CN110203977B - Preparation method of sodium-containing basic nickel carbonate - Google Patents
Preparation method of sodium-containing basic nickel carbonate Download PDFInfo
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- CN110203977B CN110203977B CN201810167145.9A CN201810167145A CN110203977B CN 110203977 B CN110203977 B CN 110203977B CN 201810167145 A CN201810167145 A CN 201810167145A CN 110203977 B CN110203977 B CN 110203977B
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Abstract
The invention discloses a preparation method of sodium-containing basic nickel carbonate, which comprises the steps of adding a sodium carbonate solution and a nickel sulfate solution into a reactor at the same time, and reacting to obtain basic nickel carbonate by adjusting the pH value of a flow control system of the sodium carbonate solution and the nickel sulfate solution to be 8.2-8.8 in the feeding process; stopping feeding, adjusting the reaction temperature, and controlling the formation of hydrated carbon nickel sodium crystal; after reacting for a certain time, feeding again, controlling the pH value and the reaction temperature of the system, promoting the growth of crystal nucleus and obtaining basic nickel carbonate containing sodium; in the synthesis process, crystal seeds of hydrated nickel-sodium carbonate are formed on the surface of the basic nickel carbonate by controlling the feeding time, the pH value of a reaction system, the reaction temperature and the reaction time, and the crystal seeds are controlled to grow to obtain the basic nickel carbonate containing sodium; the invention synthesizes a catalyst precursor which can stably provide 2-5% of sodium content.
Description
Technical Field
The invention belongs to an industrial preparation method of basic carbonate, and particularly relates to a preparation method of sodium-containing basic nickel carbonate.
Background
The basic carbonate can be applied to the fields of photocatalysis, supercapacitors and secondary batteries; the basic carbonate of nickel and cobalt has important application in the fields of electrode materials, catalysts, additives of electronic materials and magnetic materials, and the like.
The basic nickel carbonate is an important inorganic fine chemical and is mainly used for preparing various nickel salts, and the high-quality basic nickel carbonate can be applied to the electronic industry; in addition, the basic nickel carbonate is widely used in the industries of electroplating, electroforming, enamel pigments, industrial catalysts and the like.
In the prior art, usually, the prepared basic carbonate does not contain sodium, and for some special reactions, sodium ions provided by the catalyst have a better promotion effect on electron transfer in a catalytic reaction in the reaction process, but the sodium ions in the existing catalyst are adsorbed on the surface of a crystal, so that the stability of the combination of the sodium ions and the crystal is poor, the content of the sodium ions provided by the basic carbonate catalyst is difficult to control, and the stability of the content of the sodium provided by the basic carbonate catalyst is difficult to control, so that the catalytic performance of the basic carbonate is influenced.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention aims to provide a preparation method of basic nickel carbonate containing sodium.
The invention also provides a preparation method of the basic nickel carbonate containing sodium, which is implemented by the following steps:
step 1, adding a sodium carbonate solution and a nickel sulfate solution into a reactor at the same time, and reacting to obtain basic nickel carbonate by adjusting the pH value of a flow control system of the sodium carbonate solution and the nickel sulfate solution to be 8.2-8.3 in the feeding process;
step 3, adding the sodium carbonate solution and the nickel sulfate solution into the reactor again, controlling the pH value of a flow control system of the sodium carbonate solution and the nickel sulfate solution in the feeding process, and controlling the growth of the hydrated sodium nickel carbonate seed crystal obtained in the step 2 by adjusting the reaction temperature to obtain a sodium-containing basic nickel carbonate crude product;
and 4, sequentially aging, washing, drying and screening the crude product of the sodium-containing basic nickel carbonate obtained in the step 3 to obtain the sodium-containing basic nickel carbonate.
In the scheme, the concentration of the sodium carbonate solution in the step 1 is 180-300 g/L, and the concentration of the nickel sulfate solution in the step 1 is 60-100 g/L.
