CN110194491A - A kind of preparation method and preparation facilities of basic nickel carbonate - Google Patents
A kind of preparation method and preparation facilities of basic nickel carbonate Download PDFInfo
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- CN110194491A CN110194491A CN201810157298.5A CN201810157298A CN110194491A CN 110194491 A CN110194491 A CN 110194491A CN 201810157298 A CN201810157298 A CN 201810157298A CN 110194491 A CN110194491 A CN 110194491A
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- C01G53/00—Compounds of nickel
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Abstract
The invention discloses a kind of preparation method of basic nickel carbonate, this method is achieved by the steps of: 1) preparing carbonate solution and nickel salt solution respectively；2) carbonate solution and nickel salt solution are added in reactor simultaneously, keep the flow of nickel salt solution constant in fill process, it is reacted by the pH value and carbon dioxide release concentration that adjust the flow control system of carbonate solution, obtains nickel carbonate mixture solution；3) said mixture solution is separated, obtains basic nickel carbonate crude product；4) the above-mentioned nickelous carbonate crude product of pure water is used, re-dry obtains basic nickel carbonate；The present invention is keeping the flow of nickel salt solution constant, pH value is controlled by adjusting the flow of carbonate solution and controls the dual monitoring method of the ratio of nickel salt and carbonate by the release concentration of detection dioxy flower carbon to prepare basic nickel carbonate, so that carbanion resolution ratio is low in reaction process, so that the content of nickel is high in basic nickel carbonate obtained, performance is good.
Description
Technical field
The invention belongs to the preparation technical fields of basic nickel carbonate, and in particular to a kind of preparation method of basic nickel carbonate and
Preparation facilities.
Background technique
Basic nickel carbonate is a kind of important inorganic fine chemicals, mainly for the preparation of various nickel salts, high-quality alkali formula
Nickelous carbonate can be applied to electrical type industry, catalyst industry；In addition, basic nickel carbonate is also widely used in plating, electroforming, enamel
Pigment etc..
Basic nickel carbonate precipitating reagent is usually sodium carbonate, ammonium carbonate, ammonium hydrogencarbonate；Subcarbonate synthesis passes through carbonate
It decomposes and generates hydroxyl with hydrolysis to realize the synthesis of basic nickel carbonate, therefore carbonate resolves into ratio hydroxy and determines alkali
The ratio of nickel hydroxide in formula nickelous carbonate controls the nickel content of basic nickel carbonate, different application field is to basic nickel carbonate
Nickel content requirement is different, such as hydrodesulfurization catalytic industry basic nickel carbonate nickel content 46% or so；And basic carbonate
Nickel synthesis generallys use reaction process pH value to control reaction growth and nickel content, but sodium carbonate, ammonium carbonate, ammonium hydrogencarbonate can divide
Solution, insensitive to pH value variation, pH variation has one to delay process, cannot reflect carbonate and hydroxide in reaction system in time
Root variation.
Summary of the invention
In view of this, being solved existing the main purpose of the present invention is to provide a kind of preparation method of basic nickel carbonate
The release concentration that basic nickel carbonate carbon dioxide in process is released cannot be prepared by detection in technology to control nickel salt and carbonate
Ratio, the problem of leading to finally to be made low nickel content in basic nickel carbonate, poor performance；The invention also discloses a kind of alkali formulas
The preparation facilities of nickelous carbonate.
In order to achieve the above objectives, the technical scheme of the present invention is realized as follows: a kind of preparation method of basic nickel carbonate,
This method is achieved by the steps of:
Step 1, the carbonate solution and nickel ion that carbonate ions concentration is 100~160g/L are prepared respectively in NaOH solution tank NaOH
Concentration is the nickel salt solution of 0.5~2moL/L；
Step 2, it is fed using peristaltic pump, carbonate solution and nickel salt solution is added in special reactor simultaneously, into
Material during keep nickel salt solution flow it is constant, by adjust carbonate solution flow control system pH value be 8.0~
8.3 and carbon dioxide release concentration be 8000~8100ppm, and react 5~10h, obtain nickel carbonate mixture solution；
Step 3, the nickel carbonate mixture solution that step 2 obtains is squeezed into centrifuge to be centrifuged, obtains alkali formula carbon
Sour nickel crude product；
Step 4, using the nickelous carbonate crude product of the acquisition of step 3 described in pure water to wash water conductivity≤100 μ s/m, then
Dry 2~3h, obtains basic nickel carbonate at 65~95 DEG C.
