CN216023264U - Nickel sulfate freezing crystallization device - Google Patents

Nickel sulfate freezing crystallization device Download PDF

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Publication number
CN216023264U
CN216023264U CN202122543545.5U CN202122543545U CN216023264U CN 216023264 U CN216023264 U CN 216023264U CN 202122543545 U CN202122543545 U CN 202122543545U CN 216023264 U CN216023264 U CN 216023264U
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outlet
pipe
inlet
pump
nickel sulfate
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尹璐
刘小凯
孙俊
王玉立
吴汉声
孙孝天
张�林
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Jiangsu Maiande Energy Saving Evaporation Equipment Co ltd
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Jiangsu Maiande Energy Saving Evaporation Equipment Co ltd
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Abstract

The utility model relates to a nickel sulfate freezing crystallization device.A feed pump outlet is connected with a hot side inlet of a precooler, a hot side outlet of the precooler is connected with a feed liquid circulating pipe, the feed liquid circulating pipe is connected with a pipe pass inlet of the freezer through a forced circulating pump, a pipe pass outlet of the freezer is connected with a freezing crystallizer, and a circulating liquid outlet on the upper side wall of the freezing crystallizer is connected with an inlet of the feed liquid circulating pipe; the discharge port of the crystallizer at the lower part of the freezing crystallizer is connected with the inlet of a discharge pump, the outlet of the discharge pump is connected with the feed inlet of a cyclone through a discharge pipe, the underflow outlet of the cyclone is connected with the inlet of a centrifuge, the separated mother liquor outlet of the centrifuge and the overflow outlet of the cyclone are both connected with the inlet of a centrifugal mother liquor tank, the outlet of the centrifugal mother liquor tank is connected with a feed liquor circulating pipe and the cold side inlet of a pre-cooler through a mother liquor pump, and the cold side outlet of the pre-cooler is connected with a centrifugal mother liquor output pipe. The device can not cause material liquid caking and dry wall, can continuously produce, and has low energy consumption and high product stability.

