CN1556250A - Electrolysis preparation method of nano cuprous oxide - Google Patents

Electrolysis preparation method of nano cuprous oxide Download PDF

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Publication number
CN1556250A
CN1556250A CNA2003101128216A CN200310112821A CN1556250A CN 1556250 A CN1556250 A CN 1556250A CN A2003101128216 A CNA2003101128216 A CN A2003101128216A CN 200310112821 A CN200310112821 A CN 200310112821A CN 1556250 A CN1556250 A CN 1556250A
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Prior art keywords
copper oxide
tetrahydrofuran
red copper
thf
electrolysis
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CN1259454C (en
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�ű�����
张爱茜
刘洪禄
孟楠
杨曦
韩朔睽
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Nanjing University
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Nanjing University
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  • Electrolytic Production Of Non-Metals, Compounds, Apparatuses Therefor (AREA)

Abstract

An electrolysis process for preparing the nano-class cuprous oxide includes electrolyzing copper anode in the electrolyte containing acetonitrile and tetrahydrofuran, adding the quaternary ammonium salt of long-chain alkyl until it is saturated to obtain cuprous oxide nanoparticles, and calcining at 400-600 deg.C under protection of N2.

Description

A kind of electrolytic preparation method of nanoscale Red copper oxide
One, technical field
The present invention relates to Red copper oxide (Cu 2O) electrolytic preparation method.
Two, background technology
According to Materials science,, enter nanoscale (10 when the particle diameter of the particulate of composition material diminishes gradually -1-10 2Nm) afterwards, the rising of primitive proportion is formed at its interface, and the degree of disorder sharply raises, and shows small-size effect, surface effects and quantum size effect etc.This series of effects has caused nano material all to demonstrate at aspects such as sound, electricity, light, magnetic the property that differs from body phase material.Because the peculiar property of nano material, nano science is subjected to more and more paying close attention to and paying attention to nanotechnology, and many countries have all dropped into the work that conducts a research of a large amount of funds.
As a kind of important Inorganic Chemicals, Red copper oxide all has purposes widely in fields such as dyestuff, catalyst, agricultural chemicals, opticglass, photocells.Process for preparing Cu 2 O commonly used has cuprous chloride hydrolysis method, electrolytic process etc.
The technology that present industrial electrolytic process prepares Red copper oxide is as follows:
NaCl:260-290g/L; NaOH:0.5g/L; Temperature: 75-80 degree; Electrode: copper; Current density: 750A/m 2
This method speed of response is very fast, and productive rate is also very high, the Red copper oxide favorable dispersity of generation.Weak point is particle diameter bigger and very inhomogeneous (300-1000nm).
China's patent (application number 03118706.4) discloses the method that a kind of metallic copper anodes oxidation style prepares the nano cupric oxide material.It is to add Cu in oxide electrolyte 2The crystal growth inhibitor of O is or/and Cu 2The nucleus of crystal of O, or contain the carrier of nucleus of crystal or/and another kind of nano material, and the concentration, the concentration of alkali of oxide salt in the control electrolytic solution, can obtain the Cu of particle diameter<100nm 2The O material.This method is many with respect to former method progress, can obtain the Cu of nanoscale 2O, shortcoming is that homogeneity is bad, process is comparatively complicated.
Three, summary of the invention
1. goal of the invention: the purpose of this invention is to provide a kind of electrolytic preparation method of nanoscale Red copper oxide, utilize the inventive method can prepare the Red copper oxide (Cu of nanoscale 2O).
