CN110092422A - A kind of minimizing technology for sulfate radical foreign matter in nickelous carbonate - Google Patents
A kind of minimizing technology for sulfate radical foreign matter in nickelous carbonate Download PDFInfo
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- CN110092422A CN110092422A CN201810091844.XA CN201810091844A CN110092422A CN 110092422 A CN110092422 A CN 110092422A CN 201810091844 A CN201810091844 A CN 201810091844A CN 110092422 A CN110092422 A CN 110092422A
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- nickelous carbonate
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G53/00—Compounds of nickel
- C01G53/06—Carbonates
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
Abstract
The invention discloses a kind of minimizing technology for sulfate radical foreign matter in nickelous carbonate, this method is achieved by the steps of: step 1, the nickelous carbonate slurry that liquid alkaline is added in the nickelous carbonate containing sulfate ion and adjusts pH value to 8.8~10.5, after obtaining neutralizing treatment；Step 2, the nickelous carbonate slurry after above-mentioned neutralizing treatment is added in aging reactor and is aged 1~20h, the nickelous carbonate slurry after being aged；Step 3, the nickelous carbonate slurry after above-mentioned ageing is eluted and is washed using pure water, then dried, obtain the nickelous carbonate of removal sulfate radical foreign matter.The present invention is by being first 40~70 DEG C with temperature and liquid alkaline that mass fraction is 10~32% washs the nickelous carbonate containing sulfate ion and is aged 1~20h to it, it is eluted and is washed with pure water again, to effectively avoid the problem that washing process is long, water loss is big, low efficiency, post-processing waste water are at high cost, and in the nickelous carbonate obtained S element content it is few.
Description
Technical field
The present invention relates to a kind of minimizing technologies for impurity in nickelous carbonate, are related to a kind of for sulfate radical in nickelous carbonate
The minimizing technology of impurity.
Background technique
Basic nickel carbonate is a kind of important inorganic fine chemicals, mainly for the preparation of various nickel salts, high-purity exquisiteness alkali
Formula nickelous carbonate can be applied to the intermediates such as smelting, ceramic paint, muffle painting ingredient, battery, contact agent, electronickelling and catalyst,
It is widely used, demand is very big, and belongs to classical catalyst intermediate, has long-term needs and market unsaturation；Its
In, conventional washing mode uses massive laundering or ammonia scrubbing etc. scheme, although there is certain effect to washing,
The too long inefficiency of washing process and a large amount of wash waters of consumption, lead to post-processing waste water higher cost, do not meet green production.
Summary of the invention
In view of this, the main purpose of the present invention is to provide a kind of removal sides for sulfate radical foreign matter in nickelous carbonate
Method solves the problems, such as that washing process is long in the prior art, water loss is big, low efficiency and post-processing waste water are at high cost.
In order to achieve the above objectives, the technical scheme of the present invention is realized as follows: it is a kind of miscellaneous for sulfate radical in nickelous carbonate
The minimizing technology of matter, this method are achieved by the steps of:
Step 1, the liquid alkaline that mass fraction is 10~32% is added in the nickelous carbonate containing sulfate ion and adjusts pH
Nickelous carbonate slurry of the value to 8.8~10.5, after obtaining neutralizing treatment；
Step 2, the nickelous carbonate slurry after the neutralizing treatment step 1 obtained, which is added in aging reactor, is aged 1~20h, obtains
Nickelous carbonate slurry after must being aged；
Step 3, the nickelous carbonate slurry after the ageing obtained using pure water to the step 2 is eluted and is washed, then is dried
It is dry, obtain the nickelous carbonate of removal sulfate radical foreign matter.
Preferably, in the step 1, the temperature of the liquid alkaline is 40~70 DEG C.
Preferably, in the step 1, the flow when liquid alkaline is added in the nickelous carbonate containing sulfate ion is 1~
10L/h。
Preferably, in the step 3, the temperature of the pure water is 70~85 DEG C, conductivity≤100 μ s/ of the pure water
m。
Preferably, in the step 3, the temperature of the drying is 95~105 DEG C, and the time of the drying is 2~3h.
Preferably, in the step 1, the nickelous carbonate containing sulfate ion specific the preparation method comprises the following steps:
Step 1.1, sodium carbonate liquor, the nickel that carbon acid ion concentration is 100~250g/L are prepared respectively in NaOH solution tank NaOH
The complexing agent that the nickel sulfate solution and mass fraction that ion concentration is 1~2moL/L are 0.1~2%；
Step 1.2, it is fed with metering pump, by sodium carbonate liquor described in step 1.1, nickel sulfate solution and complexing
Agent is added in reactor simultaneously, keeps the flow of nickel sulfate solution constant in fill process, by the stream for adjusting sodium carbonate liquor
The pH value of control system is measured, and is reacted at 70~99 DEG C, the mixture containing nickelous carbonate is obtained；
Step 1.3, the mixture containing the nickelous carbonate step 1.2 obtained is squeezed into centrifuge and is centrifuged,
Obtain the nickelous carbonate containing sulfate ion.
