CN101786673B - Synthesis method for basic cobalt carbonate ferrum nano material - Google Patents

Synthesis method for basic cobalt carbonate ferrum nano material Download PDF

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CN101786673B
CN101786673B CN2010101285965A CN201010128596A CN101786673B CN 101786673 B CN101786673 B CN 101786673B CN 2010101285965 A CN2010101285965 A CN 2010101285965A CN 201010128596 A CN201010128596 A CN 201010128596A CN 101786673 B CN101786673 B CN 101786673B
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sodium hydroxide
mixed solution
solution
iron
mol
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CN101786673A (en
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吴庆知
林强
孙海明
董明艳
李世普
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Wuhan University of Technology WUT
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Wuhan University of Technology WUT
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Abstract

The invention relates to a synthesis method for a basic cobalt carbonate ferrum nano material. The method comprises the following steps: (1) adding lysine into glycol, and stirring to obtain a lysine solution with the concentration of 0.04-0.12 mol/L; (2) adding iron chloride into the lysine solution of step (1), and stirring to obtain a mixed solution A, wherein the mol ratio of the iron chloride to the lysine is 1:1-1:3; (3) adding cobalt nitrate into the mixed solution A, and stirring to obtain a mixed solution B, wherein the mol ratio of the cobalt nitrate to the iron chloride is 1:1; (4) adding sodium hydroxide into the glycol, and stirring to obtain a sodium hydroxide solution with the concentration of 0.6-1 mol/L, wherein the mol ratio of the sodium hydroxide to the iron chloride is 9:1-15:1; and (5) and dropwise adding the sodium hydroxide solution of step (4) into the mixed solution B, stirring to obtain a mixed solution C, reacting at 180 DEG C for 10 hours, and washing and drying the product to obtain the basic cobalt carbonate ferrum nano material. The material has the characteristics of simplicity, low cost, no pollution and controllable product morphology.

