CN103232076A - Synthesis method of cobalt hydroxide with different grain diameters - Google Patents
Synthesis method of cobalt hydroxide with different grain diameters Download PDFInfo
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- CN103232076A CN103232076A CN2013101815626A CN201310181562A CN103232076A CN 103232076 A CN103232076 A CN 103232076A CN 2013101815626 A CN2013101815626 A CN 2013101815626A CN 201310181562 A CN201310181562 A CN 201310181562A CN 103232076 A CN103232076 A CN 103232076A
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Abstract
The invention discloses a synthesis method of cobalt hydroxide with different grain diameters. Organic ligands serving as complexing agents and cobalt ions form cobalt-organic ligand complexes respectively, so that the cobalt ions can be prevented from being in direct contact with hydroxyl radicals and oxygen in air and the problem that the cobalt ions are oxidized is overcome; alkaline organic matters are selected as precipitants and are hydrolyzed in an aqueous solution to generate hydroxyl radicals, so that the alkaline organic matters react with the cobalt ions to generate cobalt hydroxide precipitates; and when different alkaline compounds are selected as the precipitants, the cobalt hydroxide with different grain diameters can be obtained.
Description
Technical field
The invention relates to a kind of synthetic method of cobaltous hydroxide, refer to a kind of synthetic method of different-grain diameter cobaltous hydroxide especially.
Background technology
The synthetic method of present domestic cobaltous hydroxide generally is to adopt cobalt chloride and sodium hydroxide direct reaction method, though this method is simple to operate, faces following technical barrier:
(1) adopt sodium hydroxide directly cobalt chloride or rose vitriol to be precipitated: when utilizing sodium hydroxide for precipitation agent, because this speed of response is very fast, caused reaction conditions wayward, thereby the shape of the cobaltous hydroxide that obtains to be amorphous substantially.Simultaneously, because cobaltous hydroxide easily is oxidized to Co (OH) under alkaline condition
3, it is substantially all darker therefore to utilize this method to obtain the cobaltous hydroxide color and luster.
(2) the oxygen institute oxidation that is dissolved in easily under alkaline condition in the water owing to cobaltous hydroxide generates the trivalent cobalt, and therefore, some enterprise adopts the adding reductive agent that the dissolved oxygen in the water is eliminated.Though this method can be avoided Co (OH) to a certain extent
2Equally also there are many problems in oxidized problem in water, as: the control of the add-on of reductive agent; The raising of reaction cost; The handling problem of reductive agent reaction after product etc.
(3) there is the method report to adopt ammoniacal liquor to carry out Co (OH) as precipitation agent
2Preparation: when utilizing ammoniacal liquor as precipitation agent, can reduce Co (OH) to a certain extent
2Sedimentation speed, improve the rule degree of product.Yet, since ammoniacal liquor in the aqueous solution also easily with cobalt ion formation [Co (NH
3)
6]
2+ title complex, and this title complex still can with water in dissolved oxygen react, and generate [Co (NH
3)
6]
3+ title complex, thus the reduction of productive rate caused.
Summary of the invention
The purpose of this invention is to provide a kind of cobalt ion of can avoiding and directly directly contact with airborne oxygen with hydroxide radical, with the synthetic method of the different-grain diameter cobaltous hydroxide that overcomes the oxidized problem of cobalt ion.
For achieving the above object, solution of the present invention is:
A kind of synthetic method of different-grain diameter cobaltous hydroxide, its concrete steps are:
Step 1, cobalt salt is dissolved in the deionized water dissolving after, the adding organic ligand is complexing agent, makes these organic ligands form cobalt-organic ligand title complex with cobalt ion respectively;
Described organic ligand can be Sodium.alpha.-hydroxypropionate, Padil, pyridine, quadrol or imidazoles.
Described alkaline organic can be triethylamine, methylamine, ethamine or diethanolamine.
The mass ratio of the cobalt salt of described step 1, deionized water and imidazoles or Sodium.alpha.-hydroxypropionate is 1:5:0.4; Then be that the deionized water that is dissolved in again of the solid that will obtain in the step 1 and the mass ratio that adds the relative step 1 of quality of diethanolamine solution are 2.0-3.0:0.2-0.6:0.6-1.5 in the step 2.
Add imidazoles or Sodium.alpha.-hydroxypropionate in described step 1 cobalt salt solution, need to continue to stir 30 minutes, filter; Then step 2 is dissolved in the solid that obtains in the deionized water again, adds diethanolamine solution slowly, after diethanolamine solution all adds, continues reaction 1-3 hour, filters, and washing namely obtains the cobaltous hydroxide solid that particle diameter is about 10 microns.
The mass ratio of the cobalt salt of described step 1, deionized water and imidazoles or Sodium.alpha.-hydroxypropionate is 1:5:0.4; Then be that the deionized water that is dissolved in again of the solid that will obtain in the step 1 and the mass ratio that adds the relative step 1 of quality of ethylamine solution are 2.0-3.0:0.2-0.6:0.6-1.5 in the step 2.