Preferably, in the step 1.1, the complexing agent is at least one of ammonium hydroxide complexing agent, EDTA complexing agent.
Preferably, in the step 1.2, when metering pump is fed, the flow of the sodium carbonate liquor is 5~1000L/h,
The flow of the nickel sulfate solution is 50~1000L/h, and the flow of the complexing agent is 0.1~10L/h.
Preferably, in the step 1.2, the pH value is 8.0~8.3.
Preferably, in the step 1.2, the reaction time is 5~100h.
Compared with prior art, the present invention is by being first 40~70 DEG C with temperature and liquid that mass fraction is 10~32%
Nickelous carbonate that neutralizing treatment contains sulfate ion is simultaneously aged 1~20h to it, then with temperature is 70~85 DEG C and conductivity≤100
The pure water of μ s/m is eluted and is washed, to effectively avoid big washing process length, water loss, low efficiency, at the later period
Manage waste water problem at high cost, and in the nickelous carbonate obtained S element content it is few, can be good at being applied to smelt, pottery
The industries such as porcelain pigment, muffle painting ingredient, battery, electronickelling.
Specific embodiment
In order to make the objectives, technical solutions, and advantages of the present invention clearer, with reference to embodiments, to this hair
It is bright to be further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, not
For limiting the present invention.
The embodiment of the invention provides a kind of minimizing technologies for sulfate radical foreign matter in nickelous carbonate, and this method is by such as
Lower step is realized:
It step 1, is that 1~10L/h adds according to flow by temperature is 40~70 DEG C, mass fraction is 10~32% liquid alkaline
The nickelous carbonate slurry for entering in the nickelous carbonate containing sulfate ion and adjusting pH value to 8.8~10.5, after obtaining neutralizing treatment；It is logical
After by temperature is 40~70 DEG C, mass fraction is 10~32% liquid alkaline and according to flow being first that 1~10L/h addition contains sulphur
In the nickelous carbonate of acid ion, at this moment, hydroxyl passes through positive charge by hydrogen ion in Hydrogen Binding Adsorption water, hydrogen ion in nickelous carbonate
There is certain attraction to sulfate ion, meanwhile, sulfate ion is bigger, absorption is easy, to can have by alkali cleaning
Effect destroys the Van der Waals force that hydrogen bond and charge generate, and sulfate ion adsorption capacity is weakened significantly, be more advantageous to sulfate radical from
Son removes；
Wherein, the nickelous carbonate containing sulfate ion specific the preparation method comprises the following steps:
Step 1.1, sodium carbonate liquor, the nickel that carbon acid ion concentration is 100~250g/L are prepared respectively in NaOH solution tank NaOH
The complexing agent that the nickel sulfate solution and mass fraction that ion concentration is 1~2moL/L are 0.1~2%；Wherein, complexing agent is
At least one of ammonium hydroxide complexing agent, EDTA complexing agent；
Step 1.2, it is fed with metering pump, by sodium carbonate liquor described in step 1.1, nickel sulfate solution and complexing
Agent is added in reactor simultaneously, keeps the flow of nickel sulfate solution constant in fill process, by the stream for adjusting sodium carbonate liquor
The pH value for measuring control system is 8.0~8.3, and 5~100h of reaction is carried out at 70~99 DEG C, is obtained mixed containing nickelous carbonate
Close object；Wherein, when metering pump is fed, the flow of sodium carbonate liquor is 5~1000L/h, the flow of nickel sulfate solution is 50~
1000L/h, the flow of complexing agent are 0.1~10L/h；
Step 1.3, the mixture containing the nickelous carbonate step 1.2 obtained is squeezed into centrifuge and is centrifuged,
Obtain the nickelous carbonate containing sulfate ion.
Step 2, the nickelous carbonate slurry after neutralizing treatment step 1 obtained, which is added in aging reactor, is aged 1~20h, obtains old
Nickelous carbonate slurry after change；By being aged to the nickelous carbonate slurry after neutralizing treatment, it is therefore intended that, hydroxyl adsorbs hydrogen in water
Ion and hydrogen ion have the more fully time by adsorption energy of the positive charge to sulfate ion, so that sulfate radical has reacted
Entirely；
Step 3, after the ageing for using temperature to obtain for 70~85 DEG C, conductivity≤100 μ s/m pure water to step 2
Nickelous carbonate slurry is eluted and is washed, then 2~3h is dried at 95~105 DEG C, obtains the carbonic acid of removal sulfate radical foreign matter
Nickel.
