CN110894082B - Preparation method of large-particle nickel sulfate crystal - Google Patents
Preparation method of large-particle nickel sulfate crystal Download PDFInfo
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- CN110894082B CN110894082B CN201811063511.2A CN201811063511A CN110894082B CN 110894082 B CN110894082 B CN 110894082B CN 201811063511 A CN201811063511 A CN 201811063511A CN 110894082 B CN110894082 B CN 110894082B
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- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G53/00—Compounds of nickel
- C01G53/10—Sulfates
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Abstract
The invention discloses a preparation method of large-particle nickel sulfate crystals, which comprises the steps of adding a nickel sulfate solution into a concentration kettle, heating and concentrating at a heating rate of 0.5-2 ℃/min until the concentration of the nickel sulfate solution reaches 55-65 Baume degrees to obtain a first solution, transferring the first solution into a crystallization kettle for cooling crystallization, controlling the cooling rate until the cooling temperature is reduced to 60 +/-2 ℃, adding a nickel sulfate seed crystal into the first solution, and then sequentially performing aging crystallization, centrifugal separation and drying to obtain nickel sulfate crystals; therefore, the method can effectively solve the problems of poor crystal shape, small particle size and uneven particle size distribution of nickel sulfate crystals by strictly controlling the cooling rate and the cooling temperature and also strictly controlling the adding time and the adding proportion of the nickel sulfate crystal seeds, and obtain the nickel sulfate crystals with large particle size and uniform particle size and large particles.
Description
Technical Field
The invention belongs to the technical field of nickel sulfate preparation, and particularly relates to a preparation method of large-particle nickel sulfate crystals.
Background
The nickel sulfate is widely used in industries of semiconductors, Printed Circuit Boards (PCBs), batteries, chemical plating, electroplating and the like, is a main nickel salt of electroplated nickel and alloy, chemical nickel plating and alloy and batteries, is also a main source of metal nickel ions, and can also be used as an additive in cadmium plating and zinc plating. In the inorganic industry as nickel catalysts and other nickel salts such as nickel chloride, nickel oxide, nickel carbonate, etc. It is also used for manufacturing nickel-cadmium batteries, catalysts for hardened oil or paint, mordants for reducing dyes, metal colorants, and the like.
At present, a concentration crystallization method is generally adopted in the production of nickel sulfate in China, the crystallization process is controlled by adjusting the pH value and adding seed crystals, but the supersaturation degree in the crystallization process is still overlarge, and the variable control on the nickel sulfate crystallization process in China is relatively extensive, so that the crystal form of a product is poor, the appearance is powdery, matt, small in particle size and easy to form lumps; this results on the one hand in filtration difficulties and low single-pass yields and on the other hand in low purity and content of the product.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention aims to provide a preparation method of large-particle nickel sulfate crystals.
The invention provides a preparation method of large-particle nickel sulfate crystals, which is implemented by the following steps:
step 1, adding a nickel sulfate solution into a concentration kettle, and heating and concentrating at a heating rate of 0.5-2 ℃/min until the concentration of the nickel sulfate solution reaches 55-65 Baume degrees to obtain a first solution;
and 2, transferring the first solution obtained in the step 1 into a crystallization kettle for cooling crystallization, controlling the cooling rate until the cooling temperature is reduced to 60 +/-2 ℃, adding nickel sulfate seed crystals into the first solution, and then sequentially performing aging crystallization, centrifugal separation and drying to obtain nickel sulfate crystals.
In the scheme, the nickel content in the nickel sulfate solution in the step 1 is not lower than 80 g/L.
In the above scheme, the stirring is performed at a stirring frequency of 5Hz during the heating concentration in the step 1.
In the scheme, the cooling rate in the step 2 is 15-25 ℃/h.
In the scheme, the proportion of the nickel sulfate seed crystals added in the step 2 in the first solution is 10-15 Kg/m3。
In the scheme, the nickel sulfate crystal seed in the step 2 is undersize materials which are sieved by a 50-mesh sieve.
