CN110255600A - A kind of method that rapid precipitation prepares basic copper sulfate two-dimensional nano piece - Google Patents

A kind of method that rapid precipitation prepares basic copper sulfate two-dimensional nano piece Download PDF

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Publication number
CN110255600A
CN110255600A CN201910711655.2A CN201910711655A CN110255600A CN 110255600 A CN110255600 A CN 110255600A CN 201910711655 A CN201910711655 A CN 201910711655A CN 110255600 A CN110255600 A CN 110255600A
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CN
China
Prior art keywords
copper sulfate
basic copper
dimensional nano
nano piece
ammonium hydroxide
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
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CN201910711655.2A
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Chinese (zh)
Inventor
侴术雷
赖伟鸿
李用成
李东祥
李亚书
宫毅涛
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Liaoning Xingkong Sodium Battery Co Ltd
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Liaoning Xingkong Sodium Battery Co Ltd
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Application filed by Liaoning Xingkong Sodium Battery Co Ltd filed Critical Liaoning Xingkong Sodium Battery Co Ltd
Priority to CN201910711655.2A priority Critical patent/CN110255600A/en
Publication of CN110255600A publication Critical patent/CN110255600A/en
Pending legal-status Critical Current

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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00Nanotechnology for materials or surface science, e.g. nanocomposites
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00Manufacture or treatment of nanostructures
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01GCOMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G3/00Compounds of copper
    • C01G3/10Sulfates
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00Crystal-structural characteristics
    • C01P2002/70Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
    • C01P2002/72Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/01Particle morphology depicted by an image
    • C01P2004/03Particle morphology depicted by an image obtained by SEM
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/60Particles characterised by their size
    • C01P2004/62Submicrometer sized, i.e. from 0.1-1 micrometer

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Nanotechnology (AREA)
  • Organic Chemistry (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • General Physics & Mathematics (AREA)
  • Physics & Mathematics (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Materials Engineering (AREA)
  • Inorganic Chemistry (AREA)
  • Composite Materials (AREA)
  • Manufacturing & Machinery (AREA)
  • Manufacture Of Metal Powder And Suspensions Thereof (AREA)

Abstract

The present invention provides a kind of method that rapid precipitation prepares basic copper sulfate two-dimensional nano piece, widely applies production to be particularly important in following industrialization.This method has efficiently in preparing material, and quickly, a variety of outstanding features such as succinct overcome the huge challenge of regulation two-dimension nano materials caused by the quick crystallization of precipitation reaction, prepare two-dimension nano materials Cu2(OH)2SO4, the invention patent innovative utilize copper sulphate and ammonium hydroxide are reactant, and water is solvent, slowly releases OH using the low dissociation coefficient of ammonium hydroxideIon, so that being grown according to two-dimensional directional of can orienting during the growth process of material.The present invention provides a kind of Cu with excellent properties2(OH)2SO4The pattern of nanometer sheet mutually regulates and controls method with object.This method is at low cost, reaction rate is fast, reacts mildly easily-controllable, energy conservation and environmental protection, product purity height and the advantages such as novel in shape.