The present invention is by being first 40~70 DEG C with temperature and liquid alkaline that mass fraction is 10~32% is washed containing sulfate radical
The nickelous carbonate of ion is simultaneously aged 1~20h to it, then is drenched with temperature for 70~85 DEG C and conductivity≤100 μ s/m pure water
It washes and washs, washing process is long, water loss is big, low efficiency, post-processing waste water is at high cost asks to effectively avoid
Topic, and obtain nickelous carbonate in S element content it is few, can be good at be applied to smelting, ceramic paint, muffle painting ingredient,
The industries such as battery, electronickelling.
Embodiment 1
A kind of minimizing technology for sulfate radical foreign matter in nickelous carbonate, this method are achieved by the steps of:
It step 1, is that 5L/h addition contains sulfate radical according to flow by temperature is 55 DEG C, mass fraction is 20% liquid alkaline
In the nickelous carbonate of ion and the nickelous carbonate slurry that adjusts pH value to 9.5, after obtaining neutralizing treatment；
Step 2, the nickelous carbonate slurry after neutralizing treatment that step 1 obtains is added in aging reactor and is aged 10h, be aged
Nickelous carbonate slurry afterwards；
Step 3, the carbonic acid after the ageing for using temperature to obtain for 88 DEG C, conductivity≤100 μ s/m pure water to step 2
Nickel slurry is eluted and is washed, then 2.5h is dried at 100 DEG C, obtains the nickelous carbonate of removal sulfate radical foreign matter.
Wherein, the nickelous carbonate in step 1 containing sulfate ion specific the preparation method comprises the following steps:
Step 1.1, sodium carbonate liquor, the nickel ion concentration of carbonate ions concentration 150g/L are prepared respectively in NaOH solution tank NaOH
The ammonium hydroxide complexing agent that nickel chloride solution and mass fraction for 1.5mol/L are 1%；
Step 1.2, it is fed with metering pump, by sodium carbonate liquor, nickel chloride solution and ammonium hydroxide complexing agent in step 1.1
It is added in reactor that (reactor can flow out mother liquor during the reaction, and guarantee that nickelous carbonate is reacted with what mother liquor was constituted simultaneously
The solid content of system is continuously increased), keep that the flow of nickel salt solution is 50L/h, the flow of ammonium hydroxide complexing agent is in fill process
5L/h is constant, by flow (adjustable range of the flow of sodium carbonate liquor the is 50~1000L/h) control for adjusting sodium carbonate liquor
The pH value of system processed is 8.1, and 15h is reacted at 80 DEG C, obtains the mixture containing nickelous carbonate；
Step 1.3, the mixture containing nickelous carbonate step 1.2 obtained is squeezed into centrifuge and is centrifuged, and obtains
Nickelous carbonate containing sulfate ion.
Embodiment 2
A kind of minimizing technology for sulfate radical foreign matter in nickelous carbonate, this method are achieved by the steps of:
It step 1, is that 1L/h addition contains sulfate radical according to flow by temperature is 40 DEG C, mass fraction is 32% liquid alkaline
In the nickelous carbonate of ion and the nickelous carbonate slurry that adjusts pH value to 9.5, after obtaining neutralizing treatment；
Step 2, the nickelous carbonate slurry after neutralizing treatment that step 1 obtains is added in aging reactor and is aged 10h, be aged
Nickelous carbonate slurry afterwards；
Step 3, the carbonic acid after the ageing for using temperature to obtain for 85 DEG C, conductivity≤100 μ s/m pure water to step 2
Nickel slurry is eluted and is washed, then 3h is dried at 95 DEG C, obtains the nickelous carbonate of removal sulfate radical foreign matter.