Preferably, in the step 1, the carbonate is at least one of sodium carbonate, ammonium carbonate, ammonium hydrogen carbonate；Institute
Stating nickel salt is at least one of nickel sulfate, nickel nitrate.
Preferably, in the step 2, the flow of the sodium carbonate liquor is 5~500L/h；The flow of the nickel salt solution
For 50~500L/h；The reaction temperature is 50~90 DEG C.
Another technical solution of the invention is achieved in that a kind of preparation facilities of basic nickel carbonate, and feature exists
In comprising reacting body, the carbonate feed pipe being arranged in reacting body, nickel salt expects pipe, mixing component and titanium dioxide
Carbon detection components, pH measure component, and the mixing component is located at the central location in reacting body, the carbonate feed pipe with
The two sides in reacting body are symmetrically arranged in nickel salt expects pipe；The upper end of reacting body is arranged in the carbon dioxide detection components
The lower end of reacting body is arranged in top, the pH measurement component.
Preferably, the carbon dioxide detection components include carbon dioxide exhaust line road, carbon dioxide detector, and described two
Carbonmonoxide detector is connected by carbon dioxide exhaust line road with reacting body.
Preferably, the pH measurement component includes pH measurement pipeline, pH analyzer, and the pH analyzer is measured by pH and managed
Road is connected with reacting body.
Preferably, the mixing component includes stirring motor, agitating shaft, stirring blade, and the stirring blade is affixed
In the lower end of agitating shaft, the upper end of agitating shaft is arranged in the stirring motor and driving agitating shaft and stirring blade turn around axis
It is dynamic.
Preferably, the outer layer of the reacting body is provided with vacuum heat-preserving collet, is provided in the vacuum heat-preserving collet
Heating coil.
Preferably, the lower end outer layer of the ontology has collet for heating.
Preferably, the bottom that the vacuum heat-preserving collet on the outside of the reacting body is arranged in is provided with condensation water inlet, if
The side for setting the vacuum heat-preserving collet on the outside of the reacting body is provided with steam (vapor) outlet.
Preferably, the bottom of the reacting body is provided with discharge port, sewage draining exit.
Preferably, at least side is provided with deflector inside the reacting body.
Preferably, the lower section of the reacting body is also symmetrical arranged that there are two fixed bracket
Compared with prior art, the present invention is keeping the flow of nickel salt solution constant, by the stream for adjusting carbonate solution
It measures to control pH value and control the dual monitoring of the ratio of nickel salt and carbonate by the release concentration of detection dioxy flower carbon
Method prepares basic nickel carbonate, so that carbanion resolution ratio is low in reaction process, so that basic carbonate obtained
The content of nickel is high in nickel, and performance is good；The method of the present invention is simple and easy, is worth of widely use.
Detailed description of the invention
Fig. 1 is a kind of structural schematic diagram of the preparation facilities of basic nickel carbonate provided in an embodiment of the present invention.
Specific embodiment
In order to make the objectives, technical solutions, and advantages of the present invention clearer, with reference to the accompanying drawings and embodiments, right
The present invention is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, and
It is not used in the restriction present invention.
A kind of preparation method of basic nickel carbonate provided in an embodiment of the present invention, this method are achieved by the steps of:
Step 1, the carbonate solution and nickel ion that carbonate ions concentration is 100~160g/L are prepared respectively in NaOH solution tank NaOH
Concentration is the nickel salt solution of 0.5~2moL/L；Wherein, carbonate is at least one of sodium carbonate, ammonium carbonate, ammonium hydrogen carbonate；
Nickel salt is at least one of nickel sulfate, nickel nitrate；
Step 2, it is fed using peristaltic pump, carbonate solution and nickel salt solution is added in special reactor simultaneously, into
The flow that nickel salt solution is kept during material is that 50~500L/h is constant, by the flow (carbonic acid for adjusting carbonate solution
The range of flow of sodium solution is 5~500L/h；) pH value of control system is 8.0~8.3 and carbon dioxide release concentration is 8000
~8100ppm, and 5~10h is reacted at 50~90 DEG C, obtain nickel carbonate mixture solution；
Step 3, the nickel carbonate mixture solution that step 2 obtains is squeezed into centrifuge and acquisition basic carbonate is centrifuged
Nickel crude product；
Step 4, using the nickelous carbonate crude product of the acquisition of step 3 described in pure water to wash water conductivity≤100 μ s/m, then
Dry 2~3h, obtains basic nickel carbonate at 65~95 DEG C.