Description

Nickel sulfate freezing crystallization device
Technical Field
The utility model relates to an industrial continuous freezing and crystallizing device, in particular to a nickel sulfate freezing and crystallizing device, and belongs to the technical field of resource recycling.
Background
The nickel sulfate and the anhydrous salt are yellow powder or lemon yellow crystals, the hydrated nickel sulfate mainly comprises 7 hydrated nickel sulfate and 6 hydrated nickel sulfate, and the 6 hydrated nickel sulfate is mainly used in industrial production. The nickel sulfate is used as a chemical raw material and is mainly used in the battery and electroplating industries in industry.
The main sources of the raw materials for the current domestic industrial production of nickel sulfate are as follows: leaching waste materials containing nickel, and removing impurities to produce a nickel sulfate solution; electrolyzing nickel, and leaching to produce a nickel sulfate solution; the nickel sulfide ore is subjected to pyrometallurgy and normal-pressure acid leaching to produce high nickel matte, so that nickel sulfate is prepared. Generally, the nickel sulfate solution is subjected to the procedures of acid adjustment, evaporation, crystallization, centrifugation and the like, and then a qualified nickel sulfate product is produced. In the whole production process, the crystallization process of the nickel sulfate is very critical, and the quality of the nickel sulfate product is directly influenced.
The traditional nickel sulfate preparation method comprises direct fire concentration, electric heating evaporation concentration and steam heating concentration. The direct fire concentration method has the disadvantages of high combustion energy consumption, poor equipment sealing performance, serious environmental pollution and low automation degree, and few factories use the process at present. The electric heating evaporation concentration method uses electric heating to meet the requirement of environmental protection, has high automation degree, but has large investment cost and high production cost, and domestic existing enterprises stop using the process due to high cost. The steam heating concentration method has simple equipment and less investment and is widely adopted, but some problems of porcelain explosion and the like exist in the production.
Some enterprises have started to gradually introduce a process for producing nickel sulfate by freezing crystallization, most of the conventional devices for producing nickel sulfate by freezing crystallization use a cooling tank or a crystallization kettle, a shell is jacketed, heat exchange is carried out through the wall of the tank, the phenomenon of incomplete and uneven cooling and easy occurrence of dry wall agglomeration is caused, single kettle operation is carried out under the condition of needing to adjust the process parameters such as the cooling rate, the stirring frequency, the crystallization time and the like of the crystallization kettle, the control process parameters are more, the product batch is low, the production efficiency is low, the occupied area is large, and continuous operation cannot be carried out.
SUMMERY OF THE UTILITY MODEL
The utility model aims to overcome the problems in the prior art and provide a nickel sulfate freezing and crystallizing device, which can avoid acid mist generated in the nickel sulfate evaporation and crystallization process, avoid material liquid agglomeration and dry wall, has low energy consumption, can realize continuous production, and has stable and smooth discharging and high product stability.
In order to solve the technical problems, the nickel sulfate freezing and crystallizing device comprises a material feeding pump connected with a nickel sulfate stock solution pipe, wherein the outlet of the material feeding pump is connected with the hot side inlet of a precooler, the hot side outlet of the precooler is connected with a material liquid circulating pipe, the outlet of the material liquid circulating pipe is connected with the inlet of a forced circulating pump, the outlet of the forced circulating pump is connected with the bottom pipe pass inlet of the freezer, the top pipe pass outlet of the freezer is connected with the feed inlet of a freezing crystallizer through a freezer outlet pipe, and the circulating liquid outlet of the upper side wall of the freezing crystallizer is connected with the inlet of the material liquid circulating pipe; the bottom and the lower side wall of the freezing crystallizer are provided with crystallizer discharge ports, the crystallizer discharge ports are connected with an inlet of a discharge pump, an outlet of the discharge pump is connected with a feed inlet of a cyclone through a discharge pipe, an underflow outlet of the cyclone is connected with an inlet of a centrifuge, a solid phase of the centrifuge outputs a nickel sulfate product, a separated mother liquor outlet of the centrifuge and an overflow outlet of the cyclone are both connected with an inlet of a centrifugal mother liquor tank, an outlet of the centrifugal mother liquor tank is connected with an inlet of the mother liquor pump, an outlet of the mother liquor pump is connected with a feed liquid circulating pipe and a cold side inlet of the precooler, and a cold side outlet of the precooler is connected with a centrifugal mother liquor output pipe.
As an improvement of the utility model, the feed inlet of the freezing crystallizer is connected with a guide pipe, and the guide pipe extends to the lower part of the freezing crystallizer along the axis.
As a further improvement of the utility model, the outlet at the lower part of the shell side of the freezer is connected with the inlet at the upper part of the shell side of the freezer through a refrigerant circulating pipe and a refrigerant circulating pump, the outlet of a refrigerant supplementing pipe is connected with the refrigerant circulating pipe, and the outlet of the refrigerant circulating pump is connected with a refrigerant discharging pipe.
