CN102430760A - Preparation method of metal nickel - Google Patents

Preparation method of metal nickel Download PDF

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Publication number
CN102430760A
CN102430760A CN2011102758477A CN201110275847A CN102430760A CN 102430760 A CN102430760 A CN 102430760A CN 2011102758477 A CN2011102758477 A CN 2011102758477A CN 201110275847 A CN201110275847 A CN 201110275847A CN 102430760 A CN102430760 A CN 102430760A
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China
Prior art keywords
nickel
preparation
metallic nickel
metallic
triethylamine
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CN2011102758477A
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Chinese (zh)
Inventor
谢钢
范文
肖丹妮
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Northwest University
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Northwest University
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Priority to CN2011102758477A priority Critical patent/CN102430760A/en
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Abstract

The invention discloses a preparation method of metal nickel, and the method comprises the following specific steps of: dissolving nickel salt in water or an organic solvent in a closed container; and adding triethylamine and reacting at 190-350DEG C to obtain the metal nickel. In the invention, raw materials are easily available, and the preparation method is simple; and particularly, the metal nickel can be prepared in a short time by taking water as a solvent and using the cheap triethylamine.

Description

A kind of preparation method of metallic nickel
Technical field
The present invention relates to a kind of preparation method of metallic nickel, belong to the metal simple-substance preparing technical field.
Background technology
Nano metal Ni has unique physics, chemical property; Have broad application prospects at aspects such as catalyst, magnetic material, magnetic fluid, absorbing material, sintering activator, electrocondution slurry, coating material, high performance electrode material, carbide alloy binding agents; The market demand increases very fast, is one of focus of domestic and international novel capabilities developing material.Along with developing rapidly of automobile, electronics, machinery, information industry, the application of nanometer Ni will constantly be widened and expand.
The method for preparing at present nanometer Ni particle mainly contains two kinds of physics method and chemical methods.Physics method device therefor is expensive, and operating condition requires harsh, and chemical method usually will be with Ni in the presence of suitable reducing agent 2+Be reduced into Ni.Common reducing agent has hydrazine hydrate, metallic zinc, carbon, hypophosphite and 1,2-propane diols etc.Like (Inorg. Chem. Commun., 2002,5 such as Qian; 971) with the Metal Zn be the synthetic nickel nanotube, (mining metallurgical engineering, 2001 such as Zhang Chuanfu of having obtained of reducing agent; 21,49) utilizing the ultrasonic atomization liquid phase reduction, is that reducing agent prepares nanometer nickel with the hydrazine.Sol-gel process is the chemical method that is used for preparing nickel nano particle the earliest, (Appl. Phys. Lett., 1992 such as Chatterjee; 60; 138) reported that elder generation's oxyquinoline nickel salt that decomposition temperature is lower is dissolved in alcohol and forms gel, added several hydrochloric acid and micron-sized KBr powder then and form gel that the colloid that filters gained is heated to 300 ℃; Organic principle is removed in thermal decomposition, obtains the extra-fine nickel powder that average grain diameter is 5-11nm at last.
Hydro-thermal method is under hydrothermal condition, to react, typical hydrothermal reaction condition is to be higher than 100 ℃ in temperature, and air pressure is greater than carrying out in 1 atmospheric aqueous medium.Classical hydro-thermal reaction belongs to a branch of solid state reaction, and it is a heterogeneous reaction.In recent years, water (solvent) thermal synthesis had been widely used in crystal growth, material is synthetic, received the attention of inorganic chemist.Generally speaking, hydro-thermal reaction is in confined conditions, be higher than 100 ℃ of scope internal reaction precursors " treat different things alike " preparation end product.In the hydro-thermal synthetic technology, liquid state or vaporous water are the media that transmits pressure; Under the high pressure, most reactants all can be partially dissolved in water, impel to be reflected in liquid phase or the gas phase and carry out.The viscosity of water reduces and is easier to diffusion, makes solvent become possibility to the extraction and the crystal growth of solid constituent.Under this nonequilibrium state crystallization condition of hydro-thermal, the dynamics metastable phase more possibly separated out than thermodynamics stable phase easily, thereby the metastable phase crystal nucleation becomes possibility.Hydro-thermal is synthesized normally agitated reactor of used equipment at present, and it is made up of the inner bag of the polytetrafluoroethylene (PTFE) of a stainless steel casing and a 25-100 mL.
