CN101486494B - Method for synthesizing cobalt carbonate hydroxide nano material - Google Patents
Method for synthesizing cobalt carbonate hydroxide nano material Download PDFInfo
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- CN101486494B CN101486494B CN2009100608016A CN200910060801A CN101486494B CN 101486494 B CN101486494 B CN 101486494B CN 2009100608016 A CN2009100608016 A CN 2009100608016A CN 200910060801 A CN200910060801 A CN 200910060801A CN 101486494 B CN101486494 B CN 101486494B
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- glycine
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- 239000002086 nanomaterial Substances 0.000 title claims abstract description 8
- KDPJLLVSZLZTAN-UHFFFAOYSA-K cobalt(3+);carbonate;hydroxide Chemical compound [OH-].[Co+3].[O-]C([O-])=O KDPJLLVSZLZTAN-UHFFFAOYSA-K 0.000 title claims description 7
- 238000000034 method Methods 0.000 title abstract description 8
- 230000002194 synthesizing effect Effects 0.000 title 1
- DHMQDGOQFOQNFH-UHFFFAOYSA-N Glycine Chemical compound NCC(O)=O DHMQDGOQFOQNFH-UHFFFAOYSA-N 0.000 claims abstract description 49
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 45
- 239000000243 solution Substances 0.000 claims abstract description 31
- 239000004471 Glycine Substances 0.000 claims abstract description 25
- 239000008367 deionised water Substances 0.000 claims abstract description 15
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 15
- 238000010189 synthetic method Methods 0.000 claims abstract description 9
- 239000011259 mixed solution Substances 0.000 claims abstract description 7
- 238000006243 chemical reaction Methods 0.000 claims description 13
- 238000002156 mixing Methods 0.000 claims description 13
- 238000003756 stirring Methods 0.000 claims description 8
- 230000035484 reaction time Effects 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- 239000013078 crystal Substances 0.000 abstract description 4
- UFMZWBIQTDUYBN-UHFFFAOYSA-N cobalt dinitrate Chemical compound [Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O UFMZWBIQTDUYBN-UHFFFAOYSA-N 0.000 abstract 2
- 229910001981 cobalt nitrate Inorganic materials 0.000 abstract 2
- 239000007795 chemical reaction product Substances 0.000 abstract 1
- HIYNGBUQYVBFLA-UHFFFAOYSA-D cobalt(2+);dicarbonate;hexahydroxide Chemical compound [OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[Co+2].[Co+2].[Co+2].[Co+2].[Co+2].[O-]C([O-])=O.[O-]C([O-])=O HIYNGBUQYVBFLA-UHFFFAOYSA-D 0.000 abstract 1
- 229910000001 cobalt(II) carbonate Inorganic materials 0.000 abstract 1
- 238000002360 preparation method Methods 0.000 abstract 1
- MPMSMUBQXQALQI-UHFFFAOYSA-N cobalt phthalocyanine Chemical compound [Co+2].C12=CC=CC=C2C(N=C2[N-]C(C3=CC=CC=C32)=N2)=NC1=NC([C]1C=CC=CC1=1)=NC=1N=C1[C]3C=CC=CC3=C2[N-]1 MPMSMUBQXQALQI-UHFFFAOYSA-N 0.000 description 15
- 238000013019 agitation Methods 0.000 description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 6
- 238000001228 spectrum Methods 0.000 description 6
- 230000005540 biological transmission Effects 0.000 description 5
- 206010013786 Dry skin Diseases 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 239000000654 additive Substances 0.000 description 2
- 230000000996 additive effect Effects 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 229910017052 cobalt Inorganic materials 0.000 description 2
- 239000010941 cobalt Substances 0.000 description 2
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 2
- 230000001788 irregular Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000000975 co-precipitation Methods 0.000 description 1
- 150000001869 cobalt compounds Chemical class 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 125000003630 glycyl group Chemical group [H]N([H])C([H])([H])C(*)=O 0.000 description 1
- 230000005693 optoelectronics Effects 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
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Abstract
The invention relates to a synthetic method which comprises the following steps: 1) glycine is added into deionized water and stirred to be dissolved, thereby obtaining a glycine solution with the concentration of 0.05 mol/L; 2) according to the mole ratio of 1 to 2 between cobalt nitrate and glycine, cobalt nitrate is taken to be added into the glycine solution obtained in the step 1) and stirred to be dissolved, thereby obtaining a mixed solution A; 3) sodium hydroxide is added into deionized water and stirred to be dissolved, thereby obtaining sodium hydroxide solution with the molar concentration of 0.05 mol/L; 4) the sodium hydroxide solution obtained in the step 3) is added into the mixed solution A and stirred to obtain mixed solution B which then reacts at the temperature of 150 DEG C for 5 hours to 48 hours; the reaction products are washed and dried to obtain a basic cobaltous carbonate nano-material. The preparation method has the advantages of simple processes, low cost, no pollution, controllable shape and crystal form.