Wherein, the nickelous carbonate in step 1 containing sulfate ion specific the preparation method comprises the following steps:
Step 1.1, sodium carbonate liquor, the nickel ion concentration of carbonate ions concentration 150g/L are prepared respectively in NaOH solution tank NaOH
The ammonium hydroxide complexing agent that nickel chloride solution and mass fraction for 1.5mol/L are 1%；
Step 1.2, it is fed with metering pump, by sodium carbonate liquor, nickel chloride solution and ammonium hydroxide complexing agent in step 1.1
It is added in reactor that (reactor can flow out mother liquor during the reaction, and guarantee that nickelous carbonate is reacted with what mother liquor was constituted simultaneously
The solid content of system is continuously increased), keep that the flow of nickel salt solution is 50L/h, the flow of ammonium hydroxide complexing agent is in fill process
5L/h is constant, by flow (adjustable range of the flow of sodium carbonate liquor the is 50~1000L/h) control for adjusting sodium carbonate liquor
The pH value of system processed is 8.1, and 15h is reacted at 80 DEG C, obtains the mixture containing nickelous carbonate；
Step 1.3, the mixture containing nickelous carbonate step 1.2 obtained is squeezed into centrifuge and is centrifuged, and obtains
Nickelous carbonate containing sulfate ion.
Embodiment 3
A kind of minimizing technology for sulfate radical foreign matter in nickelous carbonate, this method are achieved by the steps of:
It step 1, is that 10L/h addition contains sulfate radical according to flow by temperature is 70 DEG C, mass fraction is 10% liquid alkaline
In the nickelous carbonate of ion and the nickelous carbonate slurry that adjusts pH value to 9.5, after obtaining neutralizing treatment；
Step 2, the nickelous carbonate slurry after neutralizing treatment that step 1 obtains is added in aging reactor and is aged 10h, be aged
Nickelous carbonate slurry afterwards；
Step 3, the carbonic acid after the ageing for using temperature to obtain for 70 DEG C, conductivity≤100 μ s/m pure water to step 2
Nickel slurry is eluted and is washed, then 2h is dried at 105 DEG C, obtains the nickelous carbonate of removal sulfate radical foreign matter.
Wherein, the nickelous carbonate in step 1 containing sulfate ion specific the preparation method comprises the following steps:
Step 1.1, sodium carbonate liquor, the nickel ion concentration of carbonate ions concentration 150g/L are prepared respectively in NaOH solution tank NaOH
The ammonium hydroxide complexing agent that nickel chloride solution and mass fraction for 1.5mol/L are 1%；
Step 1.2, it is fed with metering pump, by sodium carbonate liquor, nickel chloride solution and ammonium hydroxide complexing agent in step 1.1
It is added in reactor that (reactor can flow out mother liquor during the reaction, and guarantee that nickelous carbonate is reacted with what mother liquor was constituted simultaneously
The solid content of system is continuously increased), keep that the flow of nickel salt solution is 50L/h, the flow of ammonium hydroxide complexing agent is in fill process
5L/h is constant, by flow (adjustable range of the flow of sodium carbonate liquor the is 50~1000L/h) control for adjusting sodium carbonate liquor
The pH value of system processed is 8.1, and 15h is reacted at 80 DEG C, obtains the mixture containing nickelous carbonate；
Step 1.3, the mixture containing nickelous carbonate step 1.2 obtained is squeezed into centrifuge and is centrifuged, and obtains
Nickelous carbonate containing sulfate ion.
Embodiment 4
A kind of minimizing technology for sulfate radical foreign matter in nickelous carbonate, this method are achieved by the steps of:
It step 1, is that 5L/h addition contains sulfate radical according to flow by temperature is 55 DEG C, mass fraction is 20% liquid alkaline
In the nickelous carbonate of ion and the nickelous carbonate slurry that adjusts pH value to 8.8, after obtaining neutralizing treatment；
Step 2, the nickelous carbonate slurry after neutralizing treatment that step 1 obtains is added in aging reactor and is aged 20h, be aged
Nickelous carbonate slurry afterwards；
Step 3, the carbonic acid after the ageing for using temperature to obtain for 88 DEG C, conductivity≤100 μ s/m pure water to step 2
Nickel slurry is eluted and is washed, then 2.5h is dried at 100 DEG C, obtains the nickelous carbonate of removal sulfate radical foreign matter.
Wherein, the nickelous carbonate in step 1 containing sulfate ion specific the preparation method comprises the following steps:
Step 1.1, sodium carbonate liquor, the nickel ion concentration of carbonate ions concentration 150g/L are prepared respectively in NaOH solution tank NaOH
The ammonium hydroxide complexing agent that nickel chloride solution and mass fraction for 1.5mol/L are 1%；
Step 1.2, it is fed with metering pump, by sodium carbonate liquor, nickel chloride solution and ammonium hydroxide complexing agent in step 1.1
It is added in reactor that (reactor can flow out mother liquor during the reaction, and guarantee that nickelous carbonate is reacted with what mother liquor was constituted simultaneously
The solid content of system is continuously increased), keep that the flow of nickel salt solution is 50L/h, the flow of ammonium hydroxide complexing agent is in fill process
5L/h is constant, by flow (adjustable range of the flow of sodium carbonate liquor the is 50~1000L/h) control for adjusting sodium carbonate liquor
The pH value of system processed is 8.1, and 15h is reacted at 80 DEG C, obtains the mixture containing nickelous carbonate；
Step 1.3, the mixture containing nickelous carbonate step 1.2 obtained is squeezed into centrifuge and is centrifuged, and obtains
Nickelous carbonate containing sulfate ion.