Description

A kind of method that rapid precipitation prepares basic copper sulfate two-dimensional nano piece
Technical field
The present invention relates to technical field of nanometer material preparation, and in particular to a kind of rapid precipitation prepares basic copper sulfate two dimension The method of nanometer sheet.
Background technique
Basic copper sulfate (Cu2(OH)2SO4) belong to metal hydroxides, because its special crystal structure kills it medical It bacterium and is agriculturally widely used.In addition, its Derived Oxides has this substance extensively in fields such as energy storage, catalysis Potential application.Rapid, high volume, which prepares this electrode material and synthesis ionic conductor material, has wide application prospect.Especially, Special two-dimensional structure has the electronic and ionic conduction orientation of orientation, and powerful stress ability to bear and short axial ion pass Defeated path, it is considered to be particularly significant nano material branch.Existing preparation Cu2(OH)2SO4Method be using copper sulphate and hydrogen Calcium oxide is mixed with, and this method is difficult to pattern, size, and structure is controlled, and complex process, and impurity content is high.In addition, Although higher using basic copper sulfate purity prepared by urea, the disadvantages such as grain diameter is big, and specific surface is low.And CuSO4NaCO is added dropwise in solution3It is prepared, but its preparation but nanometer little particle, is not had two-dimensional material feature.
Therefore, two-dimentional Cu can simply, quickly be prepared by inventing one kind2(OH)2SO4The method of nanometer sheet material will be in future Industrialization, and widely apply production it is particularly important.The precipitation method have efficient, quick, succinct etc. a variety of in preparing material Outstanding feature.But simultaneously, the quick crystallization of precipitation reaction makes preparation, regulates and controls along specific dimension nano material: such as two-dimentional Nano material has very big challenge.
Summary of the invention
For the prior art is insufficient or Improvement requirement, the present invention provides a kind of rapid precipitation and prepares two wiener of basic copper sulfate The method of rice piece, the huge challenge of two-dimension nano materials is regulated and controled caused by the quick crystallization the method overcome precipitation reaction, Prepare two-dimension nano materials Cu2(OH)2SO4.For the present invention using ammonium hydroxide as precipitating reagent, water is solvent, utilizes the low dissociation system of ammonium hydroxide Number slowly releases OH-Ion, so that being grown according to two-dimensional directional of can orienting during the growth process of material.
To achieve the above object, the invention is realized by the following technical scheme:
The present invention provides a kind of method that rapid precipitation prepares basic copper sulfate two-dimensional nano piece, which is characterized in that with copper sulphate It is raw material with ammonium hydroxide, is synthesized by liquid-phase precipitation method, specific steps are as follows:
Step 1, at 25-30 DEG C, by percentage to the quality, by 70-80% copper sulphate and 20-30% ammonia solvent Yu Shuizhong, and Persistently stir 10-20 minutes;
The copper sulphate is the aqueous solution of concentration 0.3-0.8%;
The ammonium hydroxide is the aqueous solution of concentration 0.09-0.11%;
Step 2 is separated 5-10 minutes, is obtained shallowly by mixed material supercentrifuge obtained by step 1 with 3500-5000r/min Blue precipitate;
Step 3 cleans light blue sediment obtained by step 2 3-5 times with ethyl alcohol;
Step 4, by step 3 resulting material 60-80 DEG C dry 5-12 hours to get basic copper sulfate two-dimensional nano piece.
Ethyl alcohol used is 96% ethanol solution in the step 3.
Compared with prior art, the beneficial effects of the present invention are: the present invention carries out material system using the liquid phase room temperature precipitation method Standby, compared with conventional hydrothermal method, this method is easy to operate, and prepared product morphology is novel, quality is stablized.
Detailed description of the invention
Fig. 1 is Cu in embodiment 12(OH)2SO4Nanometer sheet X-ray diffraction (XRD) figure.
Fig. 2 is Cu in embodiment 12(OH)2SO4Nanometer sheet scanning electron microscope (SEM) test chart.
Specific embodiment
Preparation method of the invention is described further below with reference to embodiment:
Embodiment 1:
The present invention provides a kind of method that rapid precipitation prepares basic copper sulfate two-dimensional nano piece.This method is with copper sulphate and ammonium hydroxide For raw material, synthesized by liquid-phase precipitation method, specific steps are as follows:
Step 1, at 25 DEG C, by 700g concentration be 0.3% copper sulphate and 300g concentration is 0.09% ammonia solvent Yu Shuizhong, And continue stirring 10 minutes;
Step 2 separates 5 minutes by mixed material supercentrifuge obtained by step 1 with 4000r/min;
Step 3 cleans the light blue sediment of gained 3 times with 96 % ethanol solutions;
Step 3 resulting material is dried 10 hours at 60 DEG C to get basic copper sulfate two-dimensional nano piece by step 4.
XRD result such as Fig. 1 product structure is basic copper sulfate, and pattern is received as shown in Fig. 2, be nanoscale laminated structure The width of rice piece is 500nm or so.
Embodiment 2:
The present invention provides a kind of method that rapid precipitation prepares basic copper sulfate two-dimensional nano piece.This method is with copper sulphate and ammonium hydroxide For raw material, synthesized by liquid-phase precipitation method, specific steps are as follows:
Step 1, at 25 DEG C, by 750g concentration be 0.5% copper sulphate and 250g concentration is 0.10% ammonia solvent Yu Shuizhong, And continue stirring 10 minutes;
Step 2 separates 5 minutes by mixed material supercentrifuge obtained by step 1 with 4000 r/min;
Step 3 cleans the light blue sediment of gained 3 times with 96 % ethanol solutions;
Step 3 resulting material is dried 10 hours at 60 DEG C to get basic copper sulfate two-dimensional nano piece by step 4.
Embodiment 3:
The present invention provides a kind of method that rapid precipitation prepares basic copper sulfate two-dimensional nano piece.This method is with copper sulphate and ammonium hydroxide For raw material, synthesized by liquid-phase precipitation method, specific steps are as follows:
Step 1, at 25 DEG C, by 800g concentration be 0.8% copper sulphate and 200g concentration is 0.11% ammonia solvent Yu Shuizhong, And continue stirring 10 minutes;
Step 2 separates 5 minutes by mixed material supercentrifuge obtained by step 1 with 4000r/min;
Step 3 cleans the light blue sediment of gained 3 times with 96 % ethanol solutions;
Step 3 resulting material is dried 10 hours at 60 DEG C to get basic copper sulfate two-dimensional nano piece by step 4.

