CN101786673A - Synthesis method for basic cobalt carbonate ferrum nano material - Google Patents

Synthesis method for basic cobalt carbonate ferrum nano material Download PDF

Info

Publication number
CN101786673A
CN101786673A CN 201010128596 CN201010128596A CN101786673A CN 101786673 A CN101786673 A CN 101786673A CN 201010128596 CN201010128596 CN 201010128596 CN 201010128596 A CN201010128596 A CN 201010128596A CN 101786673 A CN101786673 A CN 101786673A
Authority
CN
China
Prior art keywords
sodium hydroxide
mol
iron
chloride
solution
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.)
Granted
Application number
CN 201010128596
Other languages
Chinese (zh)
Other versions
CN101786673B (en
Inventor
吴庆知
林强
孙海明
董明艳
李世普
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Wuhan University of Technology WUT
Original Assignee
Wuhan University of Technology WUT
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Wuhan University of Technology WUT filed Critical Wuhan University of Technology WUT
Priority to CN2010101285965A priority Critical patent/CN101786673B/en
Publication of CN101786673A publication Critical patent/CN101786673A/en
Application granted granted Critical
Publication of CN101786673B publication Critical patent/CN101786673B/en
Expired - Fee Related legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Images

Landscapes

  • Inorganic Compounds Of Heavy Metals (AREA)
  • Compounds Of Iron (AREA)

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 (4)

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 was in 180 ℃ of reactions 10 hours, and product obtains basic carbonate iron cobalt nano material through washing, drying.
2. the synthetic method of a kind of basic cobalt carbonate ferrum nano material according to claim 1, it is characterized in that: the concentration of lysine solution described in the step 1) is 0.04 mol, step 2) mol ratio of iron(ic) chloride and Methionin is 1: 1 in, and 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.
3. the synthetic method of a kind of basic cobalt carbonate ferrum nano material according to claim 1, it is characterized in that: the concentration of lysine solution described in the step 1) is 0.04 mol, step 2) mol ratio of iron(ic) chloride and Methionin is 1: 1 in, and 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.
4. the synthetic method of a kind of basic cobalt carbonate ferrum nano material according to claim 1, it is characterized in that: the concentration of lysine solution described in the step 1) is 0.12 mol, step 2) mol ratio of iron(ic) chloride and Methionin is 1: 3 in, and 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.
CN2010101285965A 2010-03-18 2010-03-18 Synthesis method for basic cobalt carbonate ferrum nano material Expired - Fee Related CN101786673B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN2010101285965A CN101786673B (en) 2010-03-18 2010-03-18 Synthesis method for basic cobalt carbonate ferrum nano material

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN2010101285965A CN101786673B (en) 2010-03-18 2010-03-18 Synthesis method for basic cobalt carbonate ferrum nano material

Publications (2)

Publication Number Publication Date
CN101786673A true CN101786673A (en) 2010-07-28
CN101786673B CN101786673B (en) 2011-11-02

Family

ID=42530074

Family Applications (1)

Application Number Title Priority Date Filing Date
CN2010101285965A Expired - Fee Related CN101786673B (en) 2010-03-18 2010-03-18 Synthesis method for basic cobalt carbonate ferrum nano material

Country Status (1)

Country Link
CN (1) CN101786673B (en)

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102560656A (en) * 2010-12-22 2012-07-11 中国科学院大连化学物理研究所 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
CN105047421A (en) * 2015-06-15 2015-11-11 昆明理工大学 Method for preparing graphene/basic carbonate nanocomposite 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
CN110475752A (en) * 2017-03-08 2019-11-19 尤米科尔公司 The precursor of cathode material for rechargable lithium ion cell

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

Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102560656A (en) * 2010-12-22 2012-07-11 中国科学院大连化学物理研究所 Preparation method of micron flower-like composite metal basic carbonate
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
CN105047421A (en) * 2015-06-15 2015-11-11 昆明理工大学 Method for preparing graphene/basic carbonate nanocomposite material
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
CN110475752A (en) * 2017-03-08 2019-11-19 尤米科尔公司 The precursor of cathode material for rechargable lithium ion cell
CN110475752B (en) * 2017-03-08 2022-08-09 尤米科尔公司 Precursor for cathode material for rechargeable lithium ion batteries

Also Published As

Publication number Publication date
CN101786673B (en) 2011-11-02

Similar Documents

Publication Publication Date Title
CN101786673B (en) Synthesis method for basic cobalt carbonate ferrum nano material
CN102126762B (en) Method for preparing NiO nano flowerlike microspheres with surface topography controllable
CN103708551B (en) The preparation method of a kind of ethylene glycol-water mixed solvent thermal synthesis bismuth oxycarbonate flower-like microsphere
CN105399152B (en) A kind of solvothermal preparation method of the sour nickel nano material of cobalt
CN103316691B (en) Magnetic solid acid and preparation method thereof
CN101318710B (en) Iron oxide multi-stage hollow core-shell material and preparation method thereof
CN111420664B (en) Preparation method of flaky cuprous oxide/cobaltous oxide nanocomposite and application of flaky cuprous oxide/cobaltous oxide nanocomposite in catalyzing ammonia borane hydrolysis hydrogen production
CN101962211B (en) Preparation method of nano nickel bicarbonate
CN108579661B (en) A kind of doped modified lithium ion sieve and preparation method thereof, application
CN106830049A (en) A kind of Cu of nanometer sheet composition9 S5The preparation method of hollow 26 face body
CN102744107A (en) Ferrite/polypyrrole (PPy) magnetic nano-photocatalyst and preparation method thereof
CN104001474A (en) Carbon-coated ferroferric oxide core-shell nano particle and preparation method thereof
CN101857260A (en) Method for preparing spherical cerium dioxide nano material with square-sheet surface structure by hydrothermal method
CN105268483B (en) A kind of preparation method and application of core-shell material catalyst
CN107252690B (en) One kind base catalyst of supported copper oxide containing auxiliary agent and preparation method thereof
CN102502770A (en) Flower-like copper oxide catalyst and preparation method and application thereof
CN107175340A (en) A kind of preparation method of core shell structure Cu@Ag nano-particles
CN101486494B (en) Method for synthesizing cobalt carbonate hydroxide nano material
CN101928034A (en) A kind of method for preparing cuprous chloride
CN102764654B (en) Based on FexOyInorganic nano composite material and preparation method thereof
CN101691672A (en) Method for preparing nano-sheet assembled bismuthyl bromide superstructure by adjusting and controlling surfactant
CN102580640B (en) Magnetic organic and inorganic hybrid material with multi-level nuclear shell structure and preparation method thereof
CN102502842B (en) Preparation method for radial copper molybdate microspheres assembled by nanowires
CN103880093B (en) Hollow spherical nickel bicarbonate aggregate
CN101555042A (en) Method for preparing spinel type iron-containing oxide nano-materials by low heat solid state reaction

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
C14 Grant of patent or utility model
GR01 Patent grant
C17 Cessation of patent right
CF01 Termination of patent right due to non-payment of annual fee

Granted publication date: 20111102

Termination date: 20140318