Embodiment 5
A kind of minimizing technology for sulfate radical foreign matter in nickelous carbonate, this method are achieved by the steps of:
It step 1, is that 1L/h addition contains sulfate radical according to flow by temperature is 40 DEG C, mass fraction is 32% liquid alkaline
In the nickelous carbonate of ion and the nickelous carbonate slurry that adjusts pH value to 8.8, after obtaining neutralizing treatment；
Step 2, the nickelous carbonate slurry after neutralizing treatment that step 1 obtains is added in aging reactor and is aged 20h, be aged
Nickelous carbonate slurry afterwards；
Step 3, the carbonic acid after the ageing for using temperature to obtain for 85 DEG C, conductivity≤100 μ s/m pure water to step 2
Nickel slurry is eluted and is washed, then 3h is dried at 95 DEG C, obtains the nickelous carbonate of removal sulfate radical foreign matter.
Wherein, the nickelous carbonate in step 1 containing sulfate ion specific the preparation method comprises the following steps:
Step 1.1, sodium carbonate liquor, the nickel ion concentration of carbonate ions concentration 150g/L are prepared respectively in NaOH solution tank NaOH
The ammonium hydroxide complexing agent that nickel chloride solution and mass fraction for 1.5mol/L are 1%；
Step 1.2, it is fed with metering pump, by sodium carbonate liquor, nickel chloride solution and ammonium hydroxide complexing agent in step 1.1
It is added in reactor that (reactor can flow out mother liquor during the reaction, and guarantee that nickelous carbonate is reacted with what mother liquor was constituted simultaneously
The solid content of system is continuously increased), keep that the flow of nickel salt solution is 50L/h, the flow of ammonium hydroxide complexing agent is in fill process
5L/h is constant, by flow (adjustable range of the flow of sodium carbonate liquor the is 50~1000L/h) control for adjusting sodium carbonate liquor
The pH value of system processed is 8.1, and 15h is reacted at 80 DEG C, obtains the mixture containing nickelous carbonate；
Step 1.3, the mixture containing nickelous carbonate step 1.2 obtained is squeezed into centrifuge and is centrifuged, and obtains
Nickelous carbonate containing sulfate ion.
Embodiment 6
A kind of minimizing technology for sulfate radical foreign matter in nickelous carbonate, this method are achieved by the steps of:
It step 1, is that 10L/h addition contains sulfate radical according to flow by temperature is 70 DEG C, mass fraction is 10% liquid alkaline
In the nickelous carbonate of ion and the nickelous carbonate slurry that adjusts pH value to 8.8, after obtaining neutralizing treatment；
Step 2, the nickelous carbonate slurry after neutralizing treatment that step 1 obtains is added in aging reactor and is aged 20h, be aged
Nickelous carbonate slurry afterwards；
Step 3, the carbonic acid after the ageing for using temperature to obtain for 70 DEG C, conductivity≤100 μ s/m pure water to step 2
Nickel slurry is eluted and is washed, then 2h is dried at 105 DEG C, obtains the nickelous carbonate of removal sulfate radical foreign matter.
Wherein, the nickelous carbonate in step 1 containing sulfate ion specific the preparation method comprises the following steps:
Step 1.1, sodium carbonate liquor, the nickel ion concentration of carbonate ions concentration 150g/L are prepared respectively in NaOH solution tank NaOH
The ammonium hydroxide complexing agent that nickel chloride solution and mass fraction for 1.5mol/L are 1%；
Step 1.2, it is fed with metering pump, by sodium carbonate liquor, nickel chloride solution and ammonium hydroxide complexing agent in step 1.1
It is added in reactor that (reactor can flow out mother liquor during the reaction, and guarantee that nickelous carbonate is reacted with what mother liquor was constituted simultaneously
The solid content of system is continuously increased), keep that the flow of nickel salt solution is 50L/h, the flow of ammonium hydroxide complexing agent is in fill process
5L/h is constant, by flow (adjustable range of the flow of sodium carbonate liquor the is 50~1000L/h) control for adjusting sodium carbonate liquor
The pH value of system processed is 8.1, and 15h is reacted at 80 DEG C, obtains the mixture containing nickelous carbonate；
Step 1.3, the mixture containing nickelous carbonate step 1.2 obtained is squeezed into centrifuge and is centrifuged, and obtains
Nickelous carbonate containing sulfate ion.