In the scheme, the stirring is carried out at a stirring frequency of 5Hz and a rotating speed of 60-80 rmp/min in the process of cooling and crystallizing in the step 2.
In the scheme, the temperature for aging and crystallizing in the step 2 is 50-70 ℃, and the time is 1-3 h.
In the scheme, the rotation frequency of the centrifugal machine in the step 2 during centrifugal separation is 40-50 Hz, and the rotation speed is 1200-1500 rmp/min.
In the scheme, the drying temperature in the step 2 is 55-65 ℃.
Compared with the prior art, the method has the advantages that the concentration of the nickel sulfate solution used as the raw material is controlled, the cooling rate and the cooling temperature are strictly controlled in the cooling crystallization process, the adding time and the adding proportion of the nickel sulfate seed crystal are strictly controlled, the phenomena of poor crystallization shape, small particle size and uneven particle size distribution of nickel sulfate crystals can be effectively solved, the phenomena of nickel sulfate crystal agglomeration and powder existing in the nickel sulfate crystals are avoided, the nickel sulfate crystals with large particle sizes and uniform particle sizes can be obtained, and the impurity content of finished nickel sulfate crystals is low.
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 do not limit the invention.
The embodiment of the invention provides a preparation method of large-particle nickel sulfate crystals, which is implemented by the following steps:
step 1, adding a nickel sulfate solution into a concentration kettle, wherein the nickel content in the nickel sulfate solution is not lower than 80g/L, then heating and concentrating at a heating rate of 0.5-2 ℃/min, and continuously stirring at a stirring frequency of 5Hz in the heating and concentrating process until the concentration of the nickel sulfate solution reaches 55-65 Baume degrees, so as to obtain a first solution;
step 2, transferring the first solution obtained in the step 1 into a crystallization kettle for cooling crystallization, cooling at a cooling rate of 15-25 ℃/h until the cooling temperature is reduced to 60 +/-2 ℃, treating nickel sulfate seed crystals by adopting a 50-mesh screen, adding the treated nickel sulfate seed crystals into the first solution, wherein the nickel sulfate seed crystals are added in a proportion of 10-15 Kg/m of the first solution3Stirring at a stirring frequency of 5Hz and a rotating speed of 60-80 rmp/min in the cooling crystallization process, then sequentially stirring at a temperature of 50-70 ℃ for 1-3 h, and then adjusting the rotating frequency of a centrifugal machine to be 40-50 Hz and the rotating speed Performing centrifugal separation at 1200-1500 rmp/mi, and finally drying at 55-65 ℃ to obtain nickel sulfate crystals.
According to the invention, the concentration of the nickel sulfate solution used as the raw material is controlled, the cooling rate and the cooling temperature are strictly controlled in the cooling crystallization process, the time for adding the nickel sulfate seed crystal and the adding proportion are strictly controlled, the phenomena of poor nickel sulfate crystal shape, small particle size and uneven particle size distribution can be effectively solved, the phenomena of nickel sulfate crystal agglomeration and powder existing in the nickel sulfate crystal are avoided, the nickel sulfate crystal with large particle size and even particle size and uniform large particle size can be obtained, the impurity content of the finished product of the nickel sulfate crystal is low, and the average particle size of the obtained nickel sulfate crystal is 2-3 mm.
