CN103387488A - Preparation method of square cobalt oxalate powder - Google Patents
Preparation method of square cobalt oxalate powder Download PDFInfo
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- CN103387488A CN103387488A CN201210145540XA CN201210145540A CN103387488A CN 103387488 A CN103387488 A CN 103387488A CN 201210145540X A CN201210145540X A CN 201210145540XA CN 201210145540 A CN201210145540 A CN 201210145540A CN 103387488 A CN103387488 A CN 103387488A
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Abstract
The invention discloses a preparation method of square cobalt oxalate powder. The method comprises the following steps: adding a surface modifying agent to a cobalt chloride solid, sequentially adding an oxalic acid solid and distilled water, carrying out constant temperature stirring for a precipitation reaction of the obtained mixture solution, carrying out solid-liquid separation to obtain precipitated powder, washing the obtained powder, and drying to prepare the square cobalt oxalate powder. The method which utilizes oxalic acid as a precipitating agent has the advantages of no need of the pH value adjustment, simple operation flow, high production efficiency, and extremely small impurity content. The prepared cobalt oxalate powder has a particle size of 0.2-10mum, and has uniform particle distribution.
Description
Technical field
The present invention relates to field of metallurgy and chemical engineering, more specifically relate to a kind of manufacture method of cobalt oxalate.
Background technology
There are two weakness in the method for existing production cobalt oxalate: 1, due to the discharging of ammonia nitrogens in a large number, cause serious environmental pollution, although also can process again its discharging, but processing costs is high, part domestic manufacturer adopts thin up at present, with directly produce contain ammonia nitrogen approximately the waste liquid of 2 grams per liters be diluted to and meet GB (directly discharging environment) 2.5 mg/litre, the amount of dilution of its water reaches 800～1000 times; 2, the pattern state difference of cobalt oxalate powder: the concrete pattern of cobalt oxalate powder is needle-like or dendroid, causes the cobalt oxide of sintering or the cobalt powder of reduction also to inherit this similar shape, has affected the application performance of cobalt oxide or cobalt powder.It is unfavorable that product under this pattern has brought application in the future, as: there are the shortcomings such as batch mixing is inhomogeneous, dust from flying is large, mobility of particle is poor, tamped density is low, specific surface area is little in dendritic cobalt powder aspect the alloy compacting.
Summary of the invention
The present invention proposes a kind of manufacture method of square cobalt oxalate.
According to an aspect of the present invention, provide a kind of manufacture method of square cobalt oxalate, comprise the steps,
Step 1: add coating materials in the cobalt chloride solid, then add the oxalic acid solid;
Step 2: drip distilled water in the mixture of step 1 gained, constant temperature stirs and impels mixture solution generation precipitin reaction;
Step 3: the solution of abundant precipitin reaction is carried out solid-liquid separation, obtain the powder of precipitation;
Step 4: washing gained powder carries out drying again, makes square cobalt oxalate powder.
In some embodiments, coating materials is analytically pure methyl alcohol or ethanol.
In some embodiments, the purity of methyl alcohol and ethanol is technical pure.
In some embodiments, in step 2, the time of controlling the reaction of mixing solutions is 20～60 minutes.
In some embodiments, in step 2, constant temperature is 35～45 ℃.
In some embodiments, in step 4, dry temperature is 80～110 ℃, and be 4～6 hours time of drying.
Use methyl alcohol or ethanol organic solvent to make surperficial modifier in the present invention, the cobalt oxalate product is square structure, size between 0.2～10 μ m, even particle distribution; Production process is carried out under neutrallty condition, do not need to regulate the pH value, and operating process is simple, production efficiency is high, foreign matter content is few; Do not use in process of production ammonia nitrogen, emit environmentally safe without amine substance.Cobalt ion and the oxalate denominationby of the free shape of the adsorbable cobalt oxalate plane of crystal of coating materials, prevent that crystal from being club shaped structure at the preferred growth of a direction, and this growth pattern can obtain square cobalt oxalate powder.
