CN108069461A - The synthetic method of cobalt disulfide powder - Google Patents
The synthetic method of cobalt disulfide powder Download PDFInfo
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- CN108069461A CN108069461A CN201711386415.7A CN201711386415A CN108069461A CN 108069461 A CN108069461 A CN 108069461A CN 201711386415 A CN201711386415 A CN 201711386415A CN 108069461 A CN108069461 A CN 108069461A
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- cobalt disulfide
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- disulfide powder
- cobalt
- synthetic method
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G51/00—Compounds of cobalt
- C01G51/30—Sulfides
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention discloses a kind of synthetic method of cobalt disulfide powder, the step of method in contain：(a) analytically pure disodium ethylene diamine tetraacetate is added in deionized water, fully dissolving obtains solution A；(b) cobaltous sulfate and sodium thiosulfate are sequentially added in solution A, and is stirred, obtains solution B；(c) pH value for adjusting solution B is 1~12；(d) solution B after adjusting pH value is poured into reaction kettle, compactedness control is 60% 80%, and add in cobalt disulfide crystal seed, after closed reactor, it places it at 140 DEG C 250 DEG C after 5 50h of middle reaction, cooled to room temperature filters out bottom sediment, then the cobalt disulfide powder up to pyrite is dried in vacuo at 60 DEG C with dilute hydrochloric acid, carbon disulfide, absolute ethyl alcohol, deionized water rinsing respectively.The reaction of the present invention is disposably completed in the liquid phase, and process equipment is simple, and raw material is easy to get, and the cobalt disulfide powder dispersibility of preparation is good.
Description
Technical field
The present invention relates to a kind of synthetic methods of cobalt disulfide powder.
Background technology
At present, the cobalt disulfide with 3d valence electron shell structurres has excellent optics, electricity with pyrite
The properties such as, magnetics, high-purity cobalt disulfide powder may be used as the electrode material of thermal cell, on the one hand, during thermoelectricity tank discharge its
Internal temperature reaches as high as 600 DEG C, and the decomposition temperature of cobalt disulfide is more than 650 DEG C, is conducive to long life thermal battery；The opposing party
Face, the resistivity of cobalt disulfide is 0.002 Ω .cm, is conducive to the heavy-current discharge of thermal cell.
The report of the existing development results on cobalt disulfide, J.D.Passaretti et al. pass through [Co (NH3)6]Cl2With
H2S vulcanizes to obtain cobalt disulfide crystal under cryogenic, but crystal property is bad.
The content of the invention
The technical problems to be solved by the invention are the defects of overcoming the prior art, provide a kind of conjunction of cobalt disulfide powder
Into method, its reaction is disposably completed in the liquid phase, and process equipment is simple, and raw material is easy to get, the cobalt disulfide powder point of preparation
It is good to dissipate property.
The present invention solves above-mentioned technical problem and adopts the technical scheme that：A kind of synthetic method of cobalt disulfide powder, side
Contain in the step of method：
(a) analytically pure disodium ethylene diamine tetraacetate is added in deionized water, fully dissolving obtains solution A；
(b) cobaltous sulfate and sodium thiosulfate are sequentially added in solution A, and is stirred, obtains solution B；Wherein, wherein, sulphur
The molar concentration rate of sour cobalt and disodium ethylene diamine tetraacetate is 1：(0~1)；The molar concentration rate of cobaltous sulfate and sodium thiosulfate is
1：(1~2)；
(c) pH value for adjusting solution B is 1~12；
(d) solution B after adjusting pH value is poured into reaction kettle, compactedness control is 60%-80%, and adds in curing
Cobalt crystal seed after closed reactor, is placed it at 140 DEG C -250 DEG C after middle reaction 5-50h, cooled to room temperature filters out kettle
Then bottom sediment is dried in vacuo with dilute hydrochloric acid, carbon disulfide, absolute ethyl alcohol, deionized water rinsing at 60 DEG C respectively to obtain the final product
The cobalt disulfide powder of pyrite；.
Further, in the step (c), dilute hydrochloric acid is added in solution B or sodium hydroxide adjusts pH value.
Further, in the step (d), the grain size of the cobalt disulfide crystal seed of addition is 15-30nm.
Further, in the step (d), the cobalt disulfide crystal seed of addition accounts for the curing cobalt powder of estimation final production
The 1%~5% of the gross mass at end.