2. technical scheme:
The principle of this programme: anode copper slowly dissolves, and moves to negative electrode under effect of electric field, is reduced to nano level copper atom.Dissolved oxygen residual in the solution is oxidized to Red copper oxide with nano level copper atom.Cause particle to be grown up for reducing the gathering of copper atom generation secondary, follow dispersion agent as stablizer so add the quaternary ammonium salt of chain alkyl.
Technical scheme of the present invention is as follows:
A kind of nanoscale Red copper oxide (Cu 2O) electrolytic preparation method is characterized in that metallic copper anodes electrolysis in the electrolytic solution that contains acetonitrile and tetrahydrofuran (THF), and the quaternary ammonium salt that adds chain alkyl is extremely saturated, the Red copper oxide median size<50nm that makes.
The volume ratio of acetonitrile and tetrahydrofuran (THF) is 3~5: 1 in the electrolytic solution, and the volume ratio of water and tetrahydrofuran (THF) is 0~1.5: 1.The employed current density of electrolysis is 50~200mA/cm 2Temperature during electrolysis is 20~90 ℃.The quaternary ammonium salt of chain alkyl is cetyl trimethylammonium bromide, tetradecyl trimethyl ammonium chloride or Trimethyllaurylammonium bromide.The Red copper oxide that makes after 400~600 ℃ of nitrogen protections calcining median size less than 200nm.
3. beneficial effect: the characteristics of present method be reaction temperature and, condition control is convenient, the Red copper oxide particle diameter of generation is even, mean diameter is less than 50 nanometers.After the nitrogen protection calcining, Red copper oxide crystal formation diameter is less than 200 nanometers.
Four, embodiment
Below further specify the present invention by example.
Embodiment 1:
Acetonitrile: tetrahydrofuran (THF): water=4: 1: 1
Add cetyl trimethylammonium bromide (CTAB) to saturated
Current density: 150mA/cm 2
Electrolysis time: 6min
Calcining temperature: 500 ℃
Particle diameter (nm) before the calcining: 10~30
Calcining back particle diameter (nm): 80~110
Embodiment 2:
Acetonitrile: tetrahydrofuran (THF)=4: 1
Add cetyl trimethylammonium bromide (CTAB) to saturated
Current density: 150mA/cm 2
Electrolysis time: 8min
Calcining temperature: 500 ℃
Particle diameter (nm) before the calcining: 5~20
Calcining back particle diameter (nm): 70~100
Embodiment 3:
Acetonitrile: tetrahydrofuran (THF): water=4: 1: 1
Add tetradecyl trimethyl ammonium chloride (TTAC) to saturated
Current density: 150mA/cm 2
Electrolysis time: 8min
Calcining temperature: 500
Particle diameter (nm) before the calcining: 15~35
Calcining back particle diameter (nm): 80~130
Embodiment 4:
Acetonitrile: tetrahydrofuran (THF): water=4: 1: 1
Add Trimethyllaurylammonium bromide (DTAB) to saturated
Current density: 150mA/cm 2
Electrolysis time: 8min
Calcining temperature: 500
Particle diameter (nm) before the calcining: 20~40
Calcining back particle diameter (nm): 80~130
Embodiment 5:
Acetonitrile: tetrahydrofuran (THF): water=4: 1: 1
Add tetradecyl trimethyl ammonium chloride (TTAC) to saturated
Current density: 150mA/cm 2
Electrolysis time: 9min
Calcining temperature: 500
Particle diameter (nm) before the calcining: 20~40
Calcining back particle diameter (nm): 100~140
Embodiment 6:
Acetonitrile: tetrahydrofuran (THF): water=3: 0.5: 1
Add Trimethyllaurylammonium bromide (DTAB) to saturated
Current density: 50mA/cm 2
Electrolysis time: 3min
Calcining temperature: 550
Particle diameter (nm) before the calcining: 20~40
Calcining back particle diameter (nm): 80~120
Embodiment 7:
Acetonitrile: tetrahydrofuran (THF): water=5: 1: 1
Add Trimethyllaurylammonium bromide (DTAB) to saturated
Current density: 100mA/cm 2
Electrolysis time: 20min
Calcining temperature: 500
Particle diameter (nm) before the calcining: 30~50
Calcining back particle diameter (nm): 80~110

Claims (7)