The embodiment of the invention also provides a kind of preparation facilities of basic nickel carbonate, as shown in Figure 1 comprising reacting body
1, carbonate feed pipe 2 in reacting body, nickel salt expects pipe 3, mixing component 4 and carbon dioxide detection components 5, pH are set
Component 6 is measured, mixing component 4 is located at the central location in reacting body 1, and carbonate feed pipe 2 and nickel salt expects pipe 3 are symmetrically set
Set the two sides in reacting body 1；Carbon dioxide detection components 5 are arranged at the top of the upper end of reacting body 1, and pH measures component 6
The lower end of reacting body 1 is set.
Further, carbon dioxide detection components 5 include carbon dioxide exhaust line road 51, carbon dioxide detector 52, two
Carbonmonoxide detector 52 is connected by carbon dioxide exhaust line road 51 with reacting body 1.
Further, it includes that pH measures pipeline 61, pH analyzer 62 that pH, which measures component 6, and pH analyzer 62 is measured by pH
Pipeline 61 is connected with reacting body 1.
Further, mixing component 4 includes stirring motor 41, agitating shaft 42, stirring blade 43, and stirring blade 43 is fixed in
The lower end of agitating shaft 42, the stirring motor 41 be arranged in the upper end of agitating shaft 42 and driving agitating shaft 42 and stirring blade 43 around
Axis rotation.
Further, the outer layer of reacting body 1 is provided with vacuum heat-preserving collet 11, is provided with and adds in vacuum heat-preserving collet 11
Hot coil 111.
Further, the lower end outer layer of reacting body 1 has collet 12 for heating.
Further, be arranged in the vacuum heat-preserving collet 11 in 1 outside of the reacting body bottom be provided with condensed water into
Mouth 112, the side that the vacuum heat-preserving collet 11 in 1 outside of reacting body is arranged in are provided with steam (vapor) outlet 113.
Further, the bottom of reacting body 1 is provided with discharge port 12, sewage draining exit 13.
Further, at least side is provided with deflector 14 inside reacting body 1.
Further, the lower section of reacting body 1 is also symmetrical arranged that there are two fixed brackets 7.
The present invention keep nickel salt solution flow it is constant, by adjust carbonate solution flow come control pH value and
The dual monitoring method of the ratio of nickel salt and carbonate is controlled by the release concentration of detection dioxy flower carbon to prepare alkali formula carbon
Sour nickel, so that carbanion resolution ratio is low in reaction process, so that the content of nickel is high in basic nickel carbonate obtained, property
It can be good；The method of the present invention is simple and easy, is worth of widely use.
Embodiment 1
Step 1, the sodium carbonate liquor and nickel ion concentration that carbonate ions concentration is 120g/L are prepared respectively in NaOH solution tank NaOH
For the nickel sulfate solution of 1.5moL/L；
Step 2, it is fed using peristaltic pump, carbonate solution and nickel salt solution is added in special reactor simultaneously, into
The flow that nickel salt solution is kept during material is that 200L/h is constant, the pH value of the flow control system by adjusting carbonate solution
It is 8050ppm for 8.1 and carbon dioxide release concentration, and reacts 8h at 70 DEG C, obtains nickel carbonate mixture solution；
Step 3, the nickel carbonate mixture solution that step 2 obtains is squeezed into centrifuge to be centrifuged, obtains alkali formula carbon
Sour nickel crude product；
Step 4, using the nickelous carbonate crude product of the acquisition of step 3 described in pure water to wash water conductivity≤100 μ s/m, then
Dry 2.5h, obtains basic nickel carbonate at 80 DEG C.
Embodiment 2
Step 1, the sodium carbonate liquor and nickel ion concentration that carbonate ions concentration is 100g/L are prepared respectively in NaOH solution tank NaOH
For the nickel sulfate solution of 0.5moL/L；
Step 2, it is fed using peristaltic pump, carbonate solution and nickel salt solution is added in special reactor simultaneously, into
The flow that nickel salt solution is kept during material is that 50L/h is constant, the pH value of the flow control system by adjusting carbonate solution
It is 8000ppm for 8.0 and carbon dioxide release concentration, and reacts 5h at 50 DEG C, obtains nickel carbonate mixture solution；
Step 3, the nickel carbonate mixture solution that step 2 obtains is squeezed into centrifuge to be centrifuged, obtains alkali formula carbon
Sour nickel crude product；
Step 4, using the nickelous carbonate crude product of the acquisition of step 3 described in pure water to wash water conductivity≤100 μ s/m, then
Dry 2h, obtains basic nickel carbonate at 65 DEG C.