As surfactant, inferior sodium phosphate obtains nickel nano wire and nickel nano belt as reducing agent through changing the reaction condition hydrothermal preparation to Qian etc. (Adv. Mater., 2003,15,1946) with neopelex.
Summary of the invention
The purpose of this invention is to provide a kind of raw material and be easy to get, the preparation method of the simple metallic nickel of preparation method.
Implementation procedure of the present invention is following:
A kind of preparation method of metallic nickel is characterized in that: in closed container, nickel salt in the water-soluble or organic solvent, is added triethylamine, obtain 190~350 ℃ of reactions, preferred temperature range is 230~280 ℃.
Said nickel salt is common nickel chloride, nickel acetate, nickelous sulfate or nickel nitrate etc., and the mol ratio of nickel salt and triethylamine is 1:1~1:20, is preferably 1:1~1:5.
Organic solvent is a monohydric alcohol, polyalcohol, and acetone, acetonitrile, DMF etc. as with an organic solvent, are preferably simple methyl alcohol or ethanol commonly used.
The above-mentioned reaction time is more than 30 minutes, prolongs the reaction time, and product still is an elemental nickel, and the product particle diameter that just obtains is bigger, is advisable in common 30 minutes to 3 hours.
Advantage of the present invention and good effect: raw material of the present invention is easy to get, the preparation method is simple, particularly is solvent with water, uses cheap triethylamine can prepare metallic nickel in the short time.
Description of drawings
Fig. 1 is the XRD figure of the metallic nickel for preparing in the methanol system;
Fig. 2 is the SEM figure of the metallic nickel for preparing in the methanol system;
Fig. 3 is the XRD figure of the metallic nickel for preparing in the water.
The specific embodiment
Embodiment 1
With 0.36g (0.0015mol) NiCl 26H 2O is dissolved in the 10ml methanol solution; Drip 0.36g (0.0033mol) triethylamine, mixed liquor is transferred to confined reaction in the autoclave, setting reaction temperature and time are respectively 220 ℃ and 2 hours; Reaction finish centrifugal, washing, drying, grey black toner end (productive rate 92%).
As shown in Figure 1, the X-ray powder diffraction of product shows, has prepared elemental nickel, and corresponding JCPDS card number is 4-850, and scanning electron microscope analysis shows that product is the microballoon (Fig. 2) of 200~300nm.
Embodiment 2
With 0.36g (0.0015mol) NiCl 26H 2O is dissolved in the 10ml aqueous solution; Drip 0.67g (0.0066mol) triethylamine, mixed liquor is transferred to confined reaction in the autoclave, setting reaction temperature and time are respectively 240 ℃ and 2 hours; Reaction finish centrifugal, washing, drying, grey black toner end (productive rate 93%).
As shown in Figure 3, the X-ray powder diffraction of product shows, has prepared elemental nickel, and corresponding JCPDS card number is 4-850.
Embodiment 3
Similar with embodiment 2, different is: do not add triethylamine, reaction obtains the yellow green powder, through XRD analysis, shows that product is a nickel oxide.
Equally, in ethanol system, do not add triethylamine, can't obtain metallic nickel yet.
Embodiment 4
Similar with embodiment 1, different is: methyl alcohol is replaced with DMF, and 210 ℃ of reactions also obtained metallic nickel in 2 hours.
Embodiment 5
Similar with embodiment 1, different is that reaction temperature is 180 ℃ of reactions 2 hours, and product is a green powder; The X-ray powder diffraction shows that product is not a metallic nickel, when temperature is lower than 190 ℃, can not generate metallic nickel; Obviously, temperature is one of key factor to the preparation of metallic nickel.
Embodiment 6
Similar with embodiment 1, different is: do not add triethylamine, but added 0.0033mol NaOH, the product that obtains is a green powder, changes reaction temperature, does not obtain metallic nickel equally, and obviously, triethylamine is two of a key factor to the preparation of metallic nickel.
Embodiment 7
Similar with embodiment 1, different is: the methyl alcohol spent glycol is replaced, and 300 ℃ of reactions obtained metallic nickel in 1 hour equally.
Embodiment 8
Similar with embodiment 1, different is to replace nickel chloride with cobalt chloride, does not obtain simple substance cobalt, explains under this experiment condition, and it is simple substance cobalt that triethylamine can not reduce cobalt ions.