1. the electrolytic preparation method of a nanoscale Red copper oxide is characterized in that metallic copper anodes electrolysis in the electrolytic solution that contains acetonitrile and tetrahydrofuran (THF), and the quaternary ammonium salt that adds chain alkyl is extremely saturated, the Red copper oxide median size<50nm that makes.
2. root method according to claim 1 is characterized in that the volume ratio of acetonitrile and tetrahydrofuran (THF) is 3~5: 1 in the electrolytic solution, and the volume ratio of water and tetrahydrofuran (THF) is 0~1.5: 1.
3. root method according to claim 1 is characterized in that the employed current density of electrolysis is 50~200mA/cm 2
4. method according to claim 1, the temperature when it is characterized in that electrolysis are 20~90 ℃.
5. method according to claim 1, the quaternary ammonium salt that it is characterized in that chain alkyl is cetyl trimethylammonium bromide, tetradecyl trimethyl ammonium chloride or Trimethyllaurylammonium bromide.
6. method according to claim 1 is characterized in that the Red copper oxide median size<200nm after 400~600 ℃ of nitrogen protection calcinings that makes.
7. method according to claim 2 is characterized in that the Red copper oxide median size<40nm that makes.
CN200310112821.6A 2003-12-31 2003-12-31 Electrolysis preparation method of nano cuprous oxide Expired - Fee Related CN1259454C (en)

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CN1259454C CN1259454C (en) 2006-06-14

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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102925914A (en) * 2012-10-18 2013-02-13 成都华泽晶体材料有限公司 Method for preparing nanometer aluminum hydroxide powder by using electrochemical method
CN102925915A (en) * 2012-10-18 2013-02-13 苏州华泽纳米材料有限公司 Method for preparing nano aluminum oxide powder by electrochemical method
CN102943280A (en) * 2012-10-18 2013-02-27 成都华泽晶体材料有限公司 Method for preparing high-purity aluminium hydroxide powder by electrochemical method
CN104233433A (en) * 2014-10-03 2014-12-24 上海工程技术大学 Method for preparing cuprous oxide thin film
CN105483743A (en) * 2014-09-16 2016-04-13 江苏泰禾金属工业有限公司 Device and method for preparing cuprous oxide through electrolysis
CN106591922A (en) * 2017-02-05 2017-04-26 桂林理工大学 Preparation method of Cu2O nano film
CN106835242A (en) * 2017-02-05 2017-06-13 桂林理工大学 A kind of Cu2The preparation method of O nano-arrays

Cited By (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102925914A (en) * 2012-10-18 2013-02-13 成都华泽晶体材料有限公司 Method for preparing nanometer aluminum hydroxide powder by using electrochemical method
CN102925915A (en) * 2012-10-18 2013-02-13 苏州华泽纳米材料有限公司 Method for preparing nano aluminum oxide powder by electrochemical method
CN102943280A (en) * 2012-10-18 2013-02-27 成都华泽晶体材料有限公司 Method for preparing high-purity aluminium hydroxide powder by electrochemical method
CN102925915B (en) * 2012-10-18 2015-08-26 苏州华泽纳米材料有限公司 A kind of method that electrochemical production is nano alumina powder jointed
CN102943280B (en) * 2012-10-18 2016-01-06 成都华泽晶体材料有限公司 A kind of method of electrochemical production Two-step purifying body
CN105483743A (en) * 2014-09-16 2016-04-13 江苏泰禾金属工业有限公司 Device and method for preparing cuprous oxide through electrolysis
CN104233433A (en) * 2014-10-03 2014-12-24 上海工程技术大学 Method for preparing cuprous oxide thin film
CN104233433B (en) * 2014-10-03 2016-09-14 上海工程技术大学 A kind of method preparing cuprous oxide film
CN106591922A (en) * 2017-02-05 2017-04-26 桂林理工大学 Preparation method of Cu2O nano film
CN106835242A (en) * 2017-02-05 2017-06-13 桂林理工大学 A kind of Cu2The preparation method of O nano-arrays
CN106591922B (en) * 2017-02-05 2018-05-08 桂林理工大学 Cu2Preparation method of O nano film

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