Description
Technical field
The present invention relates to a kind of synthetic method of cobalt carbonate hydroxide nano material.
Background technology
Cobaltous dihydroxycarbonate is a kind of very important cobalt compound material, is widely used as alkaline battery additive agent, electrode and capacitance material, catalyzer etc.Cobaltous dihydroxycarbonate also can be used as the precursor for preparing other various cobalt/cobalt oxides.
The cobaltous dihydroxycarbonate of different shapes and crystalline form has different character and application.Study novel, simply, controllably prepare the method for the cobaltous dihydroxycarbonate of different shapes and crystalline form, significant to the property research and the application and development of cobaltous dihydroxycarbonate.At present, the method that is used to prepare cobaltous dihydroxycarbonate comprises methods such as various co-precipitation, solvent thermal and galvanic deposit, and these methods cut both ways.Wherein, advantage such as the pattern of solvent thermal synthesis method, easy handling low owing to its cost, may command target product and structure is subjected to extensive concern.
Summary of the invention
The object of the present invention is to provide the synthetic method of the cobalt carbonate hydroxide nano material of a kind of simple, low-cost, pollution-free, controllable shape and crystalline form.
Controllable shape of the present invention is meant sheet or bar-shaped, and the may command crystalline form is meant amorphous or monocrystalline.
To achieve these goals, technical scheme of the present invention is: the synthetic method of a kind of cobaltous dihydroxycarbonate nanometer sheet and nanometer rod is characterized in that it comprises the steps:
1) glycine is added in the deionized water, stir and make the glycine dissolving, make the glycine solution that concentration is 0.05 mol;
2) in the mol ratio of Xiao Suangu and glycine be 1: 2 ratio, get in the glycine solution that Xiao Suangu adds step 1), stir and make its dissolving, mixed solution A;
3) sodium hydroxide is added in the deionized water, stir and make its dissolving, make the sodium hydroxide solution that volumetric molar concentration is 0.05 mol;
4) sodium hydroxide solution with step 3) is added in the mixed solution A, stir mixing solutions B; Mixing solutions B was in 150 ℃ of reactions 5-48 hour, and product obtains cobalt carbonate hydroxide nano material through washing, drying.
Above-mentioned steps 4 of the present invention) reaction times of mixing solutions B is 5 hours in.
Perhaps, the reaction times of mixing solutions B is 10 hours in the step 4).
Perhaps, the reaction times of mixing solutions B is 48 hours in the step 4).
The invention has the beneficial effects as follows: in simple reaction system,, realized the controlledly synthesis of different shapes and crystalline form cobaltous dihydroxycarbonate at an easy rate by changing the time of reaction.The inventive method agents useful for same is commonly used, cheap, low cost; Synthesis step is simple, pollution-free; Product shape and crystalline form are controlled.The cobaltous dihydroxycarbonate of synthetic different shapes and crystalline form can be respectively applied for every field such as alkaline secondary battery additive, electrode materials, opto-electronic device and catalyzer.