Description of drawings
Figure 1 – Fig. 6 is the Electronic Speculum figure of square cobalt oxalate of embodiment 1 gained of the manufacture method of the square cobalt oxalate of the present invention;
Figure 7 – Figure 12 are Electronic Speculum figure of square cobalt oxalate of embodiment 2 gained of the manufacture method of the square cobalt oxalate of the present invention;
Figure 13 is the X-ray diffraction result of square cobalt oxalate of embodiment 2 gained of the manufacture method of the square cobalt oxalate of the present invention;
Figure 14 is the standard spectrogram of β type structure;
Figure 15 is the size distribution figure of square cobalt oxalate of embodiment 1 gained of the manufacture method of the square cobalt oxalate of the present invention;
Figure 16 is the size distribution figure of square cobalt oxalate of embodiment 2 gained of the manufacture method of the square cobalt oxalate of the present invention.
Embodiment
1mol cobalt chloride solid is added in the analytically pure ethanol of 50mL coating materials, at 40 ℃ of stirred in water bath mixtures; Add again 1mol oxalic acid solid, be uniformly mixed.Low whipping speed is under the condition of 100 rev/mins, slowly drips 2L distilled water in mixture, drips in 30 minutes.Water to be distilled dropwises, and the mixing solutions of gained was in 55 ℃ of stirred in water bath reactions 30 minutes, and reaction finishes, and obtains pink suspension.With suspension vacuum filtration, washing 4 times.Obtained square cobalt oxalate powder as shown in Figure 6 in figure 1 – in dry 4 hours under 110 ℃ of conditions, and unconventional bar-shaped or dendritic cobalt oxalate.Fig. 1 to Fig. 6 is the scanning electron microscope (SEM) photograph of cobalt oxalate powder under each magnification, can find out that cobalt oxalate powder is evenly distributed, and there is no the phenomenon of reuniting.As shown in figure 15, the particle diameter of the cobalt oxalate powder that obtains is evenly distributed between 0.2～10 μ m, distributes more even.
Embodiment 2
With adding in 1mol cobalt chloride solid in the analytically pure methyl alcohol of 50mL coating materials, at 40 ℃ of stirred in water bath mixtures; Add again 1mol oxalic acid solid, be uniformly mixed.Low whipping speed is under the condition of 100 rev/mins, slowly drips 2L distilled water in mixture, drips in 30 minutes.Water to be distilled dropwises, and the mixing solutions of gained was in 45 ℃ of stirred in water bath reactions 20 minutes, and reaction finishes, and obtains pink suspension.With suspension vacuum filtration, washing 4 times.Under 80 ℃ of conditions, drying is 6 hours, obtains square cobalt oxalate powder as shown in Figure 12 in figure 7 –.Fig. 7 to Figure 12 is the scanning electron microscope (SEM) photograph of cobalt oxalate powder under each magnification, can find out that cobalt oxalate powder is evenly distributed, and there is no the phenomenon of reuniting.Figure 13 is the X-ray diffraction result of this powder, and the β type construction standard spectrogram contrast with Figure 14, prove that its structure is typical β type cobalt oxalate.As shown in figure 16, the particle diameter of the cobalt oxalate powder that obtains is evenly distributed between 0.2～10 μ m, distributes more even.
Embodiment 3
With adding in 1mol cobalt chloride solid in the analytically pure ethanol of 50mL coating materials, 40 ℃ of stirred in water bath; Add again 1mol oxalic acid solid, be uniformly mixed.Low whipping speed is under the condition of 100 rev/mins, slowly drips 2L distilled water in mixture, drips in 30 minutes.Water to be distilled dropwises, and the mixing solutions of gained was in 35 ℃ of stirred in water bath reactions 60 minutes, and reaction finishes, and obtains pink suspension.With suspension vacuum filtration, washing 4 times.Obtained square cobalt oxalate powder in dry 5 hours under 90 ℃ of conditions, and unconventional bar-shaped or dendritic cobalt oxalate.