In the scheme, the flow rate of the sodium carbonate solution in the feeding process in the step 1 is 100-1000L/h, and the flow rate of the nickel sulfate solution is 100-1000L/h.
In the scheme, the reaction temperature in the step 1 is 60-90 ℃, and the reaction time is 20-25 h.
In the scheme, the reaction temperature in the step 2 is 50-60 ℃, and the reaction time is 30-60 min.
In the scheme, the pH value of the system in the step 3 is controlled to be 8.5-8.8.
In the scheme, the reaction temperature in the step 3 is 50-60 ℃, and the reaction time is 11-30 h.
In the scheme, the aging time in the step 4 is 0.5-3 h.
In the scheme, the washing in the step 4 is carried out by pure water, the temperature of the pure water is 70-85 ℃, and the conductivity of the pure water is less than or equal to 100 mu s/m.
In the scheme, the drying temperature in the step 4 is 95-105 ℃, and the drying time is 2-3 h; and 4, screening in the step 4 by adopting a 200-400-mesh screen.
Compared with the prior art, the invention provides a preparation method of basic nickel carbonate containing sodium, which comprises the steps of adding a sodium carbonate solution and a nickel sulfate solution into a reactor simultaneously, and reacting to obtain the basic nickel carbonate by adjusting the pH value of a flow control system of the sodium carbonate solution and the nickel sulfate solution to be 8.2-8.3 in the feeding process; stopping feeding, adjusting the reaction temperature, and controlling the formation of hydrated carbon nickel sodium crystal; after reacting for a certain time, feeding again, controlling the pH value and the reaction temperature of the system, promoting the growth of crystal nucleus and obtaining basic nickel carbonate containing sodium; in the synthesis process, crystal seeds of hydrated nickel-sodium carbonate are formed on the surface of the basic nickel carbonate by controlling the feeding time, the pH value of a reaction system, the reaction temperature and the reaction time, and the crystal seeds are controlled to grow to obtain the basic nickel carbonate containing sodium; sodium ions in the sodium-containing basic nickel carbonate synthesized by the method are embedded on the crystal face of the basic nickel carbonate, and the sodium content can be stably calculated according to the crystal seed amount, so that a catalyst precursor capable of stably providing 2-5% of the sodium content can be obtained, and the electron transfer in the catalyst reaction can be effectively promoted.
Drawings
Fig. 1 is a process flow diagram of a method for preparing basic nickel carbonate containing sodium according to an embodiment of the present invention;
FIG. 2 is an X-ray diffraction pattern of a sodium-containing basic nickel carbonate provided in example 1 of the present invention;
fig. 3 is a scanning electron microscope image of basic nickel carbonate containing sodium according to example 1 of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
The embodiment of the invention provides a preparation method of basic nickel carbonate, which has a process flow diagram as shown in fig. 1 and is implemented by the following steps:
step 1, simultaneously adding a sodium carbonate solution with the concentration of 180-300 g/L and a nickel sulfate solution with the concentration of 60-100 g/L into a reactor, adjusting the flow rate of the sodium carbonate solution to be 100-1000L/h and the flow rate of the nickel sulfate solution to be 100-1000L/h in the feeding process, so as to control the pH value of a system to be 8.2-8.3, and reacting for 20-25 h at the temperature of 60-90 ℃ to obtain basic nickel carbonate;
step 3, adding a sodium carbonate solution and a nickel sulfate solution into the reactor again, controlling the pH value of the system to be 8.5-8.8, reacting hydrated carbon nickel sodium seed crystals at 50-60 ℃ for 11-30 h, promoting the growth of crystal nuclei, and obtaining a basic nickel carbonate crude product containing sodium;
and 4, sequentially aging the sodium-containing basic nickel carbonate crude product obtained in the step 3 for 0.5-3 h, washing with pure water with the conductivity of less than or equal to 100 mu s/m and the temperature of 70-85 ℃, drying at 95-105 ℃ for 2-3 h, and finally screening with a 200-400-mesh sieve to obtain the sodium-containing basic nickel carbonate.