Embodiment 3
Step 1, the sodium carbonate liquor and nickel ion concentration that carbonate ions concentration is 160g/L are prepared respectively in NaOH solution tank NaOH
For the nickel sulfate solution of 2moL/L；
Step 2, it is fed using peristaltic pump, carbonate solution and nickel salt solution is added in special reactor simultaneously, into
The flow that nickel salt solution is kept during material is that 500L/h is constant, the pH value of the flow control system by adjusting carbonate solution
It is 8100ppm for 8.3 and carbon dioxide release concentration, and reacts 10h at 90 DEG C, obtains nickel carbonate mixture solution；
Step 3, the nickel carbonate mixture solution that step 2 obtains is squeezed into centrifuge to be centrifuged, obtains alkali formula carbon
Sour nickel crude product；
Step 4, using the nickelous carbonate crude product of the acquisition of step 3 described in pure water to wash water conductivity≤100 μ s/m, then
Dry 3h, obtains basic nickel carbonate at 95 DEG C.
Embodiment 4
Step 1, the sodium carbonate liquor and nickel ion concentration that carbonate ions concentration is 120g/L are prepared respectively in NaOH solution tank NaOH
For the nickel sulfate solution of 1.5moL/L；
Step 2, it is fed using peristaltic pump, carbonate solution and nickel salt solution is added in special reactor simultaneously, into
The flow that nickel salt solution is kept during material is that 50L/h is constant, the pH value of the flow control system by adjusting carbonate solution
It is 8000ppm for 8.0 and carbon dioxide release concentration, and reacts 5h at 50 DEG C, obtains nickel carbonate mixture solution；
Step 3, the nickel carbonate mixture solution that step 2 obtains is squeezed into centrifuge to be centrifuged, obtains alkali formula carbon
Sour nickel crude product；
Step 4, using the nickelous carbonate crude product of the acquisition of step 3 described in pure water to wash water conductivity≤100 μ s/m, then
Dry 3h, obtains basic nickel carbonate at 95 DEG C.
Embodiment 5
Step 1, the sodium carbonate liquor and nickel ion concentration that carbonate ions concentration is 100g/L are prepared respectively in NaOH solution tank NaOH
For the nickel sulfate solution of 0.5moL/L；
Step 2, it is fed using peristaltic pump, carbonate solution and nickel salt solution is added in special reactor simultaneously, into
The flow that nickel salt solution is kept during material is that 200L/h is constant, the pH value of the flow control system by adjusting carbonate solution
It is 8050ppm for 8.1 and carbon dioxide release concentration, and reacts 8h at 70 DEG C, obtains nickel carbonate mixture solution；
Step 3, the nickel carbonate mixture solution that step 2 obtains is squeezed into centrifuge to be centrifuged, obtains alkali formula carbon
Sour nickel crude product；
Step 4, using the nickelous carbonate crude product of the acquisition of step 3 described in pure water to wash water conductivity≤100 μ s/m, then
Dry 3h, obtains basic nickel carbonate at 95 DEG C.
Embodiment 6
Step 1, the sodium carbonate liquor and nickel ion concentration that carbonate ions concentration is 160g/L are prepared respectively in NaOH solution tank NaOH
For the nickel sulfate solution of 2moL/L；
Step 2, it is fed using peristaltic pump, carbonate solution and nickel salt solution is added in special reactor simultaneously, into
The flow that nickel salt solution is kept during material is that 200L/h is constant, the pH value of the flow control system by adjusting carbonate solution
It is 8050ppm for 8.1 and carbon dioxide release concentration, and reacts 8h at 70 DEG C, obtains nickel carbonate mixture solution；
Step 3, the nickel carbonate mixture solution that step 2 obtains is squeezed into centrifuge to be centrifuged, obtains alkali formula carbon
Sour nickel crude product；
Step 4, using the nickelous carbonate crude product of the acquisition of step 3 described in pure water to wash water conductivity≤100 μ s/m, then
Dry 2h, obtains basic nickel carbonate at 65 DEG C.
Experimental example
The nickel content in basic nickel carbonate obtained to embodiment 1 to embodiment 6 detects, testing result such as following table institute
Show:
Table 1 implements the testing result of the nickel content in the basic nickel carbonate that 1 obtains to embodiment 9
46% left side is respectively positioned on by the content that data in upper table can be seen that nickel in the basic nickel carbonate that the present invention obtains
The performance on the right side, the basic nickel carbonate obtained compared with the prior art, the basic nickel carbonate that the present invention obtains is more excellent, and usage range is more
Extensively.
