a kind of suitable precipitation agent again or pass through the operations such as evaporation, distillation, hydrolysis, make metal ion precipitation from homogeneous solution or crystallize out, finally precipitation or exsiccation or thermal degradation being obtained required material powder.The present invention uses Liquid preparation methods nano cupric oxide, has equipment simple, the advantages such as raw material easily obtains, and purity is high, good uniformity, chemical constitution precise control compared with additive method.
Summary of the invention
The object of the invention is to adopt sulfonated lignin to be tensio-active agent, synthesized by liquid phase method and prepare nano cupric oxide through differing temps calcining, 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:
Getting concentration under A, room temperature is 0.1-0.4mol ﹒ L
-1cuSO
4solution, by every 100mLCuSO
4solution adds 0.5-2g sulfonated lignin, stirring and dissolving, with continuous stirring, by every 100mLCuSO
4solution instillation 10-40mL2mol ﹒ L
-1naOH solution;
B, reflux above-mentioned solution at 50-90 DEG C of temperature 6-10h, is cooled to room temperature;
C, by the centrifugation of gained precipitation mixture, precipitate with deionized water cleans 3 times, then uses washes of absolute alcohol 3 times, centrifugation;
D, by be separated after solid put into the dry 12h of thermostatic drying chamber, the temperature of described thermostatic drying chamber is 60 DEG C;
E, finally by dried solid in 300-500 DEG C of roasting temperature 2-3h.
In a more excellent disclosed example of the present invention, described described mantoquita is CuSO
4.
In a more excellent disclosed example of the present invention, described sulfonated lignin are calcium lignin sulphonates.
In a more excellent disclosed example of the present invention, step B is the 6-10h that refluxed at 60-80 DEG C of temperature by above-mentioned solution, is cooled to room temperature.
This is tested reagent used and is all analytical pure, is commercially available.
beneficial effect
The present invention utilizes sulfonated lignin that are inexpensive, nontoxic, that be easy to get to be tensio-active agent, realize the controlled synthesis technology of nano cupric oxide, solve the ubiquitous dispersion problem of nano material, improve application performance and the catalytic performance of nano cupric oxide, the present invention uses Liquid preparation methods nano cupric oxide, has equipment simple compared with additive method, raw material easily obtains, the advantages such as purity is high, good uniformity, chemical constitution precise control.
Accompanying drawing explanation
The X ray diffracting spectrum (XRD) of Fig. 1 sample, for the XRD figure of embodiment 1 sample is composed.
Embodiment
Below in conjunction with concrete embodiment, the present invention will be further described, and to make those skilled in the art understand the present invention better, but the present invention is not limited to following examples.
embodiment 1
Getting concentration under room temperature is 0.1mol ﹒ L
-1cuSO
4solution 100mL, adds calcium lignin sulphonate 1g, stirring and dissolving, with continuous stirring, dropwise instills 2mol ﹒ L
-1naOH solution 10mL, reflux 6h at 50 DEG C, be cooled to room temperature, by the centrifugation of gained precipitation mixture, precipitate with deionized water cleans 3 times, then uses washes of absolute alcohol 3 times, centrifugation, thermostatic drying chamber 60 DEG C of dry 12h put into by solid after separation, then by dried solid in 300 DEG C of roasting temperature 2h, namely obtain black nano oxidation zinc-copper.Sample XRD figure is as Fig. 1.
embodiment 2
Getting concentration under room temperature is 0.4mol ﹒ L
-1cuSO
4solution 100mL, adds calcium lignin sulphonate 2g, stirring and dissolving, with continuous stirring, dropwise instills 2mol ﹒ L
-1naOH solution 40mL, reflux 10h at 90 DEG C, be cooled to room temperature, by the centrifugation of gained precipitation mixture, precipitate with deionized water cleans 3 times, then uses washes of absolute alcohol 3 times, centrifugation, thermostatic drying chamber 60 DEG C of dry 12h put into by solid after separation, then by dried solid in 300 DEG C of roasting temperature 3h, namely obtain black nano oxidation zinc-copper.
embodiment 3
Getting concentration under room temperature is 0.1mol ﹒ L
-1cuSO
4solution 100mL, adds calcium lignin sulphonate 0.5g, stirring and dissolving, with continuous stirring, dropwise instills 2mol ﹒ L
-1naOH solution 20mL, reflux 10h at 80 DEG C, be cooled to room temperature, by the centrifugation of gained precipitation mixture, precipitate with deionized water cleans 3 times, then uses washes of absolute alcohol 3 times, centrifugation, thermostatic drying chamber 60 DEG C of dry 12h put into by solid after separation, then by dried solid in 500 DEG C of roasting temperature 2h, namely obtain black nano oxidation zinc-copper.
embodiment 4
Getting concentration under room temperature is 0.4mol ﹒ L
-1cuSO
4solution 100mL, adds calcium lignin sulphonate 1g, stirring and dissolving, with continuous stirring, dropwise instills 2mol ﹒ L
-1naOH solution 40mL, reflux 10h at 70 DEG C, be cooled to room temperature, by the centrifugation of gained precipitation mixture, precipitate with deionized water cleans 3 times, then uses washes of absolute alcohol 3 times, centrifugation, thermostatic drying chamber 60 DEG C of dry 12h put into by solid after separation, then by dried solid in 300 DEG C of roasting temperature 3h, namely obtain black nano oxidation zinc-copper.
embodiment 5
Getting concentration under room temperature is 0.2mol ﹒ L
-1cuSO
4solution 100mL, adds calcium lignin sulphonate 0.5g, stirring and dissolving, with continuous stirring, dropwise instills 2mol ﹒ L
-1naOH solution 30mL, reflux 6h at 60 DEG C, be cooled to room temperature, by the centrifugation of gained precipitation mixture, precipitate with deionized water cleans 3 times, then uses washes of absolute alcohol 3 times, centrifugation, thermostatic drying chamber 60 DEG C of dry 12h put into by solid after separation, then by dried solid in 300 DEG C of roasting temperature 2h, namely obtain black nano oxidation zinc-copper.