In the synthesis process, the surface energy of the basic nickel carbonate is reduced by controlling the feeding time, the pH value of a reaction system, the reaction temperature and the reaction time and adopting a mode of stopping feeding in the step 2, the structure of the basic nickel carbonate is favorably converted into a structure of hydrated sodium-carbonate-nickel in the continuous reaction, so that the crystal seed of the hydrated sodium-carbonate-nickel is obtained, sodium ions in the synthesized sodium-containing basic nickel carbonate are embedded on the crystal face of the basic nickel carbonate, the sodium content can be stably calculated according to the crystal seed amount, so that a catalyst precursor capable of stably providing 2-5% of the sodium content is obtained, and the electron transfer in the catalyst reaction can be effectively promoted.
Example 1
Embodiment 1 of the present invention provides a method for preparing basic nickel carbonate containing sodium, which is implemented by the following steps:
step 1, simultaneously adding a sodium carbonate solution with the concentration of 180g/L and a nickel sulfate solution with the concentration of 60g/L into a reactor, adjusting the flow rate of the sodium carbonate solution to be 100-1000L/h and the flow rate of the nickel sulfate solution to be 100-1000L/h in the feeding process, thereby controlling the pH value of a system to be 8.2, and reacting for 25h at the temperature of 60 ℃ to obtain basic nickel carbonate;
step 3, adding a sodium carbonate solution and a nickel sulfate solution into the reactor again, controlling the pH value of the system to be 8.6, and enabling the hydrated sodium nickel carbonate seed crystal to react for 25 hours at 55 ℃ to promote the growth of crystal nuclei to obtain a sodium-containing basic nickel carbonate crude product;
and 4, sequentially aging the crude sodium-containing basic nickel carbonate obtained in the step 3 for 1.5h, washing with pure water with the conductivity of less than or equal to 100 mu s/m and the temperature of 80 ℃, drying at 100 ℃ for 2h, and finally screening with a 200-400-mesh sieve to obtain the sodium-containing basic nickel carbonate.
An X-ray diffraction pattern and a scanning electron microscope pattern of the sodium-containing basic nickel carbonate provided in example 1 of the present invention are shown in fig. 2 and 3, and the chemical formula of the sodium-containing basic nickel carbonate is NaNi4(CO3)3(OH)3·3H2And O, compared with the prior art, the sodium-containing basic nickel carbonate obtained by adopting the synthesis process has the sodium content of 2.6 percent.
Example 2
step 1, simultaneously adding a sodium carbonate solution with the concentration of 180g/L and a nickel sulfate solution with the concentration of 60g/L into a reactor, adjusting the flow rate of the sodium carbonate solution to be 100-1000L/h and the flow rate of the nickel sulfate solution to be 100-1000L/h in the feeding process, thereby controlling the pH value of a system to be 8.3, and reacting for 22h at 75 ℃ to obtain basic nickel carbonate;
step 3, adding a sodium carbonate solution and a nickel sulfate solution into the reactor again, controlling the pH value of the system to be 8.6, and enabling the hydrated sodium nickel carbonate seed crystal to react for 25 hours at 55 ℃ to promote the growth of crystal nuclei to obtain a sodium-containing basic nickel carbonate crude product;
and 4, sequentially aging the crude sodium-containing basic nickel carbonate obtained in the step 3 for 1.5h, washing with pure water with the conductivity of less than or equal to 100 mu s/m and the temperature of 80 ℃, drying at 100 ℃ for 2h, and finally screening with a 200-400-mesh sieve to obtain the sodium-containing basic nickel carbonate.
Compared with the prior art, the sodium-containing basic nickel carbonate obtained by the synthesis process has the sodium content of 2.7 percent.