The foregoing is only a preferred embodiment of the present invention, is not intended to limit the scope of the present invention.
Claims (10)
1. a kind of preparation method of basic nickel carbonate, which is characterized in that this method is achieved by the steps of:
Step 1, the carbonate solution and nickel ion concentration that carbonate ions concentration is 100~160g/L are prepared respectively in NaOH solution tank NaOH
For the nickel salt solution of 0.5~2moL/L；
Step 2, it is fed using peristaltic pump, carbonate solution and nickel salt solution is added in special reactor simultaneously, fed
Keep the flow of nickel salt solution constant in journey, the pH value by the flow control system for adjusting carbonate solution is 8.0~8.3 Hes
Carbon dioxide release concentration is 8000~8100ppm, and reacts 5~10h, obtains nickel carbonate mixture solution；
Step 3, the nickel carbonate mixture solution that step 2 obtains is squeezed into centrifuge to be centrifuged, obtains basic nickel carbonate
Crude product；
Step 4, the nickelous carbonate crude product obtained using step 3 described in pure water to wash water conductivity≤100 μ s/m, then 65~
Dry 2~3h, obtains basic nickel carbonate at 95 DEG C.
2. a kind of preparation method of basic nickel carbonate according to claim 1, which is characterized in that described in the step 1
Carbonate is at least one of sodium carbonate, ammonium carbonate, ammonium hydrogen carbonate；The nickel salt is nickel sulfate, at least one in nickel nitrate
Kind.
3. a kind of preparation method of basic nickel carbonate according to claim 1 or 2, which is characterized in that in the step 2,
The flow of the sodium carbonate liquor is 5~500L/h；The flow of the nickel salt solution is 50~500L/h；The reaction temperature is
50~90 DEG C.
4. a kind of preparation facilities of basic nickel carbonate, which is characterized in that it includes reacting body, the carbon that is arranged in reacting body
Hydrochlorate feed pipe, nickel salt expects pipe, mixing component and carbon dioxide detection components, pH measure component, and the mixing component is located at
The two sides in reacting body are symmetrically arranged in central location in reacting body, the carbonate feed pipe and nickel salt expects pipe；
The carbon dioxide detection components are arranged at the top of the upper end of reacting body, and the pH measurement component is arranged under reacting body
End.
5. a kind of preparation facilities of basic nickel carbonate according to claim 4, which is characterized in that the carbon dioxide detection
Component includes carbon dioxide exhaust line road, carbon dioxide detector, and the carbon dioxide detector passes through carbon dioxide exhaust line
Road is connected with reacting body.
6. a kind of preparation facilities of basic nickel carbonate according to claim 5, which is characterized in that the pH measures component packet
PH measurement pipeline, pH analyzer are included, the pH analyzer measures pipeline by pH and is connected with reacting body.
7. a kind of preparation facilities of basic nickel carbonate according to claim 6, which is characterized in that the mixing component
Including stirring motor, agitating shaft, stirring blade, the stirring blade is fixed in the lower end of agitating shaft, the stirring motor setting
Agitating shaft upper end and driving agitating shaft and stirring blade be rotated about axis.
8. a kind of preparation facilities of basic nickel carbonate according to claim 7, which is characterized in that outside the reacting body
Layer is provided with vacuum heat-preserving collet, is provided with heating coil in the vacuum heat-preserving collet.
9. a kind of preparation facilities of basic nickel carbonate according to claim 8, which is characterized in that setting is in the reaction sheet
The bottom of the vacuum heat-preserving collet of external side is provided with condensation water inlet, and the vacuum heat-preserving folder on the outside of the reacting body is arranged in
The side of set is provided with steam (vapor) outlet.
10. a kind of preparation facilities of basic nickel carbonate according to claim 4-9 any one, which is characterized in that described
The bottom of reacting body is provided with discharge port, sewage draining exit.
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| CN201810157298.5A CN110194491A (en) | 2018-02-24 | 2018-02-24 | A kind of preparation method and preparation facilities of basic nickel carbonate |
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Cited By (1)
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| CN115520916A (en) * | 2022-10-17 | 2022-12-27 | 怀化恒安石化有限公司 | PH value adjustment mechanism and basic nickel carbonate preparation facilities thereof |
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