Description of drawings
Fig. 1 (a) is the transmission electron microscope photo that embodiment 1 obtains product.
Fig. 1 (b) is the transmission electron microscope photo that embodiment 2 obtains product.
Fig. 1 (c) is the transmission electron microscope photo 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.
Fig. 3 (a) is the XPS collection of illustrative plates that embodiment 1 obtains product.
Fig. 3 (b) is the XPS collection of illustrative plates that embodiment 2 obtains product.
Fig. 3 (c) is the XPS collection of illustrative plates 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:
0.1502 the gram glycine adds in the 25mL deionized water, dissolves under magnetic agitation; With 0.2910 gram Xiao Suangu [Co (NO
3)
26H
2O] add in the above-mentioned glycine solution, under magnetic agitation, make it dissolving; 0.08 gram sodium hydroxide adds in 15 ml deionized water, dissolves under magnetic agitation; Above-mentioned sodium hydroxide solution is at the uniform velocity dripped (dripping off) in 1-2 minute in the mixing solutions of glycine and Xiao Suangu, magnetic agitation is after 15 minutes, changes volume over to and is in 50 milliliters the autoclave polytetrafluoroethyllining lining, in 150 ℃ of reactions 5 hours.After reactor naturally cools to room temperature, with deionized water and ethanol alternately centrifugal (10000 rev/mins * 5 minutes) washing; Product obtains amorphous cobaltous dihydroxycarbonate nanometer sheet in irregular shape 60 ℃ of dryings 4 hours.Fig. 1 (a) is the transmission electron microscope photo that obtains product, is presented under 5 hours the condition of reaction, and the product of gained is irregular sheet structure; Fig. 2 (a) is the XRD figure spectrum that obtains product, illustrates that the nanometer sheet that obtained under the condition in 5 hours in reaction is a non-crystal structure; Fig. 3 (a) is the XPS collection of illustrative plates that obtains product, and the valency state of Co, O and C proves that the product that obtains is the cobaltous dihydroxycarbonate nanometer sheet in the demonstration product.
Embodiment 2:
0.1502 the gram glycine adds in the 25mL deionized water, dissolves under magnetic agitation; With 0.2910 gram Xiao Suangu [Co (NO
3)
26H
2O] add in the above-mentioned glycine solution, under magnetic agitation, make it dissolving; 0.08 gram sodium hydroxide adds in 15 ml deionized water, dissolves under magnetic agitation; Above-mentioned sodium hydroxide solution is at the uniform velocity dripped (dripping off in 1-2 minute) in the mixing solutions of glycine and Xiao Suangu, magnetic agitation is after 15 minutes, changes volume over to and is in 50 milliliters the autoclave polytetrafluoroethyllining lining, in 150 ℃ of reactions 10 hours.After reactor naturally cools to room temperature, with deionized water and ethanol alternately centrifugal (10000 rev/mins * 5 minutes) washing; Product obtains the length-to-diameter ratio scope and is approximately 4.4 to 15 amorphous cobaltous dihydroxycarbonate nanometer rod 60 ℃ of dryings 4 hours.Fig. 1 (b) is the transmission electron microscope photo that obtains product, is presented under 10 hours the condition of reaction, and the product of gained is the nano bar-shape structure; Fig. 2 (b) is the XRD figure spectrum that obtains product, illustrates that the nanometer rod that obtained under the condition in 10 hours in reaction still is non-crystal structure; Fig. 3 (b) is the XPS collection of illustrative plates that obtains product, and the valency state of Co, O and C proves that the product that obtains is the cobaltous dihydroxycarbonate nanometer rod in the demonstration product.