Description

A kind of synthetic method of basic cobalt carbonate ferrum nano material
Technical field
The present invention relates to a kind of synthetic method of basic cobalt carbonate ferrum nano material.
Background technology
Basic cobalt carbonate ferrum is a kind of important cobaltous carbonate iron ore section bar material, can be used as fields such as anionite, sorbent material, molecular sieve and catalyzer.Basic cobalt carbonate ferrum also can be used as precursor and is used to prepare other various cobalt iron oxide.
The basic cobalt carbonate ferrum of similar shape pattern does not have different character and application.Study novel, controllably prepare the method for different-shape basic cobalt carbonate ferrum, significant to the recombination mechanism of the conversion of explaination natural mineral matter and geochemical process, octahedra layers of metal hydroxides structure etc.At present, the method that is used to prepare basic cobalt carbonate ferrum mainly is a coprecipitation method, and the solvent thermal synthesis method is subjected to extensive concern owing to the advantages such as pattern of its easy handling, may command target product.
Summary of the invention
The object of the present invention is to provide a kind of synthetic method of simple, low-cost, pollution-free, basic cobalt carbonate ferrum nano material that pattern is controlled.
The controlled octahedra shape or flower-shaped that is meant of pattern of the present invention.
To achieve these goals, technical scheme of the present invention is: a kind of synthetic method of basic cobalt carbonate ferrum nano material is characterized in that it comprises the steps:
1) Methionin is added in the ethylene glycol, stir and make the Methionin dissolving, make the lysine solution that concentration is the 0.04-0.12 mol;
2) mol ratio in iron(ic) chloride and Methionin is 1: 1-1: 3 ratio, take by weighing iron(ic) chloride, and add in the lysine solution of step 1), stir and make its dissolving, get mixed solution A;
3) in the mol ratio of Xiao Suangu and iron(ic) chloride be 1: 1 ratio, take by weighing Xiao Suangu, add step 2) mixed solution A in, stir and make its dissolving, mixing solutions B;
4) mol ratio in sodium hydroxide and iron(ic) chloride is 9: 1-15: 1 ratio, and weighing sodium hydroxide adds in the ethylene glycol, stirs and makes its dissolving, makes the sodium hydroxide solution that concentration is the 0.6-1 mol;
5) sodium hydroxide solution with step 4) is added drop-wise among the mixing solutions B, stir mixed solution C; Mixed solution C was in 180 ℃ of reactions 10 hours, and product obtains basic carbonate iron cobalt nano material through washing, drying.
Press such scheme, the concentration of lysine solution described in the step 1) is 0.04 mol, step 2) in the mol ratio of iron(ic) chloride and Methionin be 1: 1, the mol ratio of sodium hydroxide and iron(ic) chloride is 15: 1 in the step 4); The concentration of sodium hydroxide solution is 1 mol.
Press such scheme, the concentration of lysine solution described in the step 1) is 0.04 mol, step 2) in the mol ratio of iron(ic) chloride and Methionin be 1: 1, the mol ratio of sodium hydroxide and iron(ic) chloride is 9: 1 in the step 4); The concentration of sodium hydroxide solution is 0.6 mol.
Press such scheme, the concentration of lysine solution described in the step 1) is 0.12 mol, step 2) in the mol ratio of iron(ic) chloride and Methionin be 1: 3, the mol ratio of sodium hydroxide and iron(ic) chloride is 9: 1 in the step 4); The concentration of sodium hydroxide solution is 0.6 mol.
The invention has the beneficial effects as follows: in simple reaction system,, realized the controlledly synthesis of different-shape basic cobalt carbonate ferrum by changing the ratio of reactant.The inventive method agents useful for same is commonly used; Synthesis step is simple; Controllable product shape.The basic cobalt carbonate ferrum of institute's synthetic different-shape can be used for every field such as anionite, sorbent material, molecular sieve and catalyzer.
Description of drawings
Fig. 1 (a) is the stereoscan photograph that embodiment 1 obtains product.
Fig. 1 (b) is the stereoscan photograph that embodiment 2 obtains product.
Fig. 1 (c) is the stereoscan photograph that embodiment 3 obtains product.
Fig. 2 (a) is the XRD figure spectrum that embodiment 1 obtains product.
Fig. 2 (b) is the XRD figure spectrum that embodiment 2 obtains product.
Fig. 2 (c) is the XRD figure spectrum that embodiment 3 obtains product.
Embodiment
In order to understand the present invention better, further illustrate content of the present invention below in conjunction with embodiment, but content of the present invention not only is confined to the following examples.
Embodiment 1:
0.1462 gram Methionin adds in the 25mL ethylene glycol, dissolves under magnetic agitation; With 0.2704 gram iron(ic) chloride [FeCl 36H 2O] add in the above-mentioned lysine solution, under magnetic agitation, dissolve, obtain mixed solution A; With 0.2910 gram Xiao Suangu [Co (NO 3) 26H 2O] add in the mixed solution A, under magnetic agitation, make it dissolving, obtain mixing solutions B; 0.6000 gram sodium hydroxide adds in 15 milliliters of ethylene glycol, dissolves under magnetic agitation; Above-mentioned sodium hydroxide solution is at the uniform velocity dripped (dripping off) in 1-2 minute in mixing solutions B, magnetic agitation obtained mixed solution C after 20 minutes; It was in 50 milliliters the autoclave polytetrafluoroethyllining lining that mixed solution C changes volume over to, in 180 ℃ of reactions 10 hours.After reaction finished, reactor naturally cooled to room temperature, with deionized water and ethanol alternately centrifugal (10000 rev/mins * 5 minutes) washing; Product obtains flower-shaped basic cobalt carbonate ferrum nano material 60 ℃ of dryings 4 hours.Fig. 1 (a) is the stereoscan photograph that obtains product, shows that the product of gained is the flower-like structure that nanometer sheet is assembled into; Fig. 2 (a) is the XRD figure spectrum that obtains product, and JCPDS card number: 50-0235 (Co 5.84Fe 2.16(OH) 16(CO 3) 1.080.32H 2O)) contrast, the product that gained is described is a basic cobalt carbonate ferrum.
Embodiment 2:
0.1462 gram Methionin adds in the 25mL ethylene glycol, dissolves under magnetic agitation; With 0.2704 gram iron(ic) chloride [FeCl 36H 2O] add in the above-mentioned lysine solution, under magnetic agitation, dissolve, obtain mixed solution A; With 0.2910 gram Xiao Suangu [Co (NO 3) 26H 2O] add in the mixed solution A, under magnetic agitation, make it dissolving, obtain mixing solutions B; 0.3600 gram sodium hydroxide adds in 15 milliliters of ethylene glycol, dissolves under magnetic agitation; Above-mentioned sodium hydroxide solution is at the uniform velocity dripped (dripping off) in 1-2 minute in mixing solutions B, magnetic agitation obtained mixed solution C after 20 minutes; It was in 50 milliliters the autoclave polytetrafluoroethyllining lining that mixed solution C changes volume over to, in 180 ℃ of reactions 10 hours.After reaction finished, reactor naturally cooled to room temperature, with deionized water and ethanol alternately centrifugal (10000 rev/mins * 5 minutes) washing; Product obtains octahedra shape basic cobalt carbonate ferrum nano material 60 ℃ of dryings 4 hours.Fig. 1 (b) is the stereoscan photograph that obtains product, shows that the product of gained is octahedra shape structure; Fig. 2 (b) is the XRD figure spectrum that obtains product, and JCPDS card number: 50-0235 (Co 5.84Fe 2.16(OH) 16(CO 3) 1.080.32H 2O)) contrast, the product that gained is described is a basic cobalt carbonate ferrum.
Embodiment 3:
0.4386 gram Methionin adds in the 25mL ethylene glycol, dissolves under magnetic agitation; With 0.2704 gram iron(ic) chloride [FeCl 36H 2O] add in the above-mentioned lysine solution, under magnetic agitation, dissolve, obtain mixed solution A; With 0.2910 gram Xiao Suangu [Co (NO 3) 26H 2O] add in the mixed solution A, under magnetic agitation, make it dissolving, obtain mixing solutions B; 0.3600 gram sodium hydroxide adds in 15 milliliters of ethylene glycol, dissolves under magnetic agitation; Above-mentioned sodium hydroxide solution is at the uniform velocity dripped (dripping off) in 1-2 minute in mixing solutions B, magnetic agitation obtained mixed solution C after 20 minutes; It was in 50 milliliters the autoclave polytetrafluoroethyllining lining that mixed solution C changes volume over to, in 180 ℃ of reactions 10 hours.After reaction finished, reactor naturally cooled to room temperature, with deionized water and ethanol alternately centrifugal (10000 rev/mins * 5 minutes) washing; Product obtains octahedra shape and nanoparticle shape basic cobalt carbonate ferrum nano material 60 ℃ of dryings 4 hours.Fig. 1 (c) is the stereoscan photograph that obtains product, shows that the product of gained contains octahedra shape structure and nanoparticle shape structure; Fig. 2 (c) is the XRD figure spectrum that obtains product, and JCPDS card number: 50-0235 (Co 5.84Fe 2.16(OH) 16(CO 3) 1.080.32H 2O)) contrast, the product that gained is described is a basic cobalt carbonate ferrum.
Used Methionin in the inventive method, English name is lysine, and molecular weight is 146.2, and its structural formula is as follows: H 2NCH 2CH 2CH 2CH 2CH (NH 2) COOH.