Claims (2)

1. a kind of method that rapid precipitation prepares basic copper sulfate two-dimensional nano piece, which is characterized in that be with copper sulphate and ammonium hydroxide Raw material is synthesized by liquid-phase precipitation method, specific steps are as follows:
Step 1, at 25-30 DEG C, by percentage to the quality, by 70-80% copper sulphate and 20-30% ammonia solvent Yu Shuizhong, and Persistently stir 10-20 minutes;
The copper sulphate is the aqueous solution of concentration 0.3-0.8%;
The ammonium hydroxide is the aqueous solution of concentration 0.09-0.11%;
Step 2 is separated 5-10 minutes, is obtained shallowly by mixed material supercentrifuge obtained by step 1 with 3500-5000r/min Blue precipitate;
Step 3 cleans light blue sediment obtained by step 2 3-5 times with ethyl alcohol;
Step 4, by step 3 resulting material 60-80 DEG C dry 5-12 hours to get basic copper sulfate two-dimensional nano piece.
2. the method that a kind of rapid precipitation according to claim 1 prepares basic copper sulfate two-dimensional nano piece, feature exist In ethyl alcohol used is 96% ethanol solution in the step 3.
CN201910711655.2A 2019-08-02 2019-08-02 A kind of method that rapid precipitation prepares basic copper sulfate two-dimensional nano piece Pending CN110255600A (en)

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CN201910711655.2A CN110255600A (en) 2019-08-02 2019-08-02 A kind of method that rapid precipitation prepares basic copper sulfate two-dimensional nano piece

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111204792A (en) * 2020-01-21 2020-05-29 中国科学院福建物质结构研究所 Method for regulating and controlling growth morphology of copper sulfate pentahydrate crystal by using urea
CN112290341A (en) * 2020-10-20 2021-01-29 南通德晋昌光电科技有限公司 Environment-friendly processing method of bus bar

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB728520A (en) * 1952-09-18 1955-04-20 Eiji Munekata Improvements in or relating to manufacturing and using a copper compound containing copper hydroxide
CN1843933A (en) * 2006-04-28 2006-10-11 常州市裕和金属材料有限公司 Novel process for leaching metal fiber copper protective layer by ammonia and ammonium sulfate
CN101391800A (en) * 2007-09-20 2009-03-25 深圳市东江环保股份有限公司 Method for producing basic copper chloride, cupric sulfate pentahydrate from copper-containing etching waste liquid
CN107956036A (en) * 2017-07-17 2018-04-24 福建省晋江市华宇织造有限公司 Support the 3D screen cloths of Pneumatic soles

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB728520A (en) * 1952-09-18 1955-04-20 Eiji Munekata Improvements in or relating to manufacturing and using a copper compound containing copper hydroxide
CN1843933A (en) * 2006-04-28 2006-10-11 常州市裕和金属材料有限公司 Novel process for leaching metal fiber copper protective layer by ammonia and ammonium sulfate
CN101391800A (en) * 2007-09-20 2009-03-25 深圳市东江环保股份有限公司 Method for producing basic copper chloride, cupric sulfate pentahydrate from copper-containing etching waste liquid
CN107956036A (en) * 2017-07-17 2018-04-24 福建省晋江市华宇织造有限公司 Support the 3D screen cloths of Pneumatic soles

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
席改卿: "硫酸铜与氨水反应实验的探讨", 《邯郸师专学报》 *

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111204792A (en) * 2020-01-21 2020-05-29 中国科学院福建物质结构研究所 Method for regulating and controlling growth morphology of copper sulfate pentahydrate crystal by using urea
CN112290341A (en) * 2020-10-20 2021-01-29 南通德晋昌光电科技有限公司 Environment-friendly processing method of bus bar

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Application publication date: 20190920