As a further development of the utility model, the cold medium feed line is connected upstream of the inlet in the upper part of the freezer housing.
As a further improvement of the utility model, the freezing crystallizer is provided with a conical lower part and a circular arc bottom part with a convex middle part, the lowest point of the circular arc bottom part is provided with the crystallizer discharge hole, and the side wall of the conical lower part is provided with a plurality of crystallizer discharge holes along the height direction.
As a further improvement of the utility model, the lower side wall of the outlet pipe of the freezer is provided with a fused salt nozzle.
Compared with the prior art, the utility model has the following beneficial effects: 1. before entering the freezer, the nickel sulfate feed liquid enters the precooler to exchange heat with the centrifugal mother liquid to precool, so that the energy consumption of a refrigerant medium is reduced, and the cold energy of the centrifugal mother liquid is recovered. 2. The external freezer reduces short-circuit temperature difference loss, and the cooling is more uniform and energy-saving. 3. The retention time of the feed liquid is long, the grain size of the discharged nickel sulfate is large, and the product quality is high. 4. Can prevent the discharge blockage and avoid influencing the continuity of production.
Drawings
The utility model will be described in further detail with reference to the following drawings and detailed description, which are provided for reference and illustration purposes only and are not intended to limit the utility model.
FIG. 1 is a flow chart of a nickel sulfate freezing and crystallizing device of the present invention.
In the figure: 1. a pre-cooler; 2. a freezing crystallizer; a flow guide pipe; 2b, a circulating liquid outlet; 2c, discharging a crystallizer; 3. a freezer; 3a. fused salt pipe orifice; 4. a swirler; 5. a centrifuge; 6. centrifuging the mother liquor tank; G1. a nickel sulfate stock solution pipe; G2. a feed liquid circulating pipe; G3. a freezer outlet pipe; G4. a cold medium circulation pipe; G5. a cold medium fluid supplementing pipe; G6. a refrigerant medium discharge pipe; G7. a discharge pipe; G8. centrifuging a mother liquor output pipe; B1. a feeding pump; B2. a forced circulation pump; B3. a discharge pump; B4. a mother liquor pump; B5. cold medium circulating pump.
Detailed Description
As shown in figure 1, the nickel sulfate freezing and crystallizing device comprises a feed pump B1 connected with a nickel sulfate raw liquid pipe G1, wherein the outlet of the feed pump B1 is connected with the hot side inlet of a precooler 1, the hot side outlet of the precooler 1 is connected with a feed liquid circulating pipe G2, the outlet of the feed liquid circulating pipe G2 is connected with the inlet of a forced circulating pump B2, the outlet of the forced circulating pump B2 is connected with the bottom pipe side inlet of a freezer 3, and the top pipe side outlet of the freezer 3 is connected with the feed inlet of a freezing crystallizer 2 through a freezer outlet pipe G3.
The forced circulation pump B2 pushes the feed liquid in the freezing crystallizer 2 to return to the freezing crystallizer 2 from the feed liquid circulation pipe G2 to the freezer 3 to form a feed liquid forced circulation process, thereby reducing the feed liquid agglomeration and blockage phenomenon, achieving continuous operation, simultaneously prolonging the retention time of the feed liquid and providing a powerful condition for the growth of crystals.
External freezer 3, the feed liquid is followed the feeding of freezer 3 lower part, and the upper portion ejection of compact has reduced the short circuit temperature difference loss, and freezing crystallizer 2 and cooler all can adopt the 316L material, and is high than traditional enamel still heat transfer efficiency, and heat transfer coefficient is big, has solved the incomplete inhomogeneous problem of cooling, has practiced thrift the cold volume consumption of refrigerant medium high-efficiently.
The feed inlet of the freezing crystallizer 2 is connected with a flow guide pipe 2a, and the flow guide pipe 2a extends to the lower part of the freezing crystallizer 2 along the axis. A circulating liquid outlet 2b on the upper side wall of the freezing crystallizer 2 is connected with an inlet of a feed liquid circulating pipe G2; the bottom and the lower side wall of the freezing crystallizer 2 are provided with crystallizer discharge ports 2c, and the crystallizer discharge ports 2c are connected with the inlet of a discharge pump B3. The freezing crystallizer 2 is internally provided with a flow guide pipe 2a, nickel sulfate feed liquid cooled by a freezer 3 enters the freezing crystallizer 2 and then is guided by the flow guide pipe 2a at the upper part to enter the lower part of the freezing crystallizer 2, then the nickel sulfate feed liquid rises to a circulating liquid outlet 2b to be discharged, nickel sulfate crystals with large particle sizes sink under the action of gravity in the whole process, the nickel sulfate crystals with small particle sizes float to the circulating liquid outlet 2b through a discharge port 2c of the crystallizer, and continuously participate in circulation to prolong the retention time, so that crystal grains grow up, and the product quality is improved.
The lower outlet of the shell side of the freezer 3 is connected with the upper inlet of the shell side of the freezer 3 through a refrigerant medium circulating pipe G4 and a refrigerant medium circulating pump B5. The refrigerant medium circulating pump B5 forces the refrigerant medium in the shell pass of the freezer to circulate, and the refrigerant medium and the nickel sulfate liquid can fully exchange heat, thereby reducing the energy consumption of the refrigerant medium.