Embodiment 3:
0.1502 the gram glycine adds in the 25mL deionized water, dissolves under magnetic agitation; With 0.2910 gram Xiao Suangu [Co (NO
3)
26H
2O] add in the above-mentioned glycine solution, under magnetic agitation, make it dissolving; 0.08 gram sodium hydroxide adds in 15 ml deionized water, dissolves under magnetic agitation; Above-mentioned sodium hydroxide solution is at the uniform velocity dripped (adding) in 1-2 minute in the mixing solutions of glycine and Xiao Suangu, magnetic agitation is after 15 minutes, changes volume over to and is in 50 milliliters the autoclave polytetrafluoroethyllining lining, in 150 ℃ of reactions 48 hours.After reactor naturally cools to room temperature, with deionized water and ethanol alternately centrifugal (10000 rev/mins * 5 minutes) washing; Product obtains the mixture of monocrystalline cobaltous dihydroxycarbonate nanometer sheet and nanometer rod 60 ℃ of dryings 4 hours.Fig. 1 (c) is the projection electromicroscopic photograph that obtains product, is presented under 48 hours the condition of reaction, and the product of gained is the mixture of nanometer sheet and nanometer rod; Fig. 2 (c) is the XRD figure spectrum that obtains product, illustrates that the nanometer sheet and the nanometer rod that obtained under the condition in 48 hours in reaction are single crystal structure; Fig. 3 (c) is the XPS collection of illustrative plates that obtains product, and the valency state of Co, O and C proves that the product that obtains is monocrystalline cobaltous dihydroxycarbonate nanometer sheet and nanometer rod mixture in the demonstration product.
Used glycine in the inventive method, English name is glycine, and molecular weight is 75.07, and its structural formula is as follows: NH
2CH
2COOH.
Claims (4)
1. the synthetic method of a cobalt carbonate hydroxide nano material is characterized in that comprising the steps:
1) glycine is added in the deionized water, stir and make the glycine dissolving, make the glycine solution that concentration is 0.05 mol;
2) in the mol ratio of Xiao Suangu and glycine be 1: 2 ratio, get in the glycine solution that Xiao Suangu adds step 1), stir and make its dissolving, mixed solution A;
3) sodium hydroxide is added in the deionized water, stir and make its dissolving, make the sodium hydroxide solution that volumetric molar concentration is 0.05 mol;
4) sodium hydroxide solution with step 3) is added in the mixed solution A, stir mixing solutions B; Mixing solutions B was in 150 ℃ of reactions 5-48 hour, and product obtains cobalt carbonate hydroxide nano material through washing, drying.
2. synthetic method according to claim 1 is characterized in that: the reaction times of mixing solutions B is 5 hours in the step 4).
3. synthetic method according to claim 1 is characterized in that: the reaction times of mixing solutions B is 10 hours in the step 4).
4. synthetic method according to claim 1 is characterized in that: the reaction times of mixing solutions B is 48 hours in the step 4).
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Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101786673B (en) * | 2010-03-18 | 2011-11-02 | 武汉理工大学 | Synthesis method for basic cobalt carbonate ferrum nano material |
| JP5758743B2 (en) * | 2010-09-02 | 2015-08-05 | 日本化学工業株式会社 | Cobalt hydroxide and method for producing the same, and cobalt oxide and method for producing the same |
| JP5961004B2 (en) * | 2012-02-21 | 2016-08-02 | 日本化学工業株式会社 | Method for producing cobalt hydroxide, method for producing cobalt oxide, and method for producing lithium cobaltate |
| CN104418388B (en) * | 2013-08-26 | 2016-09-14 | 荆门市格林美新材料有限公司 | The technique of a kind of ultra-fine powder of cobalt carbonate of continuous production and device thereof |
| CN106158401A (en) * | 2016-07-12 | 2016-11-23 | 昆明理工大学 | There is the new application of the subcarbonate of layer structure |
| CN110759387A (en) * | 2018-07-25 | 2020-02-07 | 荆门市格林美新材料有限公司 | Preparation method of manganese-doped basic cobalt carbonate |
| CN113044888B (en) * | 2019-12-26 | 2024-06-18 | 荆门市格林美新材料有限公司 | Preparation method of amorphous cobalt carbonate |
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