Embodiment 7
A kind of minimizing technology for sulfate radical foreign matter in nickelous carbonate, this method are achieved by the steps of:
It step 1, is that 5L/h addition contains sulfate radical according to flow by temperature is 55 DEG C, mass fraction is 20% liquid alkaline
In the nickelous carbonate of ion and the nickelous carbonate slurry that adjusts pH value to 10.5, after obtaining neutralizing treatment；
Step 2, the nickelous carbonate slurry after neutralizing treatment that step 1 obtains is added in aging reactor and is aged 1h, after being aged
Nickelous carbonate slurry；
Step 3, the carbonic acid after the ageing for using temperature to obtain for 88 DEG C, conductivity≤100 μ s/m pure water to step 2
Nickel slurry is eluted and is washed, then 2.5h is dried at 100 DEG C, obtains the nickelous carbonate of removal sulfate radical foreign matter.
Wherein, the nickelous carbonate in step 1 containing sulfate ion specific the preparation method comprises the following steps:
Step 1.1, sodium carbonate liquor, the nickel ion concentration of carbonate ions concentration 150g/L are prepared respectively in NaOH solution tank NaOH
The ammonium hydroxide complexing agent that nickel chloride solution and mass fraction for 1.5mol/L are 1%；
Step 1.2, it is fed with metering pump, by sodium carbonate liquor, nickel chloride solution and ammonium hydroxide complexing agent in step 1.1
It is added in reactor that (reactor can flow out mother liquor during the reaction, and guarantee that nickelous carbonate is reacted with what mother liquor was constituted simultaneously
The solid content of system is continuously increased), keep that the flow of nickel salt solution is 50L/h, the flow of ammonium hydroxide complexing agent is in fill process
5L/h is constant, by flow (adjustable range of the flow of sodium carbonate liquor the is 50~1000L/h) control for adjusting sodium carbonate liquor
The pH value of system processed is 8.1, and 15h is reacted at 80 DEG C, obtains the mixture containing nickelous carbonate；
Step 1.3, the mixture containing nickelous carbonate step 1.2 obtained is squeezed into centrifuge and is centrifuged, and obtains
Nickelous carbonate containing sulfate ion.
Embodiment 8
A kind of minimizing technology for sulfate radical foreign matter in nickelous carbonate, this method are achieved by the steps of:
It step 1, is that 1L/h addition contains sulfate radical according to flow by temperature is 40 DEG C, mass fraction is 32% liquid alkaline
In the nickelous carbonate of ion and the nickelous carbonate slurry that adjusts pH value to 10.5, after obtaining neutralizing treatment；
Step 2, the nickelous carbonate slurry after neutralizing treatment that step 1 obtains is added in aging reactor and is aged 1h, after being aged
Nickelous carbonate slurry；
Step 3, the carbonic acid after the ageing for using temperature to obtain for 85 DEG C, conductivity≤100 μ s/m pure water to step 2
Nickel slurry is eluted and is washed, then 3h is dried at 95 DEG C, obtains the nickelous carbonate of removal sulfate radical foreign matter.
Wherein, the nickelous carbonate in step 1 containing sulfate ion specific the preparation method comprises the following steps:
Step 1.1, sodium carbonate liquor, the nickel ion concentration of carbonate ions concentration 150g/L are prepared respectively in NaOH solution tank NaOH
The ammonium hydroxide complexing agent that nickel chloride solution and mass fraction for 1.5mol/L are 1%；
Step 1.2, it is fed with metering pump, by sodium carbonate liquor, nickel chloride solution and ammonium hydroxide complexing agent in step 1.1
It is added in reactor that (reactor can flow out mother liquor during the reaction, and guarantee that nickelous carbonate is reacted with what mother liquor was constituted simultaneously
The solid content of system is continuously increased), keep that the flow of nickel salt solution is 50L/h, the flow of ammonium hydroxide complexing agent is in fill process
5L/h is constant, by flow (adjustable range of the flow of sodium carbonate liquor the is 50~1000L/h) control for adjusting sodium carbonate liquor
The pH value of system processed is 8.1, and 15h is reacted at 80 DEG C, obtains the mixture containing nickelous carbonate；
Step 1.3, the mixture containing nickelous carbonate step 1.2 obtained is squeezed into centrifuge and is centrifuged, and obtains
Nickelous carbonate containing sulfate ion.