Example 3
Embodiment 3 of the present invention provides a method for preparing basic nickel carbonate containing sodium, which is implemented by the following steps:
step 1, simultaneously adding a sodium carbonate solution with the concentration of 180g/L and a nickel sulfate solution with the concentration of 60g/L into a reactor, adjusting the flow rate of the sodium carbonate solution to be 100-1000L/h and the flow rate of the nickel sulfate solution to be 100-1000L/h in the feeding process, thereby controlling the pH value of a system to be 8.3, and reacting for 20h at 90 ℃ to obtain basic nickel carbonate;
step 3, adding a sodium carbonate solution and a nickel sulfate solution into the reactor again, controlling the pH value of the system to be 8.6, and enabling the hydrated sodium nickel carbonate seed crystal to react for 25 hours at 55 ℃ to promote the growth of crystal nuclei to obtain a sodium-containing basic nickel carbonate crude product;
and 4, sequentially aging the crude sodium-containing basic nickel carbonate obtained in the step 3 for 1.5h, washing with pure water with the conductivity of less than or equal to 100 mu s/m and the temperature of 80 ℃, drying at 100 ℃ for 2h, and finally screening with a 200-400-mesh sieve to obtain the sodium-containing basic nickel carbonate.
Compared with the prior art, the sodium-containing basic nickel carbonate obtained by the synthesis process has the sodium content of 2.74 percent.
Example 4
Embodiment 4 of the present invention provides a method for preparing basic nickel carbonate containing sodium, which is implemented by the following steps:
step 1, simultaneously adding a sodium carbonate solution with the concentration of 200g/L and a nickel sulfate solution with the concentration of 80g/L into a reactor, adjusting the flow rate of the sodium carbonate solution to be 100-1000L/h and the flow rate of the nickel sulfate solution to be 100-1000L/h in the feeding process, thereby controlling the pH value of a system to be 8.3, and reacting for 20h at 60 ℃ to obtain basic nickel carbonate;
step 3, adding a sodium carbonate solution and a nickel sulfate solution into the reactor again, controlling the pH value of the system to be 8.6, and enabling the hydrated sodium nickel carbonate seed crystal to react for 28 hours at 50 ℃ to promote the growth of crystal nuclei to obtain a sodium-containing basic nickel carbonate crude product;
and 4, sequentially aging the crude sodium-containing basic nickel carbonate obtained in the step 3 for 1.5h, washing with pure water with the conductivity of less than or equal to 100 mu s/m and the temperature of 80 ℃, drying at 100 ℃ for 2h, and finally screening with a 200-400-mesh sieve to obtain the sodium-containing basic nickel carbonate.
Compared with the prior art, the sodium-containing basic nickel carbonate obtained by the synthesis process has the sodium content of 3.5%.
Example 5
Embodiment 5 of the present invention provides a method for preparing basic nickel carbonate containing sodium, which is implemented by the following steps:
step 1, simultaneously adding a sodium carbonate solution with the concentration of 200g/L and a nickel sulfate solution with the concentration of 80g/L into a reactor, adjusting the flow rate of the sodium carbonate solution to be 100-1000L/h and the flow rate of the nickel sulfate solution to be 100-1000L/h in the feeding process, thereby controlling the pH value of a system to be 8.3, and reacting for 20h at 60 ℃ to obtain basic nickel carbonate;
step 3, adding a sodium carbonate solution and a nickel sulfate solution into the reactor again, controlling the pH value of the system to be 8.6, and enabling the hydrated sodium nickel carbonate seed crystal to react for 20 hours at 55 ℃ to promote the growth of crystal nuclei to obtain a sodium-containing basic nickel carbonate crude product;
and 4, sequentially aging the crude sodium-containing basic nickel carbonate obtained in the step 3 for 1.5h, washing with pure water with the conductivity of less than or equal to 100 mu s/m and the temperature of 80 ℃, drying at 100 ℃ for 2h, and finally screening with a 200-400-mesh sieve to obtain the sodium-containing basic nickel carbonate.
Compared with the prior art, the sodium-containing basic nickel carbonate obtained by the synthesis process has the sodium content of 3.2%.