Claims (5)
1. liquid-phase precipitation method prepares a method for nano cupric oxide, carries out according to following step: getting concentration under room temperature is 0.1mol ﹒ L
-1cuSO
4solution 100mL, adds calcium lignin sulphonate 1g, stirring and dissolving, with continuous stirring, dropwise instills 2mol ﹒ L
-1naOH solution 10mL, reflux 6h at 50 DEG C, be cooled to room temperature, by the centrifugation of gained precipitation mixture, precipitate with deionized water cleans 3 times, then uses washes of absolute alcohol 3 times, centrifugation, thermostatic drying chamber 60 DEG C of dry 12h put into by solid after separation, then by dried solid in 300 DEG C of roasting temperature 2h, namely obtain black nano cupric oxide.
2. liquid-phase precipitation method prepares a method for nano cupric oxide, carries out according to following step: getting concentration under room temperature is 0.4mol ﹒ L
-1cuSO
4solution 100mL, adds calcium lignin sulphonate 2g, stirring and dissolving, with continuous stirring, dropwise instills 2mol ﹒ L
-1naOH solution 40mL, reflux 10h at 90 DEG C, be cooled to room temperature, by the centrifugation of gained precipitation mixture, precipitate with deionized water cleans 3 times, then uses washes of absolute alcohol 3 times, centrifugation, thermostatic drying chamber 60 DEG C of dry 12h put into by solid after separation, then by dried solid in 300 DEG C of roasting temperature 3h, namely obtain black nano cupric oxide.
3. liquid-phase precipitation method prepares a method for nano cupric oxide, carries out according to following step: getting concentration under room temperature is 0.1mol ﹒ L
-1cuSO
4solution 100mL, adds calcium lignin sulphonate 0.5g, stirring and dissolving, with continuous stirring, dropwise instills 2mol ﹒ L
-1naOH solution 20mL, reflux 10h at 80 DEG C, be cooled to room temperature, by the centrifugation of gained precipitation mixture, precipitate with deionized water cleans 3 times, then uses washes of absolute alcohol 3 times, centrifugation, thermostatic drying chamber 60 DEG C of dry 12h put into by solid after separation, then by dried solid in 500 DEG C of roasting temperature 2h, namely obtain black nano cupric oxide.
4. liquid-phase precipitation method prepares a method for nano cupric oxide, carries out according to following step: getting concentration under room temperature is 0.4mol ﹒ L
-1cuSO
4solution 100mL, adds calcium lignin sulphonate 1g, stirring and dissolving, with continuous stirring, dropwise instills 2mol ﹒ L
-1naOH solution 40mL, reflux 10h at 70 DEG C, be cooled to room temperature, by the centrifugation of gained precipitation mixture, precipitate with deionized water cleans 3 times, then uses washes of absolute alcohol 3 times, centrifugation, thermostatic drying chamber 60 DEG C of dry 12h put into by solid after separation, then by dried solid in 300 DEG C of roasting temperature 3h, namely obtain black nano cupric oxide.
5. liquid-phase precipitation method prepares a method for nano cupric oxide, carries out according to following step: getting concentration under room temperature is 0.2mol ﹒ L
-1cuSO
4solution 100mL, adds calcium lignin sulphonate 0.5g, stirring and dissolving, with continuous stirring, dropwise instills 2mol ﹒ L
-1naOH solution 30mL, reflux 6h at 60 DEG C, be cooled to room temperature, by the centrifugation of gained precipitation mixture, precipitate with deionized water cleans 3 times, then uses washes of absolute alcohol 3 times, centrifugation, thermostatic drying chamber 60 DEG C of dry 12h put into by solid after separation, then by dried solid in 300 DEG C of roasting temperature 2h, namely obtain black nano cupric oxide.
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| 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 |
| CN104743610B (en) * | 2015-03-12 | 2016-08-24 | 江苏大学 | A kind of liquid-phase precipitation method prepares the method for nano bismuth oxide |
| CN107413354B (en) * | 2017-09-12 | 2021-04-02 | 山东师范大学 | Preparation method of silver-loaded copper oxide nanocomposite |
| 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 |
Citations (2)
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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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| 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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| Title |
|---|
| CuO nanoparticle sensor for the electrochemical determination of dopamine;Sathish Reddy, et al.;《Electrochimica Acta》;20111201;第61卷;第79页第2栏第18-32行 * |
| Vacancy-Mediated Magnetism in Pure Copper Oxide Nanoparticles;Daqiang Gao, et al.;《Nanoscale Research Letters》;20100216;第5卷(第4期);第769-772页 * |
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