After employing above-mentioned technical proposal, the present invention has following advantageous effect：
1st, this method reaction is disposable in the liquid phase completes, and post-processing is not required, process equipment is simple；
2nd, raw material is easy to get, is at low cost, favorable repeatability, saves energy consumption, suitable for mass production；
3rd, the cobalt disulfide powder dispersibility prepared is good.
Description of the drawings
Fig. 1 is that the X-ray diffractometer of cobalt disulfide powder prepared by the present embodiment one analyzes (XRD) collection of illustrative plates.
Specific embodiment
In order that the present invention can be more clearly and readily understood, it is right below according to specific embodiment and with reference to attached drawing
The present invention is described in further detail.
Embodiment one
Contain in a kind of the step of synthetic method of cobalt disulfide powder, method：
(a) analytically pure disodium ethylene diamine tetraacetate is added in deionized water, fully dissolving obtains solution A；
(b) cobaltous sulfate and sodium thiosulfate are sequentially added in solution A, and passes through magnetic stirrer, obtains solution
B；Wherein, the molar concentration rate of cobaltous sulfate and disodium ethylene diamine tetraacetate is 1：0.5；Cobaltous sulfate and sodium thiosulfate it is mole dense
Degree is than being 1：2；
(c) pH value for adjusting solution B is 4；
(d) solution B after adjusting pH value is poured into reaction kettle, compactedness control is 70%, and adds in cobalt disulfide crystalline substance
Kind, after closed reactor, place it at 200 DEG C after middle reaction for 24 hours, cooled to room temperature filters out bottom sediment, then
Respectively with dilute hydrochloric acid, carbon disulfide, absolute ethyl alcohol, deionized water rinsing, it is dried in vacuo at 60 DEG C up to pyrite
Cobalt disulfide powder；Wherein, the cobalt disulfide crystal seed of addition accounts for the gross mass of the cobalt disulfide powder of estimation final production
3%, grain size is about 20nm.
In step (c), dilute hydrochloric acid is added in solution B or sodium hydroxide adjusts pH value.
The X-ray diffractometer of cobalt disulfide powder manufactured in the present embodiment analyzes (XRD) collection of illustrative plates as shown in Figure 1, through overscan
The pattern and grain size of electron microscopic observation sample are retouched, can substantially find the good dispersion of gained cobalt disulfide powder, even particle size distribution.
Embodiment two
Contain in a kind of the step of synthetic method of cobalt disulfide powder, method：
(a) analytically pure disodium ethylene diamine tetraacetate is added in deionized water, fully dissolving obtains solution A；
(b) cobaltous sulfate and sodium thiosulfate are sequentially added in solution A, and is stirred, obtains solution B；Wherein, cobaltous sulfate and
The molar concentration rate of disodium ethylene diamine tetraacetate is 1：0.1；The molar concentration rate of cobaltous sulfate and sodium thiosulfate is 1：1；
(c) pH value for adjusting solution B is 2；
(d) solution B after adjusting pH value is poured into reaction kettle, compactedness control is 60%, and adds in cobalt disulfide crystalline substance
Kind, after closed reactor, place it at 150 DEG C after middle reaction 6h, cooled to room temperature filters out bottom sediment, then
Respectively with dilute hydrochloric acid, carbon disulfide, absolute ethyl alcohol, deionized water rinsing, it is dried in vacuo at 60 DEG C up to pyrite
Cobalt disulfide powder；Wherein, the cobalt disulfide crystal seed of addition accounts for the gross mass of the cobalt disulfide powder of estimation final production
2%, grain size is about 15nm.
In the step (c), dilute hydrochloric acid is added in solution B or sodium hydroxide adjusts pH value.
Cobalt disulfide powder manufactured in the present embodiment is scanned through the pattern and grain size of electron microscopic observation sample, can substantially find
The good dispersion of gained cobalt disulfide powder, even particle size distribution.
Embodiment three
Contain in a kind of the step of synthetic method of cobalt disulfide powder, method：
(a) analytically pure disodium ethylene diamine tetraacetate is added in deionized water, fully dissolving obtains solution A；
(b) cobaltous sulfate and sodium thiosulfate are sequentially added in solution A, and is stirred, obtains solution B；Wherein, cobaltous sulfate and
The molar concentration rate of disodium ethylene diamine tetraacetate is 1：1；The molar concentration rate of cobaltous sulfate and sodium thiosulfate is 1：2；
(c) pH value for adjusting solution B is 11；
(d) solution B after adjusting pH value is poured into reaction kettle, compactedness control is 80%, and adds in cobalt disulfide crystalline substance
Kind, after closed reactor, place it at 240 DEG C after middle reaction 45h, cooled to room temperature filters out bottom sediment, then
Respectively with dilute hydrochloric acid, carbon disulfide, absolute ethyl alcohol, deionized water rinsing, it is dried in vacuo at 60 DEG C up to pyrite
Cobalt disulfide powder；Wherein, the cobalt disulfide crystal seed of addition accounts for the gross mass of the cobalt disulfide powder of estimation final production
5%, grain size is about 30nm.