The outlet of the cold medium liquid supplementing pipe G5 is connected with a cold medium circulating pipe G4, and the outlet of the cold medium circulating pump B5 is connected with a cold medium discharging pipe G6; the refrigerant medium liquid supplementing pipe G5 is connected to the upper part of the inlet on the upper part of the shell of the refrigerator, and can supplement the low-temperature refrigerant medium and discharge the refrigerant medium after heat exchange in time.
The freezing crystallizer 2 is provided with a conical lower part and a circular arc-shaped bottom part with a convex middle part, so that a dead zone is not easily formed; the lowest point of the arc-shaped bottom is provided with a crystallizer discharge port 2c, and the side wall of the conical lower part is provided with a plurality of crystallizer discharge ports 2c along the height direction, so that discharge blockage can be prevented, and the production continuity is prevented from being influenced.
The outlet of the discharging pump B3 is connected with the feed inlet of the cyclone 4 through the discharging pipe G7, the underflow outlet of the cyclone 4 is connected with the inlet of the centrifuge 5, the solid phase of the centrifuge 5 outputs nickel sulfate products, the separated mother liquor outlet of the centrifuge 5 and the overflow outlet of the cyclone 4 are both connected with the inlet of the centrifugal mother liquor tank 6, the outlet of the centrifugal mother liquor tank 6 is connected with the inlet of the mother liquor pump B4, the outlet of the mother liquor pump B4 is connected with the feed liquor circulating pipe G2 and the cold side inlet of the precooler 1, and the cold side outlet of the precooler 1 is connected with the centrifugal mother liquor output pipe G8.
In the work, incoming materials from a nickel sulfate raw liquid pipe G1 are pumped by a feed pump B1, enter the hot side of a precooler 1, and enter a feed liquid circulating pipe G2 after being subjected to heat exchange and temperature reduction with low-temperature mother liquid, a freezing crystallizer 2, a freezer 3 and a forced circulation pump B2 are connected by a feed liquid circulating pipe G2, when the liquid level in the freezing crystallizer 2 reaches a certain height, the forced circulation pump B2 is started, the forced circulation pump B2 sends the circulating feed liquid into the tube side of the freezer 3, and the circulating feed liquid is subjected to heat exchange and temperature reduction with a cold medium on the shell side to be below 0 ℃. The industrial electrolyte nickel sulfate solution is generally under the high-acid condition, the solution of the device is lower than 0 ℃, the nickel sulfate solubility is very low under the high-acid condition, nickel sulfate crystals are easy to separate out and crystallize at low temperature, and the problem of acid mist leakage caused by heating is further avoided.
The nickel sulfate feed liquid enters the freezing crystallizer 2 from an outlet pipe G3 of the freezer, nickel sulfate crystals are separated out along with the reduction of the temperature of the nickel sulfate feed liquid, the nickel sulfate crystals descend to the lower part of the freezing crystallizer 2 along a guide pipe 2a, then nickel sulfate crystal slurry rises to a circulating liquid outlet 2B, and after flowing out from a feed liquid circulating pipe G2, the nickel sulfate crystal slurry is conveyed to the freezer again by a forced circulating pump B2, and in the whole process, the nickel sulfate crystal slurry sinks under the action of gravity, the nickel sulfate crystals with large particle size float to the circulating liquid outlet 2B, and participate in circulation with precooled incoming materials. The forced circulation of the feed liquid reduces the blocking phenomenon of feed liquid agglomeration, prolongs the retention time, enables crystal grains to grow up and improves the product quality.
After being discharged from a discharge port 2c of the crystallizer, crystal slurry of nickel sulfate crystals with larger particle size is sent into a cyclone 4 by a discharge pump B3 for concentration and thickening, the concentrated nickel sulfate crystal slurry enters a centrifuge 5 for solid-liquid separation to obtain a nickel sulfate product, the separated mother liquor flows into a centrifugal mother liquor tank 6 through a pipeline, the low-temperature nickel sulfate mother liquor is sent out by a mother liquor pump B4, one part of the low-temperature nickel sulfate mother liquor enters a cold side of a precooler 1 to exchange heat with nickel sulfate incoming materials, and the other part of the low-temperature nickel sulfate mother liquor flows back to a feed liquor circulating pipe G2 to enter circulation again.
The refrigerant medium of the shell layer of the refrigerator realizes forced circulation operation through a refrigerant medium circulating pipe G4 and a refrigerant medium circulating pump B5, so that heat can be fully exchanged with the nickel sulfate liquid, and the energy of the refrigerant medium is saved.
The side wall of the lower part of the outlet pipe G3 of the freezer is provided with a fused salt pipe orifice 3a, if feed liquid is caked or the wall is dry in the crystallization process, the fused salt pipe orifice 3a can be opened in time to introduce heat medium, so that the problem can be solved immediately, and continuous production is ensured.
The above description is only a preferred embodiment of the present invention, and not intended to limit the scope of the present invention. In addition to the above embodiments, the present invention may have other embodiments. All technical solutions formed by adopting equivalent substitutions or equivalent transformations fall within the protection scope of the claims of the present invention.