Example 1
The embodiment 1 of the invention provides a preparation method of large-particle nickel sulfate crystals, which is implemented by the following steps:
step 1, adding a nickel sulfate solution into a concentration kettle, wherein the nickel content in the nickel sulfate solution is not lower than 80g/L, then heating and concentrating at a heating rate of 0.5 ℃/min, and continuously stirring at a stirring frequency of 5Hz in the heating and concentrating process until the concentration of the nickel sulfate solution reaches 55 Baume degrees, so as to obtain a first solution;
Step 2, transferring the first solution obtained in the step 1 into a crystallization kettle for cooling crystallization, cooling at a cooling rate of 20 ℃/h until the cooling temperature is reduced to 60 ℃, treating nickel sulfate seed crystals by adopting a 50-mesh screen, adding the treated nickel sulfate seed crystals into the first solution, wherein the nickel sulfate seed crystals are added in a proportion of 12Kg/m of the first solution3Stirring at a stirring frequency of 5Hz and a rotating speed of 68rmp/min in the cooling crystallization process, then sequentially stirring at 60 ℃ for 2h, then adjusting the rotating frequency of a centrifugal machine to be 40-50 Hz and the rotating speed to be 1350rmp/mi for centrifugal separation, and finally drying at 60 ℃ to obtain nickel sulfate crystals.
Compared with the prior art, the nickel sulfate crystal obtained by adopting the synthesis process has the average grain diameter of 2-3 mm.
Example 2
The embodiment 2 of the invention provides a preparation method of large-particle nickel sulfate crystals, which is implemented by the following steps:
step 1, adding a nickel sulfate solution into a concentration kettle, wherein the nickel content in the nickel sulfate solution is not lower than 80g/L, heating and concentrating at a heating rate of 1 ℃/min, and continuously stirring at a stirring frequency of 5Hz in the heating and concentrating process until the concentration of the nickel sulfate solution reaches 60 baume degrees to obtain a first solution;
Step 2, transferring the first solution obtained in the step 1 into a crystallization kettle for cooling crystallization, cooling at a cooling rate of 20 ℃/h until the cooling temperature is reduced to 60 ℃, treating nickel sulfate seed crystals by adopting a 50-mesh screen, adding the treated nickel sulfate seed crystals into the first solution, wherein the nickel sulfate seed crystals are added in a proportion of 12Kg/m of the first solution3Stirring at a stirring frequency of 5Hz and a rotating speed of 68rmp/min in the cooling crystallization process, then sequentially stirring at 60 ℃ for 2h, then adjusting the rotating frequency of a centrifugal machine to be 40-50 Hz and the rotating speed to be 1350rmp/mi for centrifugal separation, and finally drying at 60 ℃ to obtain nickel sulfate crystals.
Compared with the prior art, the nickel sulfate crystal obtained by adopting the synthesis process has the average grain diameter of 2-3 mm.
Example 3
Embodiment 3 of the present invention provides a method for preparing large-particle nickel sulfate crystals, which is implemented by the following steps:
step 1, adding a nickel sulfate solution into a concentration kettle, wherein the nickel content in the nickel sulfate solution is not lower than 80g/L, heating and concentrating at a heating rate of 2 ℃/min, and continuously stirring at a stirring frequency of 5Hz in the heating and concentrating process until the concentration of the nickel sulfate solution reaches 65 baume degrees to obtain a first solution;
Step 2, transferring the first solution obtained in the step 1 into a crystallization kettle for cooling crystallization, cooling at a cooling rate of 20 ℃/h until the cooling temperature is reduced to 60 ℃, treating nickel sulfate crystal seeds by adopting a 50-mesh screen, and adding the treated nickel sulfate crystal seeds into the first solutionThe nickel sulfate seed crystal is added, and the proportion of the nickel sulfate seed crystal in the first solution is 12Kg/m3Stirring at a stirring frequency of 5Hz and a rotating speed of 68rmp/min in the cooling crystallization process, then sequentially stirring at 60 ℃ for 2h, then adjusting the rotating frequency of a centrifugal machine to be 40-50 Hz and the rotating speed to be 1350rmp/mi for centrifugal separation, and finally drying at 60 ℃ to obtain nickel sulfate crystals.
Compared with the prior art, the nickel sulfate crystal obtained by adopting the synthesis process has the average grain diameter of 2-3 mm.