Claims (6)

1. the preparation method of a metallic nickel is characterized in that: in closed container, nickel salt in the water-soluble or organic solvent, is added triethylamine, obtain metallic nickel 190~350 ℃ of reactions.
2. according to the preparation method of the said metallic nickel of claim 1, it is characterized in that: said nickel salt is common nickel chloride, nickel acetate, nickelous sulfate or nickel nitrate.
3. according to the preparation method of the said metallic nickel of claim 1, it is characterized in that: organic solvent is a monohydric alcohol, polyalcohol, acetone, acetonitrile, DMF.
4. according to the preparation method of the said metallic nickel of claim 3, it is characterized in that: said organic solvent is methyl alcohol or ethanol.
5. according to the preparation method of the said metallic nickel of claim 1, it is characterized in that: reaction temperature is 230~280 ℃.
6. according to the preparation method of one of any said metallic nickel of claim 1 to 5, it is characterized in that: the mol ratio of said nickel salt and triethylamine is 1:1~1:20.
CN2011102758477A 2011-09-18 2011-09-18 Preparation method of metal nickel Pending CN102430760A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103170649A (en) * 2013-04-15 2013-06-26 南京理工大学 Preparation method of magnetic nickel nano material

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3816098A (en) * 1972-10-20 1974-06-11 Sherritt Gordon Mines Ltd Production of nickel powder from impure nickel compounds
CN1539581A (en) * 2003-04-08 2004-10-27 ���ǵ�����ʽ���� Metal nickel powder, its prepn. method, conductive paste and multi-layer ceramic capacitor
CN1572398A (en) * 2003-05-27 2005-02-02 三星电子株式会社 Method for preparing non-magnetic nickel powders
KR20100016821A (en) * 2008-08-05 2010-02-16 삼성전기주식회사 Preparing method of nickel nanoparticles
WO2010021600A1 (en) * 2008-08-22 2010-02-25 Agency For Science, Technology And Research Methods and compositions comprising polyoxometalates

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3816098A (en) * 1972-10-20 1974-06-11 Sherritt Gordon Mines Ltd Production of nickel powder from impure nickel compounds
CN1539581A (en) * 2003-04-08 2004-10-27 ���ǵ�����ʽ���� Metal nickel powder, its prepn. method, conductive paste and multi-layer ceramic capacitor
CN1572398A (en) * 2003-05-27 2005-02-02 三星电子株式会社 Method for preparing non-magnetic nickel powders
KR20100016821A (en) * 2008-08-05 2010-02-16 삼성전기주식회사 Preparing method of nickel nanoparticles
WO2010021600A1 (en) * 2008-08-22 2010-02-25 Agency For Science, Technology And Research Methods and compositions comprising polyoxometalates

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
GEOFFREY C.BOND等: "《黄金的催化作用 现象.原理.应用》", 31 October 2008, 科学出版社 *
罗晓华: "单分散磁性金属纳米粒子的液相法合成与表征", 《中国优秀硕士学位论文全文数据库》 *

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103170649A (en) * 2013-04-15 2013-06-26 南京理工大学 Preparation method of magnetic nickel nano material

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Application publication date: 20120502