Embodiment 9
A kind of minimizing technology for sulfate radical foreign matter in nickelous carbonate, this method are achieved by the steps of:
It step 1, is that 10L/h addition contains sulfate radical according to flow by temperature is 70 DEG C, mass fraction is 10% liquid alkaline
In the nickelous carbonate of ion and the nickelous carbonate slurry that adjusts pH value to 10.5, after obtaining neutralizing treatment；
Step 2, the nickelous carbonate slurry after neutralizing treatment that step 1 obtains is added in aging reactor and is aged 1h, after being aged
Nickelous carbonate slurry；
Step 3, the carbonic acid after the ageing for using temperature to obtain for 70 DEG C, conductivity≤100 μ s/m pure water to step 2
Nickel slurry is eluted and is washed, then 2h is dried at 105 DEG C, obtains the nickelous carbonate of removal sulfate radical foreign matter.
Wherein, the nickelous carbonate in step 1 containing sulfate ion specific the preparation method comprises the following steps:
Step 1.1, sodium carbonate liquor, the nickel ion concentration of carbonate ions concentration 150g/L are prepared respectively in NaOH solution tank NaOH
The ammonium hydroxide complexing agent that nickel chloride solution and mass fraction for 1.5mol/L are 1%；
Step 1.2, it is fed with metering pump, by sodium carbonate liquor, nickel chloride solution and ammonium hydroxide complexing agent in step 1.1
It is added in reactor that (reactor can flow out mother liquor during the reaction, and guarantee that nickelous carbonate is reacted with what mother liquor was constituted simultaneously
The solid content of system is continuously increased), keep that the flow of nickel salt solution is 50L/h, the flow of ammonium hydroxide complexing agent is in fill process
5L/h is constant, by flow (adjustable range of the flow of sodium carbonate liquor the is 50~1000L/h) control for adjusting sodium carbonate liquor
The pH value of system processed is 8.1, and 15h is reacted at 80 DEG C, obtains the mixture containing nickelous carbonate；
Step 1.3, the mixture containing nickelous carbonate step 1.2 obtained is squeezed into centrifuge and is centrifuged, and obtains
Nickelous carbonate containing sulfate ion.
Embodiment 10
A kind of minimizing technology for sulfate radical foreign matter in nickelous carbonate, this method are achieved by the steps of:
It step 1, is that 5L/h addition contains sulfate radical according to flow by temperature is 40 DEG C, mass fraction is 32% liquid alkaline
In the nickelous carbonate of ion and the nickelous carbonate slurry that adjusts pH value to 9.0, after obtaining neutralizing treatment；
Step 2, the nickelous carbonate slurry after neutralizing treatment that step 1 obtains is added in aging reactor and is aged 20h, be aged
Nickelous carbonate slurry afterwards；
Step 3, the carbonic acid after the ageing for using temperature to obtain for 85 DEG C, conductivity≤100 μ s/m pure water to step 2
Nickel slurry is eluted and is washed, then 3h is dried at 95 DEG C, obtains the nickelous carbonate of removal sulfate radical foreign matter.
Wherein, the nickelous carbonate in step 1 containing sulfate ion specific the preparation method comprises the following steps:
Step 1.1, sodium carbonate liquor, the nickel ion concentration of carbonate ions concentration 150g/L are prepared respectively in NaOH solution tank NaOH
The EDTA complexing agent that nickel chloride solution and mass fraction for 1.5mol/L are 1%；
Step 1.2, it is fed with metering pump, by sodium carbonate liquor, nickel chloride solution and ammonium hydroxide complexing agent in step 1.1
It is added in reactor that (reactor can flow out mother liquor during the reaction, and guarantee that nickelous carbonate is reacted with what mother liquor was constituted simultaneously
The solid content of system is continuously increased), keep that the flow of nickel salt solution is 50L/h, the flow of ammonium hydroxide complexing agent is in fill process
5L/h is constant, by flow (adjustable range of the flow of sodium carbonate liquor the is 50~1000L/h) control for adjusting sodium carbonate liquor
The pH value of system processed is 8.1, and 15h is reacted at 80 DEG C, obtains the mixture containing nickelous carbonate；
Step 1.3, the mixture containing nickelous carbonate step 1.2 obtained is squeezed into centrifuge and is centrifuged, and obtains
Nickelous carbonate containing sulfate ion.