Example 4
Embodiment 4 of the present invention provides a method for preparing large-particle nickel sulfate crystals, which is implemented by the following steps:
step 1, adding a nickel sulfate solution into a concentration kettle, wherein the nickel content in the nickel sulfate solution is not lower than 80g/L, then heating and concentrating at a heating rate of 1.2 ℃/min, and continuously stirring at a stirring frequency of 5Hz in the heating and concentrating process until the concentration of the nickel sulfate solution reaches 62 Baume degrees to obtain a first solution;
Step 2, transferring the first solution obtained in the step 1 into a crystallization kettle for cooling crystallization, cooling at a cooling rate of 15 ℃/h until the cooling temperature is reduced to 58 ℃, treating nickel sulfate seed crystals by adopting a 50-mesh screen, adding the treated nickel sulfate seed crystals into the first solution, wherein the nickel sulfate seed crystals are added in a proportion of 10Kg/m of the first solution3Stirring at a stirring frequency of 5Hz and a rotating speed of 60rmp/min in the cooling crystallization process, then sequentially stirring at 60 ℃ for 2h, then adjusting the rotating frequency of a centrifugal machine to be 40-50 Hz and the rotating speed of 1380rmp/mi for centrifugal separation, and finally drying at 61 ℃ to obtain the nickel sulfate crystal.
Compared with the prior art, the nickel sulfate crystal obtained by adopting the synthesis process has the average grain diameter of 2-3 mm.
Example 5
Embodiment 5 of the present invention provides a method for preparing large-particle nickel sulfate crystals, which is implemented by the following steps:
step 1, adding a nickel sulfate solution into a concentration kettle, wherein the nickel content in the nickel sulfate solution is not lower than 80g/L, then heating and concentrating at a heating rate of 1.2 ℃/min, and continuously stirring at a stirring frequency of 5Hz in the heating and concentrating process until the concentration of the nickel sulfate solution reaches 62 Baume degrees to obtain a first solution;
Step 2, transferring the first solution obtained in the step 1 into a crystallization kettle for cooling crystallization, cooling at a cooling rate of 20 ℃/h until the cooling temperature is reduced to 60 ℃, treating nickel sulfate seed crystals by adopting a 50-mesh screen, adding the treated nickel sulfate seed crystals into the first solution, wherein the nickel sulfate seed crystals are added in a proportion of 13Kg/m of the first solution3Stirring at a stirring frequency of 5Hz and a rotating speed of 70rmp/min in the cooling crystallization process, then sequentially stirring at 60 ℃ for 2h, then adjusting the rotating frequency of a centrifugal machine to be 40-50 Hz and the rotating speed to be 1380rmp/mi for centrifugal separation, and finally drying at 61 ℃ to obtain the nickel sulfate crystal.
Compared with the prior art, the nickel sulfate crystal obtained by adopting the synthesis process has the average grain diameter of 2-3 mm.
Example 6
Embodiment 6 of the present invention provides a method for preparing large-particle nickel sulfate crystals, which is implemented by the following steps:
step 1, adding a nickel sulfate solution into a concentration kettle, wherein the nickel content in the nickel sulfate solution is not lower than 80g/L, then heating and concentrating at a heating rate of 1.2 ℃/min, and continuously stirring at a stirring frequency of 5Hz in the heating and concentrating process until the concentration of the nickel sulfate solution reaches 62 Baume degrees, so as to obtain a first solution;
Step 2, transferring the first solution obtained in the step 1 into a crystallization kettle for cooling crystallization, cooling at a cooling rate of 25 ℃/h until the cooling temperature is reduced to 62 ℃, treating nickel sulfate seed crystals by adopting a 50-mesh screen, adding the treated nickel sulfate seed crystals into the first solution, wherein the nickel sulfate seed crystals are added in a proportion of 15Kg/m of the first solution3Stirring at 5Hz and 80rmp/min during cooling crystallization, sequentially standing at 60 deg.C for 2 hr, and regulating rotation speed of centrifugeAnd (3) performing centrifugal separation at a dynamic frequency of 40-50 Hz and a rotating speed of 1380rmp/mi, and finally drying at 61 ℃ to obtain nickel sulfate crystals.