Add imidazoles or Sodium.alpha.-hydroxypropionate in described step 1 cobalt salt solution, need to continue to stir 30 minutes, filter; Then step 2 is dissolved in the solid that obtains in the deionized water again, adds ethylamine solution slowly, after ethylamine solution all adds, continues reaction 1-3 hour, filters, and washing namely obtains the cobaltous hydroxide solid that particle diameter is about 300 nanometers.
After adopting such scheme, the present invention is that the employing organic ligand is complexing agent, make these organic ligands form cobalt-organic ligand title complex with cobalt ion respectively, avoid cobalt ion directly directly to contact with airborne oxygen with hydroxide radical, thereby overcome the oxidized problem of cobalt ion; And then to select the organism of alkalescence be precipitation agent, utilizes alkaline organic in aqueous solution generation hydrolysis and generate hydroxide radical, thereby react with cobalt ion and generate the cobaltous hydroxide precipitation.When selecting for use different organo-alkali compounds to be precipitation agent, can obtain the cobaltous hydroxide of different-grain diameter.
Description of drawings
Fig. 1 is about the cobaltous hydroxide electron-microscope scanning figure of 10 μ m for the synthetic particle diameter of the inventive method;
Fig. 2 is about the cobaltous hydroxide electron-microscope scanning figure of 300nm for the synthetic particle diameter of the inventive method.
Embodiment
Explain embodiments of the present invention below in conjunction with accompanying drawing:
The present invention has disclosed a kind of synthetic method of different-grain diameter cobaltous hydroxide, and its concrete steps are:
Step 1, cobalt salt is dissolved in the deionized water dissolving after, the adding organic ligand is complexing agent, makes these organic ligands form cobalt-organic ligand title complex with cobalt ion respectively; Described organic ligand can be Sodium.alpha.-hydroxypropionate, Padil, pyridine, quadrol or imidazoles etc.; Wherein the mass ratio of cobalt salt, deionized water and organic ligand can be 1:5:0.4;
Embodiment 1:
1 kilogram cobalt salt is dissolved in 5 liters the deionized water, after the stirring and dissolving, adds 0.4 kilogram imidazoles, continue to stir 30 minutes, filter.And then the solid that obtains is dissolved in the deionized water of 2L, add 0.3 kilogram of diethanolamine solution slowly, after diethanolamine solution all adds, continue reaction 1 hour, filter, washing namely obtains the cobaltous hydroxide solid (seeing shown in Figure 1) that particle diameter is about 10 microns.
Embodiment 2:
1 kilogram cobalt salt is dissolved in 5 liters the deionized water, after the stirring and dissolving, adds 0.4 kilogram imidazoles, continue to stir 30 minutes, filter.And then the solid that obtains is dissolved in the deionized water of 2L, add 0.5 kilogram of ethylamine solution slowly, after ethylamine solution all adds, continue reaction 1 hour, filter, washing namely obtains the cobaltous hydroxide solid (seeing shown in Figure 2) that particle diameter is about 300 nanometers.
Embodiment 3:
1 kilogram cobalt salt is dissolved in 5 liters the deionized water, after the stirring and dissolving, adds 0.4 kilogram Sodium.alpha.-hydroxypropionate, continue to stir 30 minutes, filter.And then the solid that obtains is dissolved in the deionized water of 2L, add 0.3 kilogram of diethanolamine solution slowly, after diethanolamine solution all adds, continue reaction 1 hour, filter, washing namely obtains the cobaltous hydroxide solid (seeing shown in Figure 1) that particle diameter is about 10 microns.
Embodiment 4:
1 kilogram cobalt salt is dissolved in 5 liters the deionized water, after the stirring and dissolving, adds 0.4 kilogram Sodium.alpha.-hydroxypropionate, continue to stir 30 minutes, filter.And then the solid that obtains is dissolved in the deionized water of 2L, add 0.5 kilogram of ethylamine solution slowly, after ethylamine solution all adds, continue reaction 1 hour, filter, washing namely obtains the cobaltous hydroxide solid (seeing shown in Figure 2) that particle diameter is about 300 nanometers.
Composition principle of the present invention is as follows, (wherein be organic ligand with lactic acid, methylamine is that alkaline organic is example).
In sum, synthetic method of the present invention is that the employing organic ligand is complexing agent, make these organic ligands form cobalt-organic ligand title complex with cobalt ion respectively, avoid cobalt ion directly directly to contact with airborne oxygen with hydroxide radical, thereby overcome the oxidized problem of cobalt ion; And then to select the organism of alkalescence be precipitation agent, utilizes alkaline organic in aqueous solution generation hydrolysis and generate hydroxide radical, thereby react with cobalt ion and generate the cobaltous hydroxide precipitation.When selecting for use different organo-alkali compounds to be precipitation agent, can obtain the cobaltous hydroxide of different-grain diameter.