Example 6
Embodiment 6 of the present invention provides a method for preparing basic nickel carbonate containing sodium, which is implemented by the following steps:
step 1, simultaneously adding a sodium carbonate solution with the concentration of 200g/L and a nickel sulfate solution with the concentration of 80g/L into a reactor, adjusting the flow rate of the sodium carbonate solution to be 100-1000L/h and the flow rate of the nickel sulfate solution to be 100-1000L/h in the feeding process, thereby controlling the pH value of a system to be 8.3, and reacting for 20h at 60 ℃ to obtain basic nickel carbonate;
step 3, adding a sodium carbonate solution and a nickel sulfate solution into the reactor again, controlling the pH value of the system to be 8.6, and enabling the hydrated sodium nickel carbonate seed crystal to react for 11 hours at 60 ℃ to promote the growth of crystal nuclei to obtain a sodium-containing basic nickel carbonate crude product;
and 4, sequentially aging the crude sodium-containing basic nickel carbonate obtained in the step 3 for 1.5h, washing with pure water with the conductivity of less than or equal to 100 mu s/m and the temperature of 80 ℃, drying at 100 ℃ for 2h, and finally screening with a 200-400-mesh sieve to obtain the sodium-containing basic nickel carbonate.
Compared with the prior art, the sodium-containing basic nickel carbonate obtained by the synthesis process has the sodium content of 3.52 percent.
Example 7
Embodiment 7 of the present invention provides a method for preparing basic nickel carbonate containing sodium, which is implemented by the following steps:
step 1, simultaneously adding a sodium carbonate solution with the concentration of 300g/L and a nickel sulfate solution with the concentration of 100g/L into a reactor, adjusting the flow rate of the sodium carbonate solution to be 100-1000L/h and the flow rate of the nickel sulfate solution to be 100-1000L/h in the feeding process, thereby controlling the pH value of a system to be 8.2, and reacting for 20h at 80 ℃ to obtain basic nickel carbonate;
step 3, adding a sodium carbonate solution and a nickel sulfate solution into the reactor again, controlling the pH value of the system to be 8.6, and enabling the hydrated sodium nickel carbonate seed crystal to react for 25 hours at 50 ℃ to promote the growth of crystal nuclei to obtain a sodium-containing basic nickel carbonate crude product;
and 4, sequentially aging the crude sodium-containing basic nickel carbonate obtained in the step 3 for 0.5h, washing with pure water with the conductivity of less than or equal to 100 mu s/m and the temperature of 70 ℃, drying at 95 ℃ for 3h, and finally screening with a 200-400-mesh sieve to obtain the sodium-containing basic nickel carbonate.
Compared with the prior art, the sodium-containing basic nickel carbonate obtained by the synthesis process has the sodium content of 4.9%.
Example 8
Embodiment 8 of the present invention provides a method for preparing basic nickel carbonate containing sodium, which is implemented by the following steps:
step 1, simultaneously adding a sodium carbonate solution with the concentration of 300g/L and a nickel sulfate solution with the concentration of 100g/L into a reactor, adjusting the flow rate of the sodium carbonate solution to be 100-1000L/h and the flow rate of the nickel sulfate solution to be 100-1000L/h in the feeding process, thereby controlling the pH value of a system to be 8.2, and reacting for 20h at 80 ℃ to obtain basic nickel carbonate;
step 3, adding a sodium carbonate solution and a nickel sulfate solution into the reactor again, controlling the pH value of the system to be 8.6, and enabling the hydrated sodium nickel carbonate seed crystal to react for 25 hours at 50 ℃ to promote the growth of crystal nuclei to obtain a sodium-containing basic nickel carbonate crude product;
and 4, sequentially aging the crude sodium-containing basic nickel carbonate obtained in the step 3 for 2 hours, washing with pure water with the conductivity of less than or equal to 100 mu s/m and the temperature of 80 ℃, drying at 100 ℃ for 3 hours, and finally screening with a 200-400-mesh sieve to obtain the sodium-containing basic nickel carbonate.