Embodiment 4
With adding in 1mol cobalt chloride solid in the analytically pure methyl alcohol of 50mL coating materials, 40 ℃ of stirred in water bath; Add again 1mol oxalic acid solid, be uniformly mixed.Low whipping speed is under the condition of 100 rev/mins, slowly drips 2L distilled water in mixture, drips in 30 minutes.Water to be distilled dropwises, and mixing solutions was in 40 ℃ of stirred in water bath reactions 40 minutes, and reaction finishes, and obtains pink suspension.With suspension vacuum filtration, washing 4 times.Obtained square cobalt oxalate powder in dry 4.5 hours under 100 ℃ of conditions, and unconventional bar-shaped or dendritic cobalt oxalate.
Above-described is only some embodiments of the present invention, should be pointed out that for the person of ordinary skill of the art, under the prerequisite that does not break away from creation design of the present invention, can also make other distortion and improvement, and these all belong to protection scope of the present invention.
Claims (7)
1. the manufacture method of square cobalt oxalate powder, is characterized in that, comprise the following steps,
Step 1: add coating materials in the cobalt chloride solid, then add the oxalic acid solid;
Step 2: drip distilled water under constant temperature in the mixture of step 1 gained, form mixed solution, stir and impel mixture solution generation precipitin reaction under constant temperature;
Step 3: the solution of abundant precipitin reaction is carried out solid-liquid separation, obtain throw out;
Step 4: washing gained throw out, carry out drying, make square cobalt oxalate powder.
2. the manufacture method of square cobalt oxalate powder according to claim 1, is characterized in that, described coating materials is selected methyl alcohol or ethanol.
3. the manufacture method of square cobalt oxalate powder according to claim 2, is characterized in that, the purity of described methyl alcohol and ethanol is technical pure.
4. the manufacture method of square cobalt oxalate powder according to claim 1, is characterized in that, in described step 2, the time of the precipitin reaction of mixing solutions is 20～60 minutes.
5. according to claim 1, the manufacture method of 2,3 or 4 described square cobalt oxalate powders, it is characterized in that, in described step 2, described constant temperature is 35～45 ℃.
6. according to claim 1, the manufacture method of 2,3 or 4 described square cobalt oxalate powders, it is characterized in that, in described step 4, dry temperature is 80～110 ℃, be 4～6 hours time of drying.
7. the manufacture method of square cobalt oxalate powder according to claim 5, is characterized in that, in described step 4, dry temperature is 80～110 ℃, and be 4～6 hours time of drying.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3803191A (en) * | 1971-03-24 | 1974-04-09 | Graham Magnetics Inc | Acicular salts and their preparation |
| US6464750B1 (en) * | 1999-06-10 | 2002-10-15 | Asb Aerospatiale Batteries | Method of preparing metal powders, metal powders prepared in this way and compacts that include these powders |
| CN101781186A (en) * | 2009-01-21 | 2010-07-21 | 尤米科尔公司 | Cobalt oxalate powder and its application for producing co powder with superior cold compression and sintering characters |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3803191A (en) * | 1971-03-24 | 1974-04-09 | Graham Magnetics Inc | Acicular salts and their preparation |
| US6464750B1 (en) * | 1999-06-10 | 2002-10-15 | Asb Aerospatiale Batteries | Method of preparing metal powders, metal powders prepared in this way and compacts that include these powders |
| CN101781186A (en) * | 2009-01-21 | 2010-07-21 | 尤米科尔公司 | Cobalt oxalate powder and its application for producing co powder with superior cold compression and sintering characters |
Non-Patent Citations (2)
| Title |
|---|
| 袁平: "草酸钴沉淀工艺对钴粉粒影响的研究", 《硬质合金》 * |
| 高晋: "前驱物颗粒的形貌对钴粉形貌的影响", 《稀有金属与硬质合金》 * |
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Effective date of registration: 20170411 Address after: 214121 Jiangsu City, Wuxi Province, Lake Road, stone road, No. Venice Garden District, apartment building, room 607, room 2, Room 502 Patentee after: Wuxi city Naimitexin Material Co. Ltd. Address before: 214000 Xishan City, Wuxi Province, an area of the town of rubber Village Street Patentee before: Wuxi Shunye Technology Co., Ltd. |