Compared with the prior art, the nickel sulfate crystal obtained by adopting the synthesis process has the average grain diameter of 2-3 mm.
Example 7
Embodiment 7 of the present invention provides a method for preparing large-particle nickel sulfate crystals, which is implemented by the following steps:
step 1, adding a nickel sulfate solution into a concentration kettle, wherein the nickel content in the nickel sulfate solution is not lower than 80g/L, then heating and concentrating at a heating rate of 1.8 ℃/min, and continuously stirring at a stirring frequency of 5Hz in the heating and concentrating process until the concentration of the nickel sulfate solution reaches 65 Baume degrees, so as to obtain a first solution;
Step 2, transferring the first solution obtained in the step 1 into a crystallization kettle for cooling crystallization, cooling at a cooling rate of 20 ℃/h until the cooling temperature is reduced to 60 ℃, treating nickel sulfate seed crystals by adopting a 50-mesh screen, adding the treated nickel sulfate seed crystals into the first solution, wherein the nickel sulfate seed crystals are added in a proportion of 15Kg/m of the first solution3Stirring at a stirring frequency of 5Hz and a rotating speed of 72rmp/min in the cooling crystallization process, then sequentially stirring at 50 ℃ for 3h, then adjusting the rotating frequency of a centrifugal machine to be 40-50 Hz and the rotating speed of 1200rmp/mi for centrifugal separation, and finally drying at 55 ℃ to obtain nickel sulfate crystals.
Compared with the prior art, the nickel sulfate crystal obtained by adopting the synthesis process has the average grain diameter of 2-3 mm.
Example 8
Embodiment 8 of the present invention provides a method for preparing large-particle nickel sulfate crystals, which is implemented by the following steps:
step 1, adding a nickel sulfate solution into a concentration kettle, wherein the nickel content in the nickel sulfate solution is not lower than 80g/L, then heating and concentrating at a heating rate of 1.8 ℃/min, and continuously stirring at a stirring frequency of 5Hz in the heating and concentrating process until the concentration of the nickel sulfate solution reaches 65 Baume degrees, so as to obtain a first solution;
Step 2, transferring the first solution obtained in the step 1 into a crystallization kettle for cooling crystallization, cooling at a cooling rate of 20 ℃/h until the cooling temperature is reduced to 60 ℃, treating nickel sulfate seed crystals by adopting a 50-mesh screen, adding the treated nickel sulfate seed crystals into the first solution, wherein the nickel sulfate seed crystals are added in a proportion of 15Kg/m of the first solution3Stirring at a stirring frequency of 5Hz and a rotating speed of 72rmp/min in the cooling crystallization process, then sequentially stirring at 60 ℃ for 2h, then adjusting the rotating frequency of a centrifugal machine to be 40-50 Hz and the rotating speed of 1280rmp/mi for centrifugal separation, and finally drying at 60 ℃ to obtain the nickel sulfate crystal.
Compared with the prior art, the nickel sulfate crystal obtained by adopting the synthesis process has the average grain diameter of 2-3 mm.
Example 9
Embodiment 9 of the present invention provides a method for preparing large-particle nickel sulfate crystals, which is implemented by the following steps:
step 1, adding a nickel sulfate solution into a concentration kettle, wherein the nickel content in the nickel sulfate solution is not lower than 80g/L, then heating and concentrating at a heating rate of 1.8 ℃/min, and continuously stirring at a stirring frequency of 5Hz in the heating and concentrating process until the concentration of the nickel sulfate solution reaches 65 Baume degrees, so as to obtain a first solution;
Step 2, transferring the first solution obtained in the step 1 into a crystallization kettle for cooling crystallization, cooling at a cooling rate of 20 ℃/h until the cooling temperature is reduced to 60 ℃, treating nickel sulfate seed crystals by adopting a 50-mesh screen, adding the treated nickel sulfate seed crystals into the first solution, wherein the nickel sulfate seed crystals are added in a proportion of 15Kg/m of the first solution3Stirring at a stirring frequency of 5Hz and a rotating speed of 72rmp/min in the cooling crystallization process, then sequentially stirring at 70 ℃ for 1h, then adjusting the rotating frequency of a centrifugal machine to be 40-50 Hz and the rotating speed to be 1500rmp/mi for centrifugal separation, and finally drying at 65 ℃ to obtain nickel sulfate crystals.