Compared with the prior art, the sodium-containing basic nickel carbonate obtained by the synthesis process has the sodium content of 5.0%.
Example 9
Embodiment 9 of the present invention provides a method for preparing basic nickel carbonate containing sodium, which is implemented by the following steps:
step 1, simultaneously adding a sodium carbonate solution with the concentration of 300g/L and a nickel sulfate solution with the concentration of 100g/L into a reactor, adjusting the flow rate of the sodium carbonate solution to be 100-1000L/h and the flow rate of the nickel sulfate solution to be 100-1000L/h in the feeding process, thereby controlling the pH value of a system to be 8.2, and reacting for 20h at 80 ℃ to obtain basic nickel carbonate;
step 3, adding a sodium carbonate solution and a nickel sulfate solution into the reactor again, controlling the pH value of the system to be 8.6, and enabling the hydrated sodium nickel carbonate seed crystal to react for 25 hours at 50 ℃ to promote the growth of crystal nuclei to obtain a sodium-containing basic nickel carbonate crude product;
and 4, sequentially aging the crude sodium-containing basic nickel carbonate obtained in the step 3 for 3 hours, washing with pure water with the conductivity of less than or equal to 100 mu s/m and the temperature of 85 ℃, drying at 105 ℃ for 2 hours, and finally screening with a 200-400-mesh sieve to obtain the sodium-containing basic nickel carbonate.
Compared with the prior art, the sodium-containing basic nickel carbonate obtained by the synthesis process has the sodium content of 5.1%.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the scope of the present invention.
Claims (1)
1. A preparation method of basic nickel carbonate containing sodium is characterized by comprising the following steps:
step 1, adding a sodium carbonate solution with the concentration of 180-300 g/L and a nickel sulfate solution with the concentration of 60-100 g/L into a reactor at the same time, adjusting the flow rate of the sodium carbonate solution to be 100-1000L/h and the flow rate of the nickel sulfate solution to be 100-1000L/h in the feeding process, so as to control the pH value of a system to be 8.2-8.3, and reacting for 20-25 h at the temperature of 60-90 ℃ to obtain basic nickel carbonate;
step 2, stopping adding the sodium carbonate solution and the nickel sulfate solution into the reactor, reacting the basic nickel carbonate obtained in the step 1 at 50-60 ℃ for 30-60 min, and transforming the crystal form to obtain hydrated carbon nickel sodium seed crystals;
step 3, adding the sodium carbonate solution and the nickel sulfate solution into the reactor again, adjusting the pH value of a flow control system of the sodium carbonate solution and the nickel sulfate solution to 8.5-8.8 in the feeding process, adjusting the reaction temperature to 50-60 ℃ and the reaction time to 11-30 h, and controlling the growth of the hydrated nickel sodium carbonate crystal seed obtained in the step 2 to obtain a basic nickel carbonate crude product containing sodium;
step 4, sequentially aging the sodium-containing basic nickel carbonate crude product obtained in the step 3 for 0.5-3 h, and washing with pure water at the temperature of 70-85 ℃ and the conductivity of less than or equal to 100 mu s/m; drying for 2-3 h at 95-105 ℃; and finally, sieving by using a 200-400-mesh sieve to obtain the sodium-containing basic nickel carbonate.
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CN101016173A (en) * | 2006-12-29 | 2007-08-15 | 金川集团有限公司 | Method of preparing electronic grade nickel carbonate by sodium carbonate deposition |
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CN101708868A (en) * | 2009-11-20 | 2010-05-19 | 江西核工业兴中科技有限公司 | Process for rapidly producing basic nickel carbonate or basic cobaltous carbonate |
CN102923794A (en) * | 2012-11-23 | 2013-02-13 | 长沙矿冶研究院有限责任公司 | Method for continuously compounding high-purity alkali nickel carbonate |
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