Claims (1)

1. the synthetic method of a basic cobalt carbonate ferrum nano material is characterized in that comprising the steps:
1) Methionin is added in the ethylene glycol, stir and make the Methionin dissolving, make the lysine solution that concentration is the 0.04-0.12 mol;
2) mol ratio in iron(ic) chloride and Methionin is 1: 1-1: 3 ratio, take by weighing iron(ic) chloride, and add in the lysine solution of step 1), stir and make its dissolving, get mixed solution A;
3) in the mol ratio of Xiao Suangu and iron(ic) chloride be 1: 1 ratio, take by weighing Xiao Suangu, add step 2) mixed solution A in, stir and make its dissolving, mixing solutions B;
4) mol ratio in sodium hydroxide and iron(ic) chloride is 9: 1-15: 1 ratio, and weighing sodium hydroxide adds in the ethylene glycol, stirs and makes its dissolving, makes the sodium hydroxide solution that concentration is the 0.6-1 mol;
5) sodium hydroxide solution with step 4) is added drop-wise among the mixing solutions B, stir mixed solution C; Mixed solution C in the autoclave polytetrafluoroethyllining lining 180 ℃ the reaction 10 hours, product through the washing, drying, obtain basic carbonate iron cobalt nano material.
CN2010101285965A 2010-03-18 2010-03-18 Synthesis method for basic cobalt carbonate ferrum nano material Expired - Fee Related CN101786673B (en)

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CN102560656B (en) * 2010-12-22 2015-10-28 中国科学院大连化学物理研究所 The preparation method of micron flower-like composite metal basic carbonate
CN102731078A (en) * 2012-06-26 2012-10-17 武汉理工大学 Octahedral porous cobalt ferrite material and its preparation method
CN103887500A (en) * 2014-04-15 2014-06-25 山东大学 Rod-like cobalt carbonate iron composite material and application thereof
CN105047421B (en) * 2015-06-15 2017-11-10 昆明理工大学 A kind of preparation method of graphene/subcarbonate nano composite material
CN105185606A (en) * 2015-09-14 2015-12-23 南京大学 Preparation method of novel cobaltous dihydroxycarbonate-nitrogen-doped graphene combined electrode material
CN110475752B (en) * 2017-03-08 2022-08-09 尤米科尔公司 Precursor for cathode material for rechargeable lithium ion batteries

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1185143A (en) * 1995-05-26 1998-06-17 H·C·施塔克公司 Basic cobaltous carbonates, prodn. method and use thereof
CN1736882A (en) * 2005-08-05 2006-02-22 北京化工大学 Mesoporous structure Co3O4 nanocrystalline preparation method
CN101486494A (en) * 2009-02-20 2009-07-22 武汉理工大学 Method for synthesizing cobalt carbonate hydroxide nano material

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1185143A (en) * 1995-05-26 1998-06-17 H·C·施塔克公司 Basic cobaltous carbonates, prodn. method and use thereof
CN1736882A (en) * 2005-08-05 2006-02-22 北京化工大学 Mesoporous structure Co3O4 nanocrystalline preparation method
CN101486494A (en) * 2009-02-20 2009-07-22 武汉理工大学 Method for synthesizing cobalt carbonate hydroxide nano material

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