The detection of S content, detection knot are carried out to the nickelous carbonate for the removal sulfate radical foreign matter that embodiment 1- embodiment 10 obtains
Fruit is as shown in table 1:
The testing number of S content in the nickelous carbonate for the removal sulfate radical foreign matter that 1 1- of embodiment of the present invention embodiment 10 of table obtains
According to
| S content/% | |
| Embodiment 1 | 0.005% |
| Embodiment 2 | 0.007% |
| Embodiment 3 | 0.006% |
| Embodiment 4 | 0.008% |
| Embodiment 5 | 0.004% |
| Embodiment 6 | 0.006% |
| Embodiment 7 | 0.005% |
| Embodiment 8 | 0.007% |
| Embodiment 9 | 0.008% |
| Embodiment 10 | 0.006% |
| It is conventional | 0.025% |
From table 1 it follows that S content is respectively less than in the nickelous carbonate for the removal sulfate radical foreign matter that the present invention obtains
0.01%, it can be seen that, the performance of the nickelous carbonate for the removal sulfate radical foreign matter that the present invention obtains is superior to existing washing methods and obtains
The properties of the basic nickel carbonate obtained, so that it has a wide range of application.
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 minimizing technology for sulfate radical foreign matter in nickelous carbonate, which is characterized in that this method is achieved by the steps of:
Step 1, by mass fraction be 10~32% liquid alkaline be added the nickelous carbonate containing sulfate ion in and adjust pH value to
8.8~10.5, the nickelous carbonate slurry after obtaining neutralizing treatment；
Step 2, the nickelous carbonate slurry after the neutralizing treatment step 1 obtained, which is added in aging reactor, is aged 1~20h, obtains old
Nickelous carbonate slurry after change；
Step 3, the nickelous carbonate slurry after the ageing obtained using pure water to the step 2 is eluted and is washed, then is dried, and is obtained
The nickelous carbonate of sulfate radical foreign matter must be removed.
2. a kind of minimizing technology for sulfate radical foreign matter in nickelous carbonate according to claim 1, which is characterized in that described
In step 1, the temperature of the liquid alkaline is 40~70 DEG C.
3. a kind of minimizing technology for sulfate radical foreign matter in nickelous carbonate according to claim 2, which is characterized in that described
In step 1, the flow when liquid alkaline is added in the nickelous carbonate containing sulfate ion is 1~10L/h.
4. a kind of minimizing technology for sulfate radical foreign matter in nickelous carbonate according to claim 3, which is characterized in that described
In step 3, the temperature of the pure water is 70~85 DEG C, conductivity≤100 μ s/m of the pure water.
5. a kind of removing method for sulfate radical foreign matter in nickelous carbonate according to claim 4, which is characterized in that described
In step 3, the temperature of the drying is 95~105 DEG C, and the time of the drying is 2~3h.
6. a kind of removing method for sulfate radical foreign matter in nickelous carbonate according to claim 1, which is characterized in that described
In step 1, the nickelous carbonate containing sulfate ion specific the preparation method comprises the following steps:
Step 1.1, sodium carbonate liquor, the nickel ion that carbon acid ion concentration is 100~250g/L are prepared respectively in NaOH solution tank NaOH
The complexing agent that the nickel sulfate solution and mass fraction that concentration is 1~2moL/L are 0.1~2%；
Step 1.2, it is fed with metering pump, simultaneously by sodium carbonate liquor described in step 1.1, nickel sulfate solution and complexing agent
It is added in reactor, keeps the flow of nickel sulfate solution constant in fill process, by the flow control for adjusting sodium carbonate liquor
The pH value of system, and reacted at 70~99 DEG C, obtain the mixture containing nickelous carbonate；
Step 1.3, the mixture containing the nickelous carbonate step 1.2 obtained is squeezed into centrifuge and is centrifuged, and obtains
Nickelous carbonate containing sulfate ion.
7. a kind of removing method for sulfate radical foreign matter in nickelous carbonate according to claim 6, which is characterized in that described
In step 1.1, the complexing agent is at least one of ammonium hydroxide complexing agent, EDTA complexing agent.
8. a kind of removing method for sulfate radical foreign matter in nickelous carbonate according to claim 7, which is characterized in that described
In step 1.2, when metering pump is fed, the flow of the sodium carbonate liquor is 5~1000L/h, the flow of the nickel sulfate solution
For 50~1000L/h, the flow of the complexing agent is 0.1~10L/h.
9. a kind of removing method for sulfate radical foreign matter in nickelous carbonate according to claim 8, which is characterized in that described
In step 1.2, the pH value is 8.0~8.3.
10. a kind of minimizing technology for sulfate radical foreign matter in nickelous carbonate according to claim 6-9 any one, special
Sign is, in the step 1.2, the reaction time is 5~100h.
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| CN112441624A (en) * | 2019-08-30 | 2021-03-05 | 荆门市格林美新材料有限公司 | Preparation method of nickel-cobalt-aluminum precursor with high tap density and low impurity content |
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