Claims (6)

1. The utility model provides a nickel sulfate freeze crystallization device, includes the incoming material pump that links to each other with nickel sulfate stoste pipe, its characterized in that: the outlet of the incoming material pump is connected with the hot side inlet of the precooler, the hot side outlet of the precooler is connected with the material liquid circulating pipe, the outlet of the material liquid circulating pipe is connected with the inlet of the forced circulation pump, the outlet of the forced circulation pump is connected with the bottom pipe pass inlet of the freezer, the top pipe pass outlet of the freezer is connected with the feed inlet of the freezing crystallizer through the freezer outlet pipe, and the circulating liquid outlet of the upper side wall of the freezing crystallizer is connected with the inlet of the material liquid circulating pipe; the bottom and the lower side wall of the freezing crystallizer are provided with crystallizer discharge ports, the crystallizer discharge ports are connected with an inlet of a discharge pump, an outlet of the discharge pump is connected with a feed inlet of a cyclone through a discharge pipe, an underflow outlet of the cyclone is connected with an inlet of a centrifuge, a solid phase of the centrifuge outputs a nickel sulfate product, a separated mother liquor outlet of the centrifuge and an overflow outlet of the cyclone are both connected with an inlet of a centrifugal mother liquor tank, an outlet of the centrifugal mother liquor tank is connected with an inlet of the mother liquor pump, an outlet of the mother liquor pump is connected with a feed liquid circulating pipe and a cold side inlet of the precooler, and a cold side outlet of the precooler is connected with a centrifugal mother liquor output pipe.
2. The nickel sulfate freezing and crystallizing device of claim 1, wherein: the feed inlet of the freezing crystallizer is connected with a guide pipe, and the guide pipe extends to the lower part of the freezing crystallizer along the axis.
3. The nickel sulfate freezing and crystallizing device of claim 1, wherein: the outlet of the lower part of the shell pass of the freezer is connected with the inlet of the upper part of the shell pass of the freezer through a cold medium circulating pipe and a cold medium circulating pump, the outlet of the cold medium liquid supplementing pipe is connected with the cold medium circulating pipe, and the outlet of the cold medium circulating pump is connected with a cold medium discharging pipe.
4. The nickel sulfate freezing and crystallizing device of claim 3, wherein: the cold medium liquid replenishing pipe is connected to the upper part of the inlet of the shell side of the freezer.
5. The nickel sulfate freezing and crystallizing device of claim 1, wherein: the freezing crystallizer is provided with a conical lower part and a circular arc-shaped bottom part with a convex middle part, the lowest point of the circular arc-shaped bottom part is provided with the crystallizer discharge port, and the side wall of the conical lower part is provided with a plurality of crystallizer discharge ports along the height direction.
6. The nickel sulfate freeze crystallization apparatus according to any one of claims 1 to 5, wherein: and the side wall of the lower part of the outlet pipe of the freezer is provided with a fused salt pipe orifice.
CN202122543545.5U 2021-10-21 2021-10-21 Nickel sulfate freezing crystallization device Active CN216023264U (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202122543545.5U CN216023264U (en) 2021-10-21 2021-10-21 Nickel sulfate freezing crystallization device

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202122543545.5U CN216023264U (en) 2021-10-21 2021-10-21 Nickel sulfate freezing crystallization device

Publications (1)

Publication Number Publication Date
CN216023264U true CN216023264U (en) 2022-03-15

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Application Number Title Priority Date Filing Date
CN202122543545.5U Active CN216023264U (en) 2021-10-21 2021-10-21 Nickel sulfate freezing crystallization device

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CN (1) CN216023264U (en)

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