Compared with the prior art, the nickel sulfate crystal obtained by adopting the synthesis process has the average grain diameter of 2-3 mm.
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 (8)
1. A preparation method of large-particle nickel sulfate crystals is characterized by comprising the following steps:
step 1, adding a nickel sulfate solution into a concentration kettle, and heating and concentrating at a heating rate of 0.5-2 ℃/min until the concentration of the nickel sulfate solution reaches 55-65 Baume degrees to obtain a first solution;
Step 2, transferring the first solution obtained in the step 1 into a crystallization kettle for cooling crystallization, controlling the cooling rate to be 15-25 ℃/h until the cooling temperature is reduced to 60 +/-2 ℃, and controlling the ratio of nickel sulfate seed crystals to the first solution to be 10-15 Kg/m3Adding nickel sulfate crystal seeds into the first solution, and then sequentially performing aging crystallization, centrifugal separation and drying to obtain nickel sulfate crystals.
2. The method for preparing large-particle nickel sulfate crystals as claimed in claim 1, wherein the nickel content in the nickel sulfate solution in step 1 is not less than 80 g/L.
3. The method for preparing large-particle nickel sulfate crystals according to claim 2, wherein the stirring is performed at a stirring frequency of 5Hz during the heating concentration in the step 1.
4. The method for preparing large-particle nickel sulfate crystals according to any one of claims 1 to 3, wherein the nickel sulfate seed crystals in the step 2 are undersize products obtained by screening through a 50-mesh screen.
5. The method for preparing large-particle nickel sulfate crystals as claimed in claim 4, wherein the stirring is performed at a stirring frequency of 5Hz and a rotation speed of 60-80 rmp/min during the cooling crystallization in the step 2.
6. The method for preparing large-particle nickel sulfate crystals according to claim 5, wherein the temperature for aging and crystallizing in the step 2 is 50-70 ℃ for 1-3 hours.
7. The method for preparing large-particle nickel sulfate crystals according to claim 6, wherein the rotation frequency of the centrifuge in the step 2 is 40 to 50Hz, and the rotation speed is 1200 to 1500 rmp/min.
8. The method for preparing large-particle nickel sulfate crystals according to claim 7, wherein the drying temperature in the step 2 is 55-65 ℃.
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Citations (3)
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CN101062793A (en) * | 2007-05-08 | 2007-10-31 | 广东光华化学厂有限公司 | Crystal growth method during alpha-type six hydration nickel sulfate interval crystallization process |
CN102040252A (en) * | 2009-10-16 | 2011-05-04 | 中科铜都粉体新材料股份有限公司 | Method for producing battery-level refined nickel sulfate with electrolyte |
CN104229906A (en) * | 2014-09-28 | 2014-12-24 | 梅州环保设备有限公司 | Method and equipment for preparing electroplating-grade nickel sulfate from nickel-containing wastewater produced in surface treatment process |
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Publication number | Priority date | Publication date | Assignee | Title |
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CN101062793A (en) * | 2007-05-08 | 2007-10-31 | 广东光华化学厂有限公司 | Crystal growth method during alpha-type six hydration nickel sulfate interval crystallization process |
CN102040252A (en) * | 2009-10-16 | 2011-05-04 | 中科铜都粉体新材料股份有限公司 | Method for producing battery-level refined nickel sulfate with electrolyte |
CN104229906A (en) * | 2014-09-28 | 2014-12-24 | 梅州环保设备有限公司 | Method and equipment for preparing electroplating-grade nickel sulfate from nickel-containing wastewater produced in surface treatment process |
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