Claims (7)
1. the synthetic method of a different-grain diameter cobaltous hydroxide, its concrete steps are:
Step 1, cobalt salt is dissolved in the deionized water dissolving after, the adding organic ligand is complexing agent, makes these organic ligands form cobalt-organic ligand title complex with cobalt ion respectively;
Step 2, be dissolved in the solid of cobalt-organic cooperation title complex of obtaining in the deionized water again, and then the organism of selection alkalescence is precipitation agent, utilize alkaline organic in aqueous solution generation hydrolysis and generate hydroxide radical, thereby react with cobalt ion and generate the cobaltous hydroxide precipitation.
2. the synthetic method of different-grain diameter cobaltous hydroxide as claimed in claim 1, it is characterized in that: described organic ligand can be lactic acid, Padil, pyridine, quadrol or imidazoles.
3. the synthetic method of different-grain diameter cobaltous hydroxide as claimed in claim 1, it is characterized in that: described alkaline organic can be triethylamine, methylamine, ethamine or diethanolamine.
4. as the synthetic method of claim 1,2 or 3 described different-grain diameter cobaltous hydroxides, it is characterized in that: the mass ratio of the cobalt salt of described step 1, deionized water and imidazoles or Sodium.alpha.-hydroxypropionate is 1:5:0.4; Then be that the deionized water that is dissolved in again of the solid that will obtain in the step 1 and the mass ratio that adds the relative step 1 of quality of diethanolamine solution are 2.0-3.0:0.2-0.6:0.6-1.5 in the step 2.
5. the synthetic method of different-grain diameter cobaltous hydroxide as claimed in claim 4 is characterized in that: add imidazoles or Sodium.alpha.-hydroxypropionate in described step 1 cobalt salt solution, need to continue to stir 30 minutes, filter; Then step 2 is dissolved in the solid that obtains in the deionized water again, adds diethanolamine solution slowly, after diethanolamine solution all adds, continues reaction 1-3 hour, filters, and washing namely obtains the cobaltous hydroxide solid that particle diameter is about 10 microns.
6. as the synthetic method of claim 1,2 or 3 described different-grain diameter cobaltous hydroxides, it is characterized in that: the mass ratio of the cobalt salt of described step 1, deionized water and imidazoles or Sodium.alpha.-hydroxypropionate is 1:5:0.4; Then be that the deionized water that is dissolved in again of the solid that will obtain in the step 1 and the mass ratio that adds the relative step 1 of quality of ethylamine solution are 2.0-3.0:0.2-0.6:0.6-1.5 in the step 2.
7. the synthetic method of different-grain diameter cobaltous hydroxide as claimed in claim 6 is characterized in that: add imidazoles or Sodium.alpha.-hydroxypropionate in described step 1 cobalt salt solution, need to continue to stir 30 minutes, filter; Then step 2 is dissolved in the solid that obtains in the deionized water again, adds ethylamine solution slowly, after ethylamine solution all adds, continues reaction 1-3 hour, filters, and washing namely obtains the cobaltous hydroxide solid that particle diameter is about 300 nanometers.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105481025A (en) * | 2015-12-11 | 2016-04-13 | 郑州大学 | Porous cobalt hydroxide material, and preparation method and applications thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1359353A (en) * | 1999-06-29 | 2002-07-17 | Omg芬兰公司 | Process for making high density and large particle size cobalt hydroxide or cobalt mixed hydroxides and a product made by this process |
| CN102807255A (en) * | 2011-05-31 | 2012-12-05 | 中国科学院大连化学物理研究所 | Flower-like nanometer cobalt hydroxide material and preparation method thereof |
-
2013
- 2013-05-16 CN CN2013101815626A patent/CN103232076A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1359353A (en) * | 1999-06-29 | 2002-07-17 | Omg芬兰公司 | Process for making high density and large particle size cobalt hydroxide or cobalt mixed hydroxides and a product made by this process |
| CN102807255A (en) * | 2011-05-31 | 2012-12-05 | 中国科学院大连化学物理研究所 | Flower-like nanometer cobalt hydroxide material and preparation method thereof |
Non-Patent Citations (2)
| Title |
|---|
| 杨幼平等: "α-Co(OH)2的合成及其电化学电容行为", 《中国有色金属学报》, vol. 18, 30 June 2008 (2008-06-30), pages 326 - 330 * |
| 林海彬等: "两种不同粒径氢氧化钴的合成及表征", 《漳州师范学院学报（自然科学版）》, no. 3, 31 December 2011 (2011-12-31), pages 22 - 24 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105481025A (en) * | 2015-12-11 | 2016-04-13 | 郑州大学 | Porous cobalt hydroxide material, and preparation method and applications thereof |
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Application publication date: 20130807 |