Cobalt disulfide powder manufactured in the present embodiment is scanned through the pattern and grain size of electron microscopic observation sample, can substantially find
The good dispersion of gained cobalt disulfide powder, even particle size distribution.
Particular embodiments described above, pair present invention solves the technical problem that, technical solution and advantageous effect carry out
It is further described, it should be understood that the above is only a specific embodiment of the present invention, is not limited to this
Invention, within the spirit and principles of the invention, any modification, equivalent substitution, improvement and etc. done should be included in this hair
Within bright protection domain.
Claims (4)
1. a kind of synthetic method of cobalt disulfide powder, it is characterised in that contain in the step of method：
(a) analytically pure disodium ethylene diamine tetraacetate is added in deionized water, fully dissolving obtains solution A；
(b) cobaltous sulfate and sodium thiosulfate are sequentially added in solution A, and is stirred, obtains solution B；Wherein, cobaltous sulfate and second two
The molar concentration rate of amine tetraacethyl disodium is 1：(0~1)；The molar concentration rate of cobaltous sulfate and sodium thiosulfate is 1：(1~2)；
(c) pH value for adjusting solution B is 1~12；
(d) solution B after adjusting pH value is poured into reaction kettle, compactedness control is 60%-80%, and adds in cobalt disulfide crystalline substance
Kind, after closed reactor, place it at 140 DEG C -250 DEG C after middle reaction 5-50h, cooled to room temperature filters out bottom and sinks
Then starch is dried in vacuo at 60 DEG C with dilute hydrochloric acid, carbon disulfide, absolute ethyl alcohol, deionized water rinsing up to yellow iron respectively
The cobalt disulfide powder of ore deposit structure.
2. the synthetic method of cobalt disulfide powder according to claim 1, it is characterised in that：In the step (c),
Dilute hydrochloric acid is added in solution B or sodium hydroxide adjusts pH value.
3. the synthetic method of cobalt disulfide powder according to claim 1, it is characterised in that：In the step (d),
The grain size of the cobalt disulfide crystal seed of addition is 15-30nm.
4. the synthetic method of cobalt disulfide powder according to claim 1, it is characterised in that：In the step (d),
The cobalt disulfide crystal seed of addition accounts for the 1%~5% of the gross mass of the cobalt disulfide powder of estimation final production.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108927177A (en) * | 2018-06-06 | 2018-12-04 | 天津大学 | Graphene-supported cobalt disulfide particulate composite, preparation method and its usage |
| CN109603858A (en) * | 2018-12-14 | 2019-04-12 | 中国科学院海洋研究所 | A kind of double activated analogue enztme material and its preparation and application |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101786671A (en) * | 2009-10-30 | 2010-07-28 | 陕西科技大学 | Method for preparing bar-shaped cobalt sulfide nanocrystalline |
| CN101823769A (en) * | 2010-05-11 | 2010-09-08 | 新疆大学 | Method for preparing ternary FexCo1-xS2 powder |
-
2017
- 2017-12-20 CN CN201711386415.7A patent/CN108069461A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101786671A (en) * | 2009-10-30 | 2010-07-28 | 陕西科技大学 | Method for preparing bar-shaped cobalt sulfide nanocrystalline |
| CN101823769A (en) * | 2010-05-11 | 2010-09-08 | 新疆大学 | Method for preparing ternary FexCo1-xS2 powder |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108927177A (en) * | 2018-06-06 | 2018-12-04 | 天津大学 | Graphene-supported cobalt disulfide particulate composite, preparation method and its usage |
| CN109603858A (en) * | 2018-12-14 | 2019-04-12 | 中国科学院海洋研究所 | A kind of double activated analogue enztme material and its preparation and application |
| CN109603858B (en) * | 2018-12-14 | 2021-11-16 | 中国科学院海洋研究所 | Double-activity mimic enzyme material and preparation and application thereof |